ALBERT

Description:    High-performance counter-current chromatography has been used for the separation of delphinidin-3- O -sambubioside, cyanidin-3- O -sambubioside and p -coumaric acid from crude extract of cranberry. The separation was performed with a two-phase solvent system composed of butanol/0.05% aqueous trifluoroacetic acid/methanol at a volume ratio of 4:5:1. The two-phase solvent system was selected following the determination of partition coefficients ( K ) in a range of solvent systems using a robotic solvent system selection method. Analytical scale CCC confirmed that this phase system separated the components from a crude cranberry extract (40 mg scale) with acceptable purities. Preparative CCC of 400 mg of crude yielded 4.2 mg of p -coumaric acid at a purity of over 98%, 3.6 mg of delphinidin-3- O -sambubioside at a purity of over 97% and 4.5 mg of cyanidin-3- O -sambubioside at a purity of 73%, which was further purified by preparative high-performance liquid chromatography to yield 3 mg cyanidin-3- O -sambubioside at 95% purity. The identification of delphinidin-3- O -sambubioside, cyanidin-3- O -sambubioside and p -coumaric acid was performed by ESI-MS, 1H-NMR and 13C-NMR spectra. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2076-5 Authors Yun Wei, State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing, 100029 China M. Razwan Sardar, State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing, 100029 China Ian A. Sutherland, Advanced Bioprocessing Centre, Brunel Institute for Bioengineering, Brunel University, Uxbridge, Middlesex, UB8 3PH UK Derek Fisher, Advanced Bioprocessing Centre, Brunel Institute for Bioengineering, Brunel University, Uxbridge, Middlesex, UB8 3PH UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In this study, plasma samples were collected from 28 health volunteers and 66 lung cancer patients. Ultraperformance HILIC/Q-TOF MS-based metabonomic techniques were employed to compare the highly polar metabolites (HPMs) in the plasma of patients with lung cancer and those in the plasma of healthy volunteers. High separation efficiency and good repeatability of the HILIC/Q-TOF MS method were observed. Partial least squares discriminant analysis (PLS-DA) of the data from both ESI+ and ESI− mode revealed good classifications between the health volunteer and the lung cancer patients. This result showed that the HPMs from lung cancer patients and healthy controls were significantly different. The correct classification rate of models in both ion modes reached 100%, indicating that the metabonomics method established in this study could predict the plasma samples with high accuracy. Besides, we found 19 ions that show a significant difference in levels between lung cancer patients and healthy controls. Finally, we conducted a primary study of the effect of radiotherapy on HPMs in lung cancer patients. Clear differences among the HPMs of patients in different radiotherapy periods and significant changes in levels of the 19 ions after radiotherapy were noted. This demonstrated that radiotherapy influences the metabolism system of patients. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-2077-4 Authors Xiaoming Cai, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Jun Dong, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Lijuan Zou, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Xingya Xue, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Xiuli Zhang, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Xinmiao Liang, Dalian Institute of Chemical Physics, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Dalian, 116023 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Imperatorin (IMP) is a biologically active ingredient isolated from a traditional Chinese medicine (TCM), Angelica dahurica . To obtain the brain distribution data of IMP in rats, the concentrations of IMP in cortex, cerebellum, diencephalon, brain stem, striatum and hippocampus were measured by a simple and sensitive HPLC–UV method. The analytes were prepared by a liquid–liquid extraction method and the separation of IMP was performed on a Hypersil BDS C18 column (250 mm × 4.6 mm i.d., 5 μm) using acetonitrile–water (60:40, v/v) as mobile phase which was delivered at 1.0 mL min −1 . Ultraviolet detection was performed at 300 nm. Using a weighted (1/c 2 ) least square method, linear calibration curves for the six regions were obtained ( r  ≥ 0.9990) with a lower limit of quantification (LLOQ) of 0.075 μg g −1 for cortex, cerebellum, diencephalon and brain stem or 0.15 μg g −1 for striatum and hippocampus, and the recovery was greater than 90% for each tissue sample. The within- and between-day precisions (expressed as the relative standard deviation, RSD) were less than 10%. The validated method has been successfully applied to the brain distribution study in rats. The results showed that IMP could pass through the blood–brain barrier easily. And the higher concentration in striatum and hippocampus compared with the others might indicate that they were the target regions of IMP in rat brain. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2073-8 Authors Xiaokai Zhang, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Yanhua Xie, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Wei Cao, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Qian Yang, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Shan Miao, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Siwang Wang, Institute of Materia Medica, School of Pharmacy, Fourth Military Medical University, 169 West Changle Road, Xi’an, 710032 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A rapid and sensitive LC–MS–MS method for the simultaneous determination of escin Ia and isoescin Ia in rat plasma, urine, feces and bile samples was developed and validated. Analytes and telmisartan [internal standard (IS)] were extracted by solid-phase extraction on C 18 cartridges. Components in the extract were separated on an HC-C 18 column (5 μm, 150 × 4.6 mm i.d.) using 10 mM ammonium acetate–methanol–acetonitrile (40:30:30, v/v/v ) as the mobile phase. The method demonstrated good linearity from 5 ng mL −1 (LLOQ) to 1,500 ng mL −1 for both escin Ia and isoescin Ia. Intra- and inter-day precision measured as RSD was within ±15%. Recoveries and matrix effects of both escin Ia and isoescin Ia were satisfactory in all four matrices examined. The method was successfully applied to a pharmacokinetic study in Wistar rats after a single intravenous administration of escin Ia at the dose of 1.0 mg kg −1 . Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-2053-z Authors Mengliang Zhang, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Xiujun Wu, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Xiangyong Cui, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Feng Gao, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Chao Zhang, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Yan Yang, College of Life Science, Jilin University, Changchun, 130023 People’s Republic of China Jingkai Gu, Research Center for Drug Metabolism, Jilin University, Changchun, 130023 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The molecular structures of 117 nitrogen-containing polycyclic aromatic compounds (N-PACs) were described by a method of molecular structural characterization (MSC) called molecular electronegativity interaction vector (MEIV). The samples were divided into a training set and a test set. For the training set, a quantitative structure–retention relationship (QSRR) model was built up by multiple linear regression (MLR) and the model was evaluated by performing the cross validation with the leave-one-out (LOO) procedure. The correlation coefficient ( R ) and the cross-verification correlation coefficient ( R CV ) of the model were 0.992 and 0.991, respectively. Moreover, the model was evaluated by the test set and satisfactory results with a correlation coefficient ( R test ) of 0.993 were obtained. The results suggested good stability and predictability of the model. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2078-3 Authors Limin Liao, College of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang, 641112 Sichuan, People’s Republic of China Jianfeng Li, College of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang, 641112 Sichuan, People’s Republic of China Bi Wang, College of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang, 641112 Sichuan, People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Isoliquiritigenin, a chalcone found in licorice root and many other plants, has shown potential antioxidant, estrogenic and antitumor activities. The present study was to investigate urinary metabolism of isoliquiritigenin in Wistar rats by ultra-high pressure liquid chromatography coupled to electrospray ionization TOF–MS (UHPLC–TOF–MS)-based xenometabolomics. Urine samples were collected before and after oral administration of isoliquiritigenin, and analyzed by UHPLC–TOF–MS. After deconvolution, the resulting data matrices were subjected to multivariate data analysis. Projection to latent structures discriminant analysis was performed to screen the metabolites. Fifteen urinary metabolites of isoliquiritigenin were screened out and 13 of them were further identified by Agilent MassHunter Software. The results of this work show that UHPLC–TOF–MS-based xenometabolomics was able to comprehensively identify the metabolites of phytochemicals and may represent a valuable tool for monitoring the food consumption. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-2072-9 Authors Guangguo Tan, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Ziyang Lou, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Xing Dong, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Wuhong Li, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Wenting Liao, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Zhenyu Zhu, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Yifeng Chai, School of Pharmacy, Second Military Medical University, Shanghai, 200433 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A new facile, rapid, inexpensive, and sensitive method based on magnetic micro-solid phase extraction (M-μ-SPE) coupled to gas chromatography–mass spectrometry (GC–MS) was developed for determination of the herbicide oxadiargyl in environmental water samples. The feasibility of employing non-modified magnetic nanoparticles (MNPs) as sorbent was examined and applied to perform the extraction process. Influential parameters affecting the extraction efficiency along with desorption conditions were investigated and optimized. The limit of detection (LOD, S/N = 3) and limit of quantification (LOQ, S/N = 10) of the method under optimized conditions were 0.005 and 0.030 ng mL −1 , respectively. The relative standard deviations (RSD) ( n  = 3) at a concentration of 0.10 ng mL −1 was 11%. The calibration curve of oxadiargyl showed linearity in the range of 0.050–0.50 ng mL −1 . The developed method was successfully applied to the extraction of oxadiargyl from spiked tap water and Zayande-Rood River water samples and the relative recoveries of 98 and 94% were obtained, respectively. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-2083-6 Authors Habib Bagheri, Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran Omid Zandi, Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran Ali Aghakhani, Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Robert L. Wixom and Charles W. Gehrke (Eds.), Associate Editors Deborah L. Chance and Thomas P. Mawhinney: Chromatography. A Science of Discovery Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-2080-9 Authors Edward R. Adlard, Burton, South Wirral, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Activated charcoal column chromatography was successfully applied for preparative extraction of artemisinin with high-purity from Artemisia annua L. in one single run for the first time in this study. The adsorption kinetics study showed that powdery activated charcoal had high adsorption speed for artemisinin. The experimental adsorption data fitted well using the Langmuir adsorption model. The optimal parameters for the extraction of artemisinin were obtained using a column packed with activated charcoal: the loading amount, 1 g extract/5 g activated charcoal; the elution mode, CH 2 Cl 2 –MeOH (2:5, v/v ) for 5 BV (bed volume) after the removal of some impurities with CH 2 Cl 2 –MeOH (1:10, v/v ). With this optimized condition, artemisinin was finally obtained with purity at 95.2% and the recovery at 72.3%. The developed technique would provide a feasible large-scale method for the extraction of artemisinin in pharmaceutical industry. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2075-6 Authors Jindi Xu, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing, 210009 People’s Republic of China Jianguang Luo, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing, 210009 People’s Republic of China Lingyi Kong, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing, 210009 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Thorsten Teutenberg: High Temperature Liquid Chromatography. A User’s Guide for Method Development Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-2081-8 Authors Tony Edge, Runcorn, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A reversed-phase liquid chromatography coupled to tandem mass spectrometry (LC–MS–MS) method was developed and validated for the determination of fulvestrant in rat plasma. Sample preparation involved a liquid-liquid extraction using 1.0 mL of n -hexane–isopropanol (90:10, v/v ) to extract the analyte from 0.1 mL of rat plasma. The analytes were separated on a phenyl-based column using the mobile phase consisting of methanol/water containing 5 mM ammonium acetate at the flow rate of 0.3 mL min −1 . The analytes were monitored by tandem mass spectrometry under electrospray negative ionization mode. Linear calibration curves were generated over the fulvestrant concentration ranges of 0.05–10.0 ng mL −1 in rat plasma. The accuracy and within- and between-day precisions were within the generally accepted criteria for bioanalytical methods (〈15%). This developed and validated assay method was successfully employed to characterize the plasma concentration-time profile of fulvestrant after its intramuscular administration in rats at a dose of 10 mg kg −1 . Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-2071-x Authors Zhongyang Liu, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Guangzhi Gu, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Huimin Xia, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Qiang Liu, School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou, 350108 Fujian, People’s Republic of China Zhiqing Pang, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Xinguo Jiang, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Jun Chen, Department of Pharmaceutics, School of Pharmacy, Fudan University, Shanghai, 201203 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The purpose of the study is first to develop a sensitive and rapid ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for the determination of a new synthesized tubulin ligand, N -(2,6-dimethoxypyridine-3-yl)-9-methylcarbazole-3-sulfonamide (IG-105), in rat plasma. The analyte and internal standard (carbamazepine) were extracted by liquid/liquid extraction with petroleum ether/diethyl ether (2:1, v/v). The chromatographic separation was performed on an Acquity UPLC BEH C 18 column with a mobile phase gradient consisting of methanol and water. The mass spectrometric detection was performed by triple-quadrupole mass spectrometry with multiple reaction monitoring (MRM) via an ESI source operating in positive ionization mode. The mass transitions m / z 398→153 and m / z 237→194 were used to assay the analyte and IS, respectively. The method demonstrated good linearity over a concentration range of 0.67–333.33 ng mL −1 , and the lower limit of quantitation (LLOQ) of IG-105 was 0.67 ng mL −1 . The intra- and inter-day precision (relative standard deviation) values were 〈6%, and the accuracy (relative error) was 〈5% at three quality control levels. The extraction recovery of IG-105 and IS was 84.45 and 88.5%, respectively. Finally, the validated method was successfully applied to a pharmacokinetic study of IG-105 in rat plasma. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2033-3 Authors Xin Li, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Yinghua Sun, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Xiaohong Liu, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Yanhua Liu, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Jin Sun, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Zhonggui He, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Mailbox 59, Shenyang, 110016 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The extraction method of pharmaceutical and personal care products (PPCPs) has become a popular issue due to the emergence of PPCPs as contaminants. In this work, polycyclic musks, a typical type of PPCPs, were selected to test various techniques including microwave-assisted extraction (MAE), simultaneous distillation-solvent extraction (SDSE), Soxhlet extraction (SE), and ultrasound probe (UP). MAE and UP proved to be more effective pretreatment techniques than SE and SDSE, with high recovery, repeatability, accuracy, efficiency, little solvent consumption, and acceptable matrix effects. Notably, the chemical methods usually did not work well for the determination of bioavailability and the environmental fate of pollutants was overestimated. In this work, wheat ( Triticum aestivum L . ) was used as the ecological receptor to evaluate the bioavailability of chemical pollutants. The concentrations of polycyclic musks in sediments by way of UP extraction had a significant correlation ( R 2  〉 0.9, P  〈 0.01) with the concentrations in roots of wheat and the changes of chlorophyll, malondialdehyde and peroxidase in leaves of wheat. These changes suggest that the concentrations of polycyclic musks in sediments using UP extraction were comparable with the level of those in vivo. Through this work, it was discovered that using UP with a different solvent was suitable for determining total concentrations and the bioavailable fractions in sediments. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2084-5 Authors Xiangang Hu, Key Laboratory of Pollution Processes and Environmental Criteria (Ministry of Education), College of Environmental Science and Engineering, Nankai University, Tianjin, 300071 China Qixing Zhou, Key Laboratory of Pollution Processes and Environmental Criteria (Ministry of Education), College of Environmental Science and Engineering, Nankai University, Tianjin, 300071 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Room temperature ionic liquids are novel solvents with a rather specific blend of physical and solution properties that make them of interest for applications in separation science. In this study, a green, simple, and sensitive sample pretreatment procedure coupled with high-performance liquid chromatography (HPLC) was developed for the analysis of sulfadimidine (SM2) that exploits an aqueous two-phase system based on 1-butyl-3-methylimidazolium tetrafluoroborate ([Bmim]BF 4 ) and ammonium sulfate ((NH 4 ) 2 SO 4 ) using a liquid–liquid extraction technique in real environmental water samples. The influences of the concentration of (NH 4 ) 2 SO 4 , pH value, temperature, and concentration of SM2 on the extraction efficiency of SM2 were determined. Under optimal conditions, the extraction efficiencies of SM2 were over 93.7%. Calibration curves yielded good linearity ( R 2  = 0.9998) over the range 3–240 ng mL −1 , and the limit of detection and limit of quantification for analytes were 0.9 ng mL −1 and 3 ng mL −1 , respectively. The proposed method was successfully applied to the quantification of SM2 in water samples and recoveries were in the range of 101.2–107%. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2079-2 Authors Cuilan Yu, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Juan Han, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Yun Wang, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Yongsheng Yan, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Shiping Hu, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Yanfang Li, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Chunhong Ma, School of Chemistry and Chemical Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang, 212013 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Static headspace sampling, headspace solid-phase microextraction, and direct immersion solid-phase microextraction coupled with gas chromatography–tandem mass spectrometry have been developed for determination of the volatile components in Radix bupleuri injection. A total of 78 compounds were identified from Radix bupleuri injection. Direct immersion solid-phase microextraction gave a better extraction efficiency for polar compounds, including organic acids and alcohols, than headspace solid-phase microextraction or static headspace sampling. Product ion isotope pattern analysis was applied to determine the elemental composition of the precursor ion, which could make the qualitative analysis more accurate and reliable. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-2082-7 Authors Suhong Liu, Research Center for Health and Nutrition, Shanghai University of Traditional Chinese Medicine, 1200 Cailun Road, Shanghai, 201203 People’s Republic of China Sensen Lu, Research Center for Health and Nutrition, Shanghai University of Traditional Chinese Medicine, 1200 Cailun Road, Shanghai, 201203 People’s Republic of China Yue Su, Research Center for Health and Nutrition, Shanghai University of Traditional Chinese Medicine, 1200 Cailun Road, Shanghai, 201203 People’s Republic of China Yinlong Guo, Shanghai Mass Spectrometry Center, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai, 200032 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Tenofovir octadecyloxyethyl ester (TOE) is a novel ester prodrug of tenofovir. It is currently developed as a promising antiviral preclinical candidate. A simple and sensitive liquid chromatography–tandem mass spectrometry (LC–MS–MS) method has been developed and validated to quantify TOE in rat plasma. The method involves a simple extraction of TOE and loratadine (internal standard) from rat plasma after protein precipitation. Chromatographic separation was performed on a C 18 column by isocratic elution with acetonitrile and 5 mM ammonium acetate containing 0.03% ammonium hydroxide (70:30, v/v ), at a flow rate of 0.3 mL min −1 . MS detection was performed on an API 3000 triple quadrupole mass spectrometer operating in ESI positive ionization mode. Ions monitored in the multiple selected reaction monitoring mode were m/z 584→270 for TOE and m/z 383→337 for loratadine, respectively. A linear calibration curve was established over the concentration range from 12.5 to 2,500 ng mL −1 ( r 2  = 0.9961) with the lower quantitative limit of 12.5 ng mL −1 . The inter- and intra-day RSD were all 〈9.61%, while the accuracy (RE) was within the range from −8.40 to 4.20%. This novel method has been successfully applied to a pharmacokinetic study to obtain the oral concentration–time profile of TOE in rats. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2040-4 Authors Meng-si Liu, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Ji-fen Guo, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Hong Yi, Institution of Medicinal Biotechnology, Beijing Union Medical College, Beijing, 100050 People’s Republic of China Hua Li, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Zhuo-rong Li, Institution of Medicinal Biotechnology, Beijing Union Medical College, Beijing, 100050 People’s Republic of China Chun-jie Zhao, Shenyang Pharmaceutical University, Liaoning, 110016 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Allan J. Bard and Cynthia G. Zoski (Eds): Electroanalytical Chemistry Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-2044-0 Authors Grégoire Herzog, Life Sciences Interface, Tyndall National Institute, Lee Maltings, University College, Cork, Ireland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Trans -2-nonenal is an aldehyde contributing to an unpleasant off-flavor and odor of rancid butter in stored beer. The automated solid-phase microextraction technique (SPME) coupled with gas chromatography (GC) and solid-phase dynamic extraction (SPDE) coupled with gas chromatography were optimized and introduced to determine trans -2-nonenal in barley, malt and beer. Five types of SPME fibers coated with different stationary phases (100 μm PDMS, 65 μm PDMS/DVB, 85 μm CAR/PDMS, 50/30 μm DVB/CAR/PDMS, 85 μm PA) and two needles (PDMS, PDMS/AC) were compared and tested for their efficiencies in the headspace (HS) SPME and SPDE determination of trans -2-nonenal in barley, malt and beer. The highest extraction efficiency of HS-SPME was achieved with the PDMS/DVB fiber, and addition of 1.5 g of NaCl, extraction time was 20 min at 60 °C. The highest extraction efficiency of HS-SPDE was obtained with the PDMS needle, 15 extraction strokes at 60 °C and addition of 1.5 g of NaCl. Trans -2-nonenal was identified with the method of HS-SPME coupled gas chromatography-mass spectrometry (GC–MS); the samples were analyzed using the HS-SPME-GC-coupled gas chromatography-flame ionization detector (GC-FID) technique. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1958-x Authors Zdenek Svoboda, Research Institute of Brewing and Malting, Malting Institute, Mostecká 7, 614 00 Brno, Czech Republic Renata Mikulíková, Research Institute of Brewing and Malting, Malting Institute, Mostecká 7, 614 00 Brno, Czech Republic Sylvie Běláková, Research Institute of Brewing and Malting, Malting Institute, Mostecká 7, 614 00 Brno, Czech Republic Karolína Benešová, Research Institute of Brewing and Malting, Malting Institute, Mostecká 7, 614 00 Brno, Czech Republic Ivana Márová, Faculty of Chemistry, Brno University of Technology, Purkyňova 118, 612 00 Brno, Czech Republic Zdenek Nesvadba, Agrotest Fyto, Havlíčkova 2787/121, 768 01 Kroměříž, Czech Republic Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The separation and determination of 19 amino acids were examined using two stages derivatization with trifluoroacetylacetone and ethyl chloroformate from the column HP-5 (30 m × 0.32 mm id) with film thickness 0.25 μm at an initial column temperature 100 °C for 2 min with ramping of 20 °C min −1 up to 250 °C with nitrogen flow rate of 3 mL min −1 . The detection was performed by flame ionization detector. Total separation time was 10 min. The separation was repeatable with relative standard deviation (RSD) ( n  = 5) within 1.5–1.9 and 1.3–1.7% in terms of retention time and peak height/peak area, respectively. The method was applied for the determination of amino acids from skin samples of psoriatic patients ( n  = 6), arsenicosis patients ( n  = 5) and normal subjects ( n  = 9) and variation in the contents of the amino acids was noted. The RSDs for the determination were obtained within 3%. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1957-y Authors Muhammad Yar Khuhawar, Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Pakistan Subhan Ali Majidano, Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Pakistan Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In this study, a rapid, sensitive, and fully automated on-line solid phase extraction (SPE)–liquid chromatography (LC)–mass spectrometry (MS) method for the analysis of explosive residues in water, was systematically investigated. First, separation of explosive residues was achieved by reverse-phase chromatography using an XDB-C18 column in 30 min with an eluent containing 0.1% acetic acid, 5 mM ammonium acetate, and methanol. Secondly, atmospheric pressures chemical ionization (APCI) and electrospray ionization (ESI) interfaced with the MS detector were used to examine the explosive residues, indicating that APCI–MS was more suitable than ESI–MS for the detection of explosives. Thirdly, the conditions for on-line SPE, including solvent pH and sample injected volume, were optimized. The calibration curves obtained for all explosives studied were linear in the concentration range 0.5–50 μg L −1 . The detection limits of this method ranged from 0.05 to 0.5 μg L −1 when 4000 μL of sample was on-line pre-concentrated on C18 enrichment column. The recoveries from lake waters spiked with explosive standard solution ranged from 90.5 to 108.0%. The proposed method is simple, fast, and could be applied successfully to the analysis of explosive residues in contaminated water without any further pretreatment. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1964-z Authors Qian Sun, Key Laboratory of Urban Environment and Health, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen, 361021 China Zuliang Chen, Centre for Environmental Risk Assessment and Remediation, University of South Australia, Mawson Lakes, SA 5095, Australia Dongxing Yuan, State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen, 361005 China Chang-Ping Yu, Key Laboratory of Urban Environment and Health, Institute of Urban Environment, Chinese Academy of Sciences, Xiamen, 361021 China Megharaj Mallavarapu, Centre for Environmental Risk Assessment and Remediation, University of South Australia, Mawson Lakes, SA 5095, Australia Ravendra Naidu, Centre for Environmental Risk Assessment and Remediation, University of South Australia, Mawson Lakes, SA 5095, Australia Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The aim of this study was to screen for the anti-inflammatory components from Houttuynia cordata Thunb (HCT) using an analytical method combining cell membrane chromatography (CMC) with gas chromatography–mass spectrometry (GC–MS). The stationary phase of the CMC employed mouse peritoneal macrophage (PM) cell membranes. We investigated the performance of the PM/CMC-offline-GC–MS method using hydrocortisone (HC) as standard. The method was then applied to the identification of anti-inflammatory components in extracts of HCT. The major component retained by CMC was identified as methyl nonyl ketone (MNK) by GC–MS. In vitro experiments revealed that MNK was able to inhibit LPS-induction of TNF-α, NO, and H 2 O 2 production in a dose-dependent manner. IC 50 values were 3.3, 4.1, and 3.6 μg mL −1 , respectively. The PM/CMC-offline-GC–MS method is an effective screening system for the rapid detection, enrichment, and identification of target components from complex samples. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1926-5 Authors Weifeng Li, School of Medicine, Xi’an Jiaotong University, No. 76 Western Yanta Road, Xi’an, 710061 Shaanxi PR China Xiaofeng Niu, School of Medicine, Xi’an Jiaotong University, No. 76 Western Yanta Road, Xi’an, 710061 Shaanxi PR China Ping Zhou, School of Medicine, Xi’an Jiaotong University, No. 76 Western Yanta Road, Xi’an, 710061 Shaanxi PR China Miao Li, School of Medicine, Xi’an Jiaotong University, No. 76 Western Yanta Road, Xi’an, 710061 Shaanxi PR China Langchong He, School of Medicine, Xi’an Jiaotong University, No. 76 Western Yanta Road, Xi’an, 710061 Shaanxi PR China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A simple, rapid, and selective method to determine the concentration of mildronate in human plasma and urine using ultra performance liquid chromatography–tandem mass spectrometry (UPLC-MS-MS) was developed and validated. The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring mode via electrospray ionization at m/z 147.2–58.0 for mildronate and m/z 147.2–87.8 for the internal standard, carbachol. The UPLC separation was carried out with a UPLC BEH HILIC column. The mobile phase consisted of 0.08% formic acid in 30 mM ammonium acetate solution and acetonitrile (23:77, v/v ). Plasma samples were extracted from plasma by protein precipitation and urine samples were diluted with the mobile phase. The analysis time was 3.5 min for each sample. Linear calibration curves ranged from 0.10 to 100.00 μg mL −1 in human plasma and 0.50 to 600.00 μg mL −1 in urine. The method had been successfully applied to a pharmacokinetic study in healthy volunteers. After single intravenously administration of 250, 500, and 750 mg mildronate, the elimination half-life ( t 1/2 ) were (2.74 ± 0.67), (4.86 ± 0.82) and (5.16 ± 0.77) h, respectively. The t 1/2 for the 250 mg dose did vary significantly with other dosages ( P  〈 0.05), mildronate may have non-linear pharmacokinetics in humans. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-010-1839-8 Authors Li-Jing Cai, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Jun Zhang, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Wen-Xing Peng, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Rong-Hua Zhu, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Jian Yang, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Gang Cheng, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Xiu-Mei Wang, Clinical Pharmaceutical Research Institute, The Second Xiangya Hospital, Central South University, Changsha, 410011 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The properties of two thermally stable organic/inorganic hybrid columns, XTerra MS C 18 and XTerra phenyl were examined at elevated temperatures, using a number of test compounds, including acetophenone derivatives and phenols, with 5 and 10% methanol in water as the mobile phases. The thermodynamics of the separations were examined. The study demonstrated that a low proportion of organic modifier and moderate temperatures gave similar separations to higher temperature with superheated water, potentially reducing stress on the column and analytes. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1966-x Authors Lateefa A. Al Khateeb, Department of Chemistry, Loughborough University, Loughborough Leics, LE11 3TU, UK Roger M. Smith, Department of Chemistry, Loughborough University, Loughborough Leics, LE11 3TU, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    (−)-Ephedrine (ephedrine, EPH) and (+)-ephedrine (pseudoephedrine, PEPH) are metabolized by the liver, but the species of hepatocyte cytochrome P450 (CYP450) responsible is not yet clear. To investigate which subtype of CYP450 is involved in the metabolism of EPH and PEPH, a rapid and reliable reversed-phase ion-pair liquid chromatographic method for simultaneous analysis of EPH and PEPH in rat liver microsomes has been established and validated. Matrine was selected as a suitable internal standard (IS) for calibration. After liquid–liquid extraction of liver microsomal samples with methyl tert -butyl ether, EPH and PEPH were separated on a C 18 reversed-phase column (200 mm × 4.6 mm, 5 μm) with methanol–0.5% sodium dodecyl sulfate–phosphoric acid–triethylamine 60:40:1.25:1 ( v / v ) as mobile phase at a flow rate of 1.0 mL min. Detection was by UV absorbance at 210.5 nm. For both EPH and PEPH, calibration curves were linear over the range 1.5–60.0 μg mL −1 , the limit of quantification was 1.5 μg mL −1 , and intra-day and inter-day variability was 〈10.0%. Average extraction recovery of the two analytes was 〉73%. The validated method was successfully used to study the in-vitro metabolism of EPH and PEPH. In rat liver microsomes induced by dexamethasone, enzyme activity in the metabolism of EPH and PEPH was higher than that for metabolism of phenobarbital and β-naphthoflavone. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-1950-5 Authors Jingling Tang, Department of Pharmaceutics, School of Pharmacy, Harbin Medical University, Harbin, 150086 China Xiaoyan Zhou, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Hongyu Ji, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Na Xu, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Hongmei Liu, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Gongzan Lan, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Linhua Wu, Department of Pharmacy, The Second Affiliated Hospital of Harbin Medical University, Key Laboratory of College in Heilongjiang Province, 157 Baojian Road, Harbin, 150086 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Efficiency in HPLC can be enhanced by increasing the column length and/or decreasing the particle size. The use of high temperature in HPLC has emerged as a valuable tool to overcome the increase in column backpressure when using small packing particles, as it allows for reduction in mobile phase viscosity. In this study, high plate count was obtained by coupling sub-2 μm columns at elevated temperature to reduce the viscosity of the mobile phase, thus reducing the column backpressure. At 80 °C, up to three columns of 15 cm × 4.6 mm I.D. packed with 1.8 μm particles could be coupled generating ~84,000 theoretical plates for the last eluting compound. The number of theoretical plates was increased on average by a factor of ~3.6 when three columns were coupled at 80 °C compared with one column at 30 °C. The relationships between separation efficiency and column length were examined using Van Deemter plots constructed at 30 °C and 80 °C for different column lengths. The advantages of using coupled columns in combination with elevated temperature for the environmental analysis were illustrated using test mixtures comprised of eight sulfonamides separated on one column at 30 °C and three coupled columns at 80 °C by isocratic elution. Sample clean up was carried out by employing solid-phase extraction (SPE) using Oasis HLB cartridges. The method developed was validated based on parameters such as linearity, precision, accuracy, detection and quantification limits. Recoveries generally ranged from 71.7 to 99% (with the exception of sulfanilamide), with standard deviations not higher than 4.7%. The detection limits of the method ranged from 0.6–2 μg L −1 , while limits of quantification were in the range 2–6.7 μg L −1 with UV detection. Content Type Journal Article Pages 1-9 DOI 10.1007/s10337-011-2038-y Authors Heba Shaaban, Department of Chemistry, University of Waterloo, Waterloo, ON N2L 3G1, Canada Tadeusz Górecki, Department of Chemistry, University of Waterloo, Waterloo, ON N2L 3G1, Canada Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A rapid, sensitive and accurate high performance liquid chromatography method using tandem mass spectrometry detection for hydralazine in BALB/C mouse plasma and brain was developed and validated. The method involved a derivatization with 2,4-pentanedione at 50 °C for 1 h, and a step of solid phase extraction to purify and concentrate hydralazine derivative. Chromatographic separation was carried out on an Agilent ZORBAX SB-C18 column by elution with methanol–0.01 mol L −1 ammonium acetate (60:40, v/v ). The multiple reaction monitoring transition used for quantification was m/z 225.2 → 129.5 in the electrospray positive ionization mode. Good linearity was obtained over the concentration range of 10–200 ng mL −1 . The limits of detection were 0.49 and 1.05 ng mL −1 for hydralazine in mouse plasma and brain, respectively. The limits of quantitation were 1.5 and 3.18 ng mL −1 for hydralazine in mouse plasma and brain, respectively. Sample analysis time was 6 min including sample separation. The method was successfully applied to a pharmacokinetic study following intraperitoneal injection of hydralazine in BALB/C mice at the dose of 20 mg kg −1 . Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-2006-6 Authors Yanying Liu, Bioanalytical Laboratory, Shantou University Medical College, Xin Ling Road 22, Shantou, 515041 Guangdong, China Hui Li, Bioanalytical Laboratory, Shantou University Medical College, Xin Ling Road 22, Shantou, 515041 Guangdong, China Hongjun Luo, Bioanalytical Laboratory, Shantou University Medical College, Xin Ling Road 22, Shantou, 515041 Guangdong, China Zhexuan Lin, Bioanalytical Laboratory, Shantou University Medical College, Xin Ling Road 22, Shantou, 515041 Guangdong, China Wenhong Luo, Bioanalytical Laboratory, Shantou University Medical College, Xin Ling Road 22, Shantou, 515041 Guangdong, China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Picroside II is one of the main active constituents of Picrorhiza kurroa, which has hepatoprotective, anticholestatic, antioxidant, and immune-modulating activity. To gain an understanding of the biotransformation of picroside II in vivo, liquid chromatography – electrospray ionization ion-trap mass spectrometry (LC–ESI–IT–MS) was used to investigate the metabolism of picroside II in rats after intravenous administration of a single dose. This method could simultaneously determine picroside II and its metabolites in rat bile. The bile samples were purified by use of a C 18 solid-phase extraction (SPE) cartridge and were separated on a Hypersil ODS2 C 18 analytical column. Two phase II metabolites of picroside II in rat bile were characterized, and elucidation of their structures was performed by comparing changes in molecular masses (Δ M ), retention times, and MS 2 spectral patterns of metabolites with those of the parent drug. Two metabolites identified for the first time in this research were glucuronide and sulfate conjugates. Content Type Journal Article Pages 1-10 DOI 10.1007/s10337-011-2002-x Authors Tingting Li, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Qiaoling Yu, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Deen Han, Department of Tradition Chinese Medicine, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Ying Zhao, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Di Zhao, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Hui Ji, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Xijing Chen, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Ning Li, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Zhixia Qiu, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Yi Zheng, School of Pharmacy, China Pharmaceutical University, Nanjing, 210009 Jiangsu, People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Electrospun polystyrene (PS) nanofibers (130–500 nm) incorporating a potassium salt of imidazole-1-carbodithioate were evaluated as potential sorbents for the pre-concentration of a model organochlorine pesticide; 1,1-dichloro-2,2bis-(4-chlorophenyl)ethylene (DDE). The efficiencies of DDE (0.25–1.0 μg L −1 ) adsorption by the nanofiber sorbent followed by desorption employing pressurized hot water extraction (PHWE) were investigated and monitored using gas chromatography with electron capture detection (GC-ECD). Parameters such as time, temperature and pressure of extraction, sample volume, DDE concentration and sorbent mass were optimized. The maximum adsorption of DDE (0.50 μg L −1 ) on electrospun PS and carbodithioate incorporated PS nanofibers was at 43.7 and 94.6%, respectively, in 20 min. Incorporation of carbodithiote doubled the adsorption efficiency of PS and achieved LOD of 0.000234 μg L −1 for DDE. The optimal DDE desorption on the PHWE system was 93.8% in 10 min. It would seem that the use of electrospun nanofibers as sorbent material with subsequent desorption by PHWE has great potential and thus warrants further investigations. This approach as it uses water as an extraction solvent for an organochlorine pesticide provides an opportunity to eliminate organic solvents, especially for procedures aimed at monitoring organic pollutants in the environment. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-1989-3 Authors David Adeyemi, Department of Chemistry, Rhodes University, P O Box 94, Grahamstown, 6140 South Africa Janes Mokgadi, Department of Chemistry, Rhodes University, P O Box 94, Grahamstown, 6140 South Africa James Darkwa, Department of Chemistry, University of Johannesburg, P.O Box 524, Auckland Park, South Africa Chimezie Anyakora, Department of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Lagos, Lagos, Nigeria Grace Ukpo, Department of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Lagos, Lagos, Nigeria Charlotta Turner, Department of Chemistry, Center for Analysis and Synthesis, Lund University, 221 00 Lund, Sweden Nelson Torto, Department of Chemistry, Rhodes University, P O Box 94, Grahamstown, 6140 South Africa Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    An online dynamic pH junction method has been proposed for sensitive determination of benzoic acid (BA) and sorbic acid (SA) by capillary electrophoresis (CE). It was based on the decreased mobility of the analytes when they migrated from sample zone with low pH to background electrolytes with high pH. Under optimized conditions, the limits of detection (S/N = 3) of BA and SA were 0.03 and 0.02 mg L −1 , respectively. According to the permitted limits of BA and SA in food (GB2760), the samples can be diluted about 2,000–20,000-folds to estimate whether the contents of BA and SA are in the safety range. Beverage, vinegar and fruit jam samples were analyzed after simple dilution, and the results were satisfactory with the recoveries in the range of 91–108%. The whole analysis process needs about only 10 min, which is much faster than the method of liquid–liquid extraction followed by CE determination. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2009-3 Authors Xinfeng Zhang, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu, 610059 Sichuan, China Shuxia Xu, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu, 610059 Sichuan, China Yonghua Sun, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu, 610059 Sichuan, China Yanyan Wang, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu, 610059 Sichuan, China Cheng Wang, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu, 610059 Sichuan, China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: 60th Birthday of Professor Boguslaw Buszewski Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-2121-4 Authors Renata Gadzała-Kopciuch, Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin St, 87 100, Toruń, Poland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A simple and sensitive liquid chromatography with ultraviolet detection (LC–UV) method was developed for the determination of three impurities with a content over 0.1% ( w/w ) in technical triadimefon. A Gemini C 18 column (5 μm, 250 mm × 4.6 mm i.d.) was used for the chromatographic separations. The samples were separated by gradient elution with water (solvent A) and methanol (solvent B) using the following conditions: 70% A isocratic for 12 min, linear to 0% A within 8 min, and isocratic for 10 min at 0% A with a flow rate of 1.0 mL min −1 . Chromatograms were recorded at an absorption wavelength of 280 nm. The chromatographic resolutions between triadimefon and its potential impurities A, B, and C were greater than 3. The developed LC method was validated with respect to linearity, accuracy, precision, and robustness. This method was successfully applied to analyze the impurities in commercial technical triadimefon. In addition, the structures of the three impurities were identified to be (A) 4-chlorophenol, (B) 1-(2,4-dichlorophenoxy)-3,3-dimethyl-1-(1 H -1,2,4-triazol-1-yl)-2-butanone, and (C) 1,1-bis(4-chlorophenoxy)-3,3-dimethyl-2-butanone. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2131-2 Authors Meng-xiang Su, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, 210009 China Lin-jun You, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, 210009 China Bin Di, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, 210009 China Lan-jin Qu, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, 210009 China Tai-jun Hang, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, 210009 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In the present paper, we present our results from studies where the electrode solutions were separated from the carrier with the polytetrafluoroethylene-based membranes (Nafion ® ). We achieved a 40-fold decrease of the average ionic strength in the gel and a twofold lowering of the current already during the first 30 min from the start of IEF, as compared to the routinely employed method. The change of these parameters made it possible to carry out the electrophoresis under conditions considerably closer to steady state, and to achieve a sharp protein separation and shortening of the duration of the process. The comparative analysis of the electrophoretic parameters in question proved that the basis for this newly developed improvement of the method is the selective restriction of the processes of migration and diffusion in the whole electrophoretic system, due to the specific properties of the semi-permeable membrane Nafion ® . Content Type Journal Article Category Original Pages 1-8 DOI 10.1007/s10337-011-2158-4 Authors Cyrill L. Naydenov, Department of Chemistry and Biochemistry, Medical University Sofia, 2 Zdrave Str., 1431 Sofia, Bulgaria Evgeni P. Kirazov, Institute of Experimental Morphology and Anthropology With Museum, Bulgarian Academy of Sciences, Acad. G. Bonchev Str. Bl. 25, 1113 Sofia, Bulgaria Simeon A. Boyadjiev, Section of Genetics, Department of Pediatrics, University of California Davis, Sacramento, CA 95618 USA Ludmil P. Kirazov, Institute of Experimental Morphology and Anthropology With Museum, Bulgarian Academy of Sciences, Acad. G. Bonchev Str. Bl. 25, 1113 Sofia, Bulgaria Valentin S. Lozanov, Department of Chemistry and Biochemistry, Medical University Sofia, 2 Zdrave Str., 1431 Sofia, Bulgaria Vanio I. Mitev, Department of Chemistry and Biochemistry, Medical University Sofia, 2 Zdrave Str., 1431 Sofia, Bulgaria Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The hepatitis B surface antigen manufactured by recombinant DNA technology is extracted from the culture media by density gradient centrifugation using cesium salts. Cesium is considered to be toxic, because it affects active ion transport by blocking potassium channels. The residual trace levels of cesium in hepatitis B vaccine samples are determined by suppressed ion chromatography. Hepatitis B vaccines contain various buffer salts, aluminum-containing adjuvants, proteins and traces of iron. The polyvalent cations (Al 3+ , Fe 3+ ) and proteins degrade the chromatographic performance in terms of decreased retention time and poor reproducibility. Different sample preparation approaches were evaluated with the aim of eliminating these foulants: (1) filtration, (2) digestion and (3) digestion-protein precipitation. Quantitative elimination of these foulants was achieved in the digestion-protein precipitation sample clean-up approach. Cesium was separated on the IonPac CS17 column with suppressed conductivity detection. The results of the ion chromatography (IC) method were compared with ICP-MS analysis. The precision of determination was better than 6.5% (relative standard deviation) with a method detection limit of 45 ng mL −1 . The expanded uncertainty in the measurement at 95% confidence level (coverage factor 2) is better than 16.3%. Content Type Journal Article Category Original Pages 1-7 DOI 10.1007/s10337-011-2161-9 Authors Kulamani Dash, National Centre for Compositional Characterization of Materials (CCCM), Bhabha Atomic Research Centre, ECIL Post, Hyderabad, 500062 India Shanmugam Thangavel, National Centre for Compositional Characterization of Materials (CCCM), Bhabha Atomic Research Centre, ECIL Post, Hyderabad, 500062 India Lori Rastogi, National Centre for Compositional Characterization of Materials (CCCM), Bhabha Atomic Research Centre, ECIL Post, Hyderabad, 500062 India Shrinivas M. Dhavile, National Centre for Compositional Characterization of Materials (CCCM), Bhabha Atomic Research Centre, ECIL Post, Hyderabad, 500062 India Jayaraman Arunachalam, National Centre for Compositional Characterization of Materials (CCCM), Bhabha Atomic Research Centre, ECIL Post, Hyderabad, 500062 India Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A novel porous monolithic column was prepared by in situ free-radical polymerization in a 50 mm × 4.6 mm i.d. stainless steel column at 60 °C, which was in the presence of 2,2′-azobisisobutyronitrile (AIBN) as initiator, with N -isopropylacrylamide (NIPAAm) and methacrylic acid (MAA) as monomers, ethylene dimethacrylate (EDMA) as crosslinker, methanol and dodecanol as a porogenic solvent. The micrographs of monolithic column were characterized by scanning electron microscopy (SEM) and pore size distribution was determined by mercury intrusion porosimetry. The pressure drop across the columns was measured as a function of flow rate using water and methanol. The result showed that the monolithic columns had an excellent permeability and a high mechanical stability. Moreover, the influence of several parameters which were column temperature, mobile phase composition and flow rate was investigated in the separation of mixtures of nifedipine and nisoldipine. In addition, the effects of type and concentration of buffer on the elution of human plasma protein were investigated. The results showed that a better peak shape was obtained at higher temperature and larger flow rate on the monolithic column. Content Type Journal Article Category Original Pages 1-7 DOI 10.1007/s10337-011-2169-1 Authors Yanhui Duan, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Haiyan Liu, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Jia Li, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Junjie Ma, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Yanzhao Gu, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Cuihong Yan, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Gengliang Yang, Hebei Province Key Laboratory of Pharmaceutical Quality Control, College of Pharmacy, Hebei University, Baoding, 071002 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Chain conformation and local rigidity of two isomerized polyimides (PIs), poly(6FDA/3,3′-DMB) and poly(6FDA/2,2′-DMB) in dimethyl formamide (DMF) with either 0.1 M LiBr or 3.1 mM tetrabutylammonium bromide at 35 °C, are investigated. Size exclusion chromatography (SEC) coupled with multi-angle laser light scattering detector, viscometer, and differential refractive index detector was used. The scaling exponents α and ν related to conformation are estimated from the above results. The values of α and ν for poly(6FDA/3,3′-DMB) are 0.68 ± 0.01 and 0.54–0.55 ± 0.01, respectively. The values of α and ν for poly(6FDA/2,2′-DMB) are 0.65 ± 0.02 and 0.55 ± 0.01, respectively, which indicate that both PIs in DMF have a random coil conformation. In particular, poly(6FDA/3,3′-DMB) exhibits more extended conformation than that of poly(6FDA/2,2′-DMB). Parameters related to chain flexibility of polymers, including persistence length l p , shift factor M L (relative molecular weight per unit contour length), and backbone diameter d are evaluated from the relationship between intrinsic viscosity and molecular weight based on the wormlike continuous cylinder model. The three parameters ( l p , M L , and d ) indicate that the two samples are flexible chains with local rigidity, and poly(6FDA/3,3′-DMB) is slightly stiffer than poly(6FDA/2,2′-DMB). In addition, influence of salt types on the parameters is also discussed. Content Type Journal Article Category Original Pages 1-9 DOI 10.1007/s10337-011-2159-3 Authors Guihua Liu, State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun, 130022 People’s Republic of China Xuepeng Qiu, Polymer Composites Engineering Laboratory, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun, 130022 People’s Republic of China Shuqin Bo, State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun, 130022 People’s Republic of China Xiangling Ji, State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 5625 Renmin Street, Changchun, 130022 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Capillary electrophoresis (CE) coupled to a capacitively coupled contactless conductivity detector (C 4 D) was used for the determination in a single analysis of a pharmaceutical drug and its counter-ion. Dual-opposite end injection (DOI) was used to introduce hydrodynamically the analytes at each end of the capillary. No modification of the commercial apparatus is required. After applying the voltage, the cations and anions migrate from each end of the capillary in opposite directions toward the detector placed near the cathode outlet. The electrophoretic conditions were initially developed with three test drugs (chlorpheniramine maleate, metoprolol tartrate, clomiphene citrate) and then applied to two Vinca alkaloids (catharanthine sulfate, vinorelbine ditartrate). The 10 mM histidine–50 mM acetic acid buffer (pH 4.1)–methanol 90:10 ( v/v ) electrolyte was suitable for the analysis of these high or medium mobile anions by CE–C 4 D due to its low conductivity background and high buffer capacity. Finally, the CE procedure developed was successfully validated for catharanthine sulfate. The method developed herein is fast (〈10 min) and accurate (repeatability on migration time 〈 0.6% and peak areas 〈 1.3%, n  = 6). Content Type Journal Article Category Original Pages 1-8 DOI 10.1007/s10337-011-2154-8 Authors C. Lopez, Institut de Chimie Organique et Analytique, Université d’Orléans, CNRS, BP 6759 rue de Chartres, FR 2708-UMR 6005, 45067 Orléans, France R. Nehme, Institut de Chimie Organique et Analytique, Université d’Orléans, CNRS, BP 6759 rue de Chartres, FR 2708-UMR 6005, 45067 Orléans, France B. Claude, Institut de Chimie Organique et Analytique, Université d’Orléans, CNRS, BP 6759 rue de Chartres, FR 2708-UMR 6005, 45067 Orléans, France Ph. Morin, Institut de Chimie Organique et Analytique, Université d’Orléans, CNRS, BP 6759 rue de Chartres, FR 2708-UMR 6005, 45067 Orléans, France J. P. Max, Département de Chimie Analytique, Institut de Recherche Pierre Fabre, 17 avenue Jean Moulin, 81106 Castres, France R. Pena, Département de Chimie Analytique, Institut de Recherche Pierre Fabre, 17 avenue Jean Moulin, 81106 Castres, France M. Pelissou, Département de Chimie Analytique, Institut de Recherche Pierre Fabre, 17 avenue Jean Moulin, 81106 Castres, France J. P. Ribet, Département de Chimie Analytique, Institut de Recherche Pierre Fabre, 17 avenue Jean Moulin, 81106 Castres, France Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In the present studies, a simple rapid ultra performance liquid chromatography (UPLC) method with UV detection for the simultaneous determination of cortisol, cortisone and 6β-hydroxycortisol in human urine was developed. The three analytes and the internal standard dexamethasone were separated on a Waters Acquity UPLC-Tunable UV system with an Acquity UPLC BEH C18 column (50 × 2.1 mm ID, 1.7 μm) using a gradient elution of methanol and water (containing 0.01% formic acid) with a run time of 7 min. The method was accurate and precise, over the ranges of 5–200 ng mL −1 for cortisol, and 10–1,000 ng mL −1 for both cortisone and 6β-hydroxycortisol, and showed good linearity ( r 2  〉 0.999). This method was applied for the measurement of cortisol, cortisone and 6β-hydroxycortisol in samples collected over different periods as a tool to assess the activity of CYP3A and 11β-hydroxysteroid dehydrogenase type 2 enzymes. Content Type Journal Article Category Short Communication Pages 1-5 DOI 10.1007/s10337-011-2162-8 Authors Yajie Xiao, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Sze Wa Chan, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Miao Hu, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Tanya Ten Wah Chu, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Benny Siu Pong Fok, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Emily Wai Mei Poon, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Brian Tomlinson, Department of Medicine and Therapeutics, Prince of Wales Hospital, The Chinese University of Hong Kong, Shatin, NT, Hong Kong, China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A high-performance liquid chromatographic/tandem mass spectrometric method was developed for the determination of the major bioactive flavonolignans in silymarin, a herbal remedy extracted from the milk thistle Silybum marianum . In this study, eight active components of silymarin with the same elemental composition, including silychristins A and B, silydianin, silybin A and B, isosilybin A and B and an unknown compound were completely separated. Furthermore, three additional components were detected and partly separated; presumably two silybin stereoisomers and one isosilybin stereoisomer. The collision-induced dissociation (CID) MS/MS spectra of these silymarin constituents were studied: the spectral similarity values of the component pairs were determined, and simple criteria were found for distinguishing the components. Content Type Journal Article Category Short Communication Pages 1-6 DOI 10.1007/s10337-011-2163-7 Authors Ákos Kuki, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary Lajos Nagy, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary György Deák, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary Miklós Nagy, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary Miklós Zsuga, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary Sándor Kéki, Department of Applied Chemistry, University of Debrecen, Debrecen, 4032 Hungary Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Determination of the levels of 1-octacosanol is important in food stuff for the study of its pharmacological activities and health benefits. In this study, a novel, simple and fast internal standard method for the non-derivatization ultra-performance liquid chromatographic determination of 1-octacosanol in raw materials and health products was developed and validated based on evaporative light scattering detection. The linearity ( r 2  〉 0.998), recovery (99.1–100.2%, RSD 〈2.7%), intra- and inter-day precision (RSD 〈3.8%), limit of detection (1.0 mg/L), limit of quantification (2.2 mg/L) of the 1-octacosanol were determined. The method was successfully applied to nine real 1-octacosanol products. The results of analyses had close agreement with the labeled claims of 1-octacosanol content in these products. Compared with the classical gas chromatography method, the developed method was simpler, faster and more environmentally friendly due to avoiding any derivatization step. This protocol represents a rapid and feasible method for quality control of 1-octacosanol products. Content Type Journal Article Category Full Short Communication Pages 1-4 DOI 10.1007/s10337-011-2166-4 Authors Xiaofeng Xue, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Lanzhen Chen, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Jinhui Zhou, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Liming Wu, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Yi Li, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Fang Chen, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Jinzhen Zhang, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Jing Zhao, Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Fish oil is considered a healthy food due to the presence of large amounts of polyunsaturated fatty acids (PUFAs), especially in the form of n - 3 fatty acids 5,8,11,14,17-eicosapentaenoic acid (20:5 n - 3 ; EPA) and 4,7,10,13,16,19-docosahexaenoic acid (22:6 n - 3 ; DHA). However, fish oil is known to contain many other PUFAs, some of which are uncommon and whose bioactivity is scarcely investigated. In this study, we isolated the rare PUFA 6,9,12,15-hexadecatetraenoic fatty acid (16:4 n - 1 ) which bears a double bond on the terminal carbon from fish oil in form of its methyl ester. We used high-speed counter-current chromatography (HSCCC) for the fractionation of 500 mg-portions of fatty acid methyl esters prepared from a fish oil capsule and investigated the fractions by GC/MS. Twenty-eight 13-mL fractions were collected and fatty acid methyl esters were detected in fractions 11–23. The elution was carried out in normal phase mode, providing the long-chained saturated and monoenoic fatty acids first. More than 100 fatty acids ranging from 10:0 to 26:0 could be identified in the HSCCC fractions, and most of them were polyunsaturated. The reproducibility of the HSCCC method was shown by repeated injection of the fish oil and the fractions containing 6,9,12,15-hexadecatetraenoic fatty acid (16:4 n - 1 ). The late eluting 16:4 n - 1 methyl ester was isolated in pure form and its structure was verified. Content Type Journal Article Category Original Pages 1-6 DOI 10.1007/s10337-011-2155-7 Authors Danli Li, Institute of Food Chemistry (170b), University of Hohenheim, Garbenstr. 28, 70599 Stuttgart, Germany Markus Schröder, Institute of Food Chemistry (170b), University of Hohenheim, Garbenstr. 28, 70599 Stuttgart, Germany Walter Vetter, Institute of Food Chemistry (170b), University of Hohenheim, Garbenstr. 28, 70599 Stuttgart, Germany Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: T.S.S. Dikshith: Handbook of Chemicals and Safety Content Type Journal Article Category Book Review Pages 1-1 DOI 10.1007/s10337-011-2153-9 Authors Ken Jones, Knutsford, Cheshire, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The late location of entrapped victims in collapsed buildings is the main reason of high mortality during urban search and rescue (USaR) operations after natural or man-made disasters. Consequently, an effort is currently being made to develop proper rescue searching tools that could improve the early location of trapped casualties. In this context, the knowledge of human scent profile and its behavior in the disaster environment is crucial. The main goal of this study was to investigate the suitability of the ion mobility spectrometry (IMS) for the quantitative monitoring of specific urine-borne volatile members of human scent interacting with the materials of collapsed dwellings. For this purpose, an ion mobility spectrometer with β-radiation source ( 63 Ni) and an in-house made filling chamber mimicking the entrapment scene were employed. In preliminary experiments, quartz sand was used as imitating debris material. The experimental setup was used to investigate the permeation properties of two very promising urine-borne species, 2-heptanone and n -octanal, under the influence of two crucial operational factors; the size of quartz grain and the quartz layer thickness. 2-heptanone was found to penetrate through quartz layer by approximately a factor 4 faster than n -octanal. The twofold and threefold increase of quartz sand thickness lengthened the permeation times on average three and seven times for n -octanal, and three and five times for 2-heptanone. The presented experimental setup can be considered as a useful tool suitable for investigating the interactions of urine markers with the debris materials in the entrapment scene. However, further investigations involving different debris materials (e.g. concrete, brick, cement, wood, plastic, glass) and other urine-borne species are necessary, prior selecting a set of volatile organic compounds (VOCs) that will support the early location method of entrapped victims. Content Type Journal Article Category Original Pages 1-6 DOI 10.1007/s10337-011-2157-5 Authors P. Mochalski, Breath Research Institute of the Austrian Academy of Sciences, Rathausplatz 4, 6850 Dornbirn, Austria M. Buszewska, Breath Research Institute of the Austrian Academy of Sciences, Rathausplatz 4, 6850 Dornbirn, Austria A. Agapiou, National Technical University of Athens (NTUA), School of Chemical Engineering, Sector I, 9 Iroon Polytechniou Street, 15773 Athens, Greece M. Statheropoulos, National Technical University of Athens (NTUA), School of Chemical Engineering, Sector I, 9 Iroon Polytechniou Street, 15773 Athens, Greece B. Buszewski, Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, Gagarina Str. 7, 87100 Torun, Poland A. Amann, Breath Research Institute of the Austrian Academy of Sciences, Rathausplatz 4, 6850 Dornbirn, Austria Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Confirmation of identity of forensically relevant compounds, such as drugs of abuse, is a necessary step in medico-legal event controls of people involved in crimes, workplace accidents and driving under the influence of drugs (DUID). Plasma is a useful medium in determining the short-term use of illicit drugs and its analysis is mandatory in the case of DUID in many countries. Urine has been the sample of choice for monitoring drug abuses in workplaces and is subjective to strict regulations. The aim of this work was the development of a fast and reliable confirmatory method for the determination of multiple drugs of abuse belonging to different chemical and toxicological classes: amphetamine, methamphetamine, methylenedioxyamphetamine, methylenedioxyethylamphetamine, methylenedioxymethylamphetamine, cocaine, benzoylecgonine, ketamine, phencyclidine, psilocybin and mescaline. The procedure involves very rapid steps of sample preparation with use of automated micro-SPE. The quantitative analysis is performed by LC–ESI-MS/MS with chromatographic Core Shell™ column. The method has been fully validated according to SOFT-AAFS guidelines and applied as confirmatory analysis for real samples coming from agro-industry employees. Content Type Journal Article Category Full Short Communication Pages 1-9 DOI 10.1007/s10337-011-2156-6 Authors Sabino Napoletano, Department of Chemistry, Sapienza University of Rome, P.le A. Moro 5, 00185 Rome, Italy Camilla Montesano, Department of Chemistry, Sapienza University of Rome, P.le A. Moro 5, 00185 Rome, Italy Dario Compagnone, Department of Food Science, University of Teramo, Via Carlo Lerici 1, 64023 Mosciano Stazione (TE), Italy Roberta Curini, Department of Chemistry, Sapienza University of Rome, P.le A. Moro 5, 00185 Rome, Italy Giuseppe D’ascenzo, Department of Chemistry, Sapienza University of Rome, P.le A. Moro 5, 00185 Rome, Italy Claudia Roccia, Department of Chemistry, Sapienza University of Rome, P.le A. Moro 5, 00185 Rome, Italy Manuel Sergi, Department of Food Science, University of Teramo, Via Carlo Lerici 1, 64023 Mosciano Stazione (TE), Italy Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A highly porous fiber coating material was prepared and functionalized with 3-amino propyl triethoxysilane (APTES) on hexagonally ordered nanoporous silica (SBA-15). Applicability of this coating was assessed employing a laboratory made solid-phase microextraction (SPME) device and gas chromatography–mass spectrometry for the simultaneous sampling and determination of trace polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions. A one at the time optimization strategy was applied to investigate and optimize important extraction parameters such as extraction temperature, extraction time, ionic strength and sonication time. In the optimum conditions, the relative standard deviations for deionized water, spiked with selected PAHs were between 3.3 and 7.7% ( n  = 3), and detection limits for the studied compounds were 4.2 and 26.1 pg mL −1 . No significant change was observed in the extraction efficiency of the new SPME fiber, over 50 extractions. The proposed method was successfully applied to the extraction and determination of PAHs in the waste water samples. Content Type Journal Article Category Original Pages 1-9 DOI 10.1007/s10337-011-2146-8 Authors Mohammad Bagher Gholivand, Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran Mir Mahdi Abolghasemi, Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran Peyman Fattahpour, Department of Organic Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: John A. Conkling and Christopher J. Mocella: Chemistry of Pyrotechnics: Basic Principles and Theory Content Type Journal Article Category Book Review Pages 1-2 DOI 10.1007/s10337-011-2136-x Authors Edward R. Adlard, Burton, South Wirral, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Platycosides, main pharmacological effective compounds, are known to have several biological activities, including anti-obesity, anti-cancer and anti-diabetes. Although enzymatic preparation of platycosides was considered as effective method to obtain them, few analytical methods have been reported on process control. In the present study, we developed an application of reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous determination of six platycosides during the process of enzymatic preparation of deapio-platycodin D (dPD) and platycodin D (PD). The method employed a Hypersil ODS2 analytical column (250 × 4.6 mm I.D., 5 μm) coupled with UV detector at 210 nm with flow rate of 1.0 mg mL −1 . A step gradient of acetonitrile–water (v/v) was applied, leading to a sample analysis of 60 min. The method was validated in terms of linearity, sensitivity, precision and accuracy. The correlation coefficients ( R 2 ) for calibration curves of platycosides were in the range of 0.9995–1.0 when the linearity range was from 0.85 to 10.2 mg mL −1 . The proposed RP-HPLC method was successfully applied to the analysis of enzymatic preparation study and the recoveries of platycosides were in the range of 96.22–102.56% with RSD 〈3.3%. The method could be of use for rapid and routine evaluation of the quantity of platycosides during the enzymatic preparation process. Content Type Journal Article Category Original Pages 1-6 DOI 10.1007/s10337-011-2140-1 Authors Wei Li, College of Chinese Medicinal Materials, Jilin Agricultural University, Xincheng Street, No. 2888, Changchun, 1300118 People’s Republic of China Ming Zhang, Norman Bethune College of Medicine, Jilin University, Changchun, 130021 People’s Republic of China Zi Wang, College of Chinese Medicinal Materials, Jilin Agricultural University, Xincheng Street, No. 2888, Changchun, 1300118 People’s Republic of China Ying Ping Wang, Institute of Special Wild Economic Animals and Plant, CAAS, Jilin, 132109 People’s Republic of China Yi-nan Zheng, College of Chinese Medicinal Materials, Jilin Agricultural University, Xincheng Street, No. 2888, Changchun, 1300118 People’s Republic of China Jing Zhang, College of Chinese Medicinal Materials, Jilin Agricultural University, Xincheng Street, No. 2888, Changchun, 1300118 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Eli Grushka and Nelu Grinberg (Eds.): Advances in Chromatography, Volume 49 Content Type Journal Article Category Book Review Pages 1-2 DOI 10.1007/s10337-011-2134-z Authors Peter A. Sewell, Ormskirk, Lancashire, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Monzer Fanun (Ed.): Colloids in Drug Delivery Content Type Journal Article Category Book Review Pages 1-1 DOI 10.1007/s10337-011-2135-y Authors Neil C. Henney, The School of Pharmacy and Biomolecular Sciences, Liverpool John Moores University, Liverpool, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Monika Waksmundzka-Hajnos and Joseph Sherma (Eds.): High Performance Liquid Chromatography in Phytochemical Analysis Content Type Journal Article Pages 1-1 DOI 10.1007/s10337-011-2106-3 Authors Edward R. Adlard, Burton, South Wirral, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The α 1A -adrenoceptor (α 1A -AR) plays an important role in drug discovery and development. An online analytical method coupling prostate cell membrane chromatography (CMC) with high-performance liquid chromatography/mass spectrometry (LC/MS) was established to screen α 1A -AR antagonists in traditional Chinese medicines (TCMs). The prostate cell membrane stationary phase (CMSP) was prepared by immobilizing the prostate cell membrane onto the surface of the silica carrier. The surface and chromatographic characteristics of the prostate CMSP were studied using tamsulosin as a model molecule. The retained fractions from the prostate CMC were analyzed by transferring them to an LC/MS system through a 10-port switch valve. The active component, which could act on the prostate cell membrane and receptor on it (such as α 1A -AR), was determined using a displacement experiment. The results indicated that liensinine, isoliensine, and neferine from Lotus Plumule exhibited similar retention characteristics to the control drug tamsulosin when utilizing the prostate CMC model. This new prostate CMC–LC/MS method is applicable for screening α 1A -AR antagonists from TCMs such as Lotus Plumule and could be employed as a drug discovery tool for natural medicinal herbs. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2085-4 Authors Jing Ren, School of Medicine, Xi’an Jiaotong University, Xi’an, 710061 China Dongdong Dai, School of Medicine, Xi’an Jiaotong University, Xi’an, 710061 China Hui Du, School of Medicine, Xi’an Jiaotong University, Xi’an, 710061 China Meng Sun, School of Medicine, Xi’an Jiaotong University, Xi’an, 710061 China Sicen Wang, School of Medicine, Xi’an Jiaotong University, Xi’an, 710061 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Erratum to: Simultaneous Qualitative Analysis of Coumarins in the Rhizome of Angelica polymorpha Maxim. by LC–DAD–ESI–MS Content Type Journal Article Pages 1-1 DOI 10.1007/s10337-011-2074-7 Authors Na Liu, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Nengjiang Yu, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Jin Li, Tianjin University of Traditional Chinese Medicine, Tianjin, 300193 People’s Republic of China Yu Yang, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Jifen Guo, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Yimin Zhao, Beijing Institute of Pharmacology and Toxicology, Beijing, 100850 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    An offline two-dimensional RP/RPLC system was developed for the separation of components in Dracaena cochinchinensis (Lour.) S.C.Chen xylem containing a resin that is an important raw material in Chinese traditional medicine. In this separation method, a CN-column was used in the first dimension and a C 18 -column in the second dimension. Fractions collected from the CN-column were resolved into many additional components, which indicated that the two-dimensional RP/RPLC system based on the CN- and C 18 -columns is orthogonal. The method provides higher peak capacity and better resolution. It is suitable for the analysis of complex samples such as those found in traditional Chinese medicines. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2065-8 Authors Zhongqiu Teng, School of Life Science, Beijing Institute of Technology, Beijing, 100081 People’s Republic of China Rongji Dai, School of Life Science, Beijing Institute of Technology, Beijing, 100081 People’s Republic of China Weiwei Meng, School of Life Science, Beijing Institute of Technology, Beijing, 100081 People’s Republic of China Yan Chen, Beijing BIT&GY Pharmaceutical R&D Co.Ltd., Beijing, 100081 People’s Republic of China Yulin Deng, School of Life Science, Beijing Institute of Technology, Beijing, 100081 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Enantioseparations of methyl mandelate (MMA) and methyl α -cyclohexylmandelate (MCHMA) on permethylated β -cyclodextrin (PM- β -CD) chiral stationary phase were explored in detail using high-performance liquid chromatography. The influence of the concentration of organic modifiers, along with the column temperature, was studied. In addition, the thermodynamics parameters of the enantioseparations were determined to discuss driven power in the process of enantioseparations. In addition, host−guest complexation of PM- β -CD with MMA enantiomers was simulated by quantum mechanics PM3 method for understanding the chiral recognition mechanism. The experimental results showed that the retention factor ( k ), separation factor ( α ), and resolution factor (Rs) for MMA and MCHMA resolved on the PM- β -CD column all generally decreased with the increase of methanol content, which indicated that the main chiral recognition mechanism is that the hydrophobic portions of MMA and MCHMA are included in the hydrophobic cavity of PM- β -CD to form inclusion complexes. In addition, there is an excellent linear relationship between the logarithms of retention factors ( k ) of MMA and MCHMA enantiomers and 1/ T . It was demonstrated that the enantioseparations of MMA and MCHMA on PM- β -CD chiral column were enthalpy-driven processes. The modeling results can correctly predict the retention order and provide an atomistic account of how chiral discrimination takes place. It is found that the most stable structure of ( R )-MMA/PM- β -CD complex is different with that of ( S )-MMA/PM- β -CD complex. The main driving forces responsible for chiral recognition are hydrophobic forces and weak hydrogen bondings. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2069-4 Authors Jie-hua Shi, College of Pharmaceutical Sciences, Zhejiang University of Technology, Hangzhou, 310032 China Zuo-jing Ding, College of Pharmaceutical Sciences, Zhejiang University of Technology, Hangzhou, 310032 China Ying Hu, College of Pharmaceutical Sciences, Zhejiang University of Technology, Hangzhou, 310032 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    2-Amino-1-methyl-6-phenylimidazo[4,5- b ]pyridine (PhIP) is an abundantly present heterocyclic aromatic amine which is found to be carcinogenic in rodents, mice and rats. The biotransformation of PhIP is extensive and involves both the formation of bioactivated as well as detoxification metabolites. In order to understand its carcinogenicity, the metabolism of PhIP needs to be studied. Numerous metabolites of PhIP have been described but, so far, assays for their quantitative determination in biological matrices are scarce. We present the development and application of an assay, using reversed phase liquid chromatography coupled to ultraviolet and mass spectrometry detectors for the quantification of PhIP, three phase I and nine phase II metabolites in urine. Additionally, the identification of two PhIP-sulfates by the use of NMR is presented. Sample pretreatment consisted of straightforward dilution of urine. PhIP and its metabolites were shown to be stable in diluted urine for at least 22 h when stored at 2–8 °C. Precision of the analysis was within 15%. The assay has been successfully applied for the quantification of PhIP and 12 of its metabolites in urine from mice that received 200 mg kg −1 PhIP via oral gavage. Content Type Journal Article Pages 1-12 DOI 10.1007/s10337-011-2068-5 Authors S. F. Teunissen, Department of Pharmacy and Pharmacology, Slotervaart Hospital/The Netherlands Cancer Institute, Louwesweg 6, 1066 EC Amsterdam, The Netherlands H. Rosing, Department of Pharmacy and Pharmacology, Slotervaart Hospital/The Netherlands Cancer Institute, Louwesweg 6, 1066 EC Amsterdam, The Netherlands L. Brunsveld, Laboratory of Chemical Biology, Department of Biomedical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612 AZ Eindhoven, The Netherlands T. F. A. de Greef, Laboratory of Chemical Biology, Department of Biomedical Engineering, Eindhoven University of Technology, Den Dolech 2, 5612 AZ Eindhoven, The Netherlands S. Durmus, Division of Molecular Biology, The Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam, The Netherlands J. H. M. Schellens, Department of Clinical Pharmacology, The Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam, The Netherlands A. H. Schinkel, Division of Molecular Biology, The Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam, The Netherlands J. H. Beijnen, Department of Pharmacy and Pharmacology, Slotervaart Hospital/The Netherlands Cancer Institute, Louwesweg 6, 1066 EC Amsterdam, The Netherlands Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Thomas J. Bruno and Paris D. N. Svoronos (Eds): Handbook of Basic Tables for Chemical Analysis, 3rd Edition Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-2045-z Authors Eward R. Adlard, Burton, South Wirral, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Multiresponse optimization methodology in combination with experimental design was employed as a powerful technique for simultaneous optimization of input variables significant for evaluation of chromatographic behaviour of zolpidem tartrate, zolpacid, oxozolpidem, zolpyridine and zolpaldehyde towards various responses. In the first stage of the investigation fractional factorial design was used to decrease the number of variables that should be studied in detail. Among examined variables, pH of the mobile phase, percentage of organic modifier and buffer concentration showed to be statistically important and were consequently optimized with central composite design and Derringer’s desirability function. Four responses were considered, the retention factors of zolpacid and zolpaldehyde (the first and last peak) and the resolutions between critical peaks. Optimal conditions included Luna C 18 (2) analytical column (250 mm x 4.6 mm, 5 μm particle size), mobile phase consisted of methanol–10 mM ammonium acetate (68.4:31.6, v/v , pH 5.4) and column temperature of 35 °C. The flow rate of the mobile phase was 1 mL min −1 and the detection was performed at 254 nm. At the end, the method was successfully validated in accordance with ICH guideline and subsequently applied to the analysis of commercially available zolpidem tartrate tablets. Content Type Journal Article Pages 1-12 DOI 10.1007/s10337-011-2064-9 Authors Marija Malesevic, Medicines and Medical Devices Agency of Serbia, Vojvode Stepe 458, 11000 Belgrade, Serbia Ljiljana Zivanovic, Department of Drug Analysis, Faculty of Pharmacy, University of Belgrade, Vojvode Stepe 450, P.O. Box 146, 11000 Belgrade, Serbia Ana Protic, Department of Drug Analysis, Faculty of Pharmacy, University of Belgrade, Vojvode Stepe 450, P.O. Box 146, 11000 Belgrade, Serbia Zarko Jovic, Medicines and Medical Devices Agency of Serbia, Vojvode Stepe 458, 11000 Belgrade, Serbia Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    This study established a new methanol precipitation–ultrasonic emulsion breaking method for extraction of doxorubicin from polymeric micelles and developed a UPLC–MS/MS method for the determination of doxorubicin in rat plasma. The emulsion breaking efficiency of methanol is up to 99.2%. The plasma samples were analyzed by UPLC/MS/MS using positive electrospray ionization mode in the multiple-reaction monitoring (MRM) mode. The calibration curves were linear over the range 5–1,000 ng mL −1 with the lower limit of quantification of 5 ng mL −1 . The intra- and inter-day precisions of QC samples were all 〈10.0%. The chromatographic separation was 2.5 min. The developed method was successfully applied to a pharmacokinetic study of doxorubicin in rats following intravenous administration. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-2066-7 Authors Wenping Zhang, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Jin Sun, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Zhi Feng, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Xiaonan Su, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Meng Zhu, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Xiaofan Sui, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Yan Liu, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Mengying Tao, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Yunqiang Sun, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Guoliang Chen, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Zhonggui He, Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenyang, 110016 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A method of capillary electrophoresis with electrogenerated chemiluminescence was developed for the detection of spectinomycin. The linear ranges were from 0.01 to 1.0 mg mL −1 for spectinomycin. The limit of detection for spectinomycin with a signal-to-noise ratio of 3:1 was found to be 4.0 µg mL −1 . For practical application perchloric acid was used to eliminate the protein contained in human urine, which is very harmful to electrophoresis separation. The recoveries of spectinomycin at different levels in human urine were between 91.1 and 106.5%. The RSD was between 2.6 and 4.8% ( n  = 5–6). It was valuable in clinical and biochemical laboratories for monitoring the drug for various purposes. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-2060-0 Authors Wei Wei, College of Chemistry and Chemical Engineering, Southeast University, Nanjing, 210009 People’s Republic of China Min Wei, College of Food Science and Technology, Henan University of Technology, Zhengzhou, 450052 People’s Republic of China Zeyu Cai, Gulou Center for Disease Control and Prevention, Nanjing, 210009 People’s Republic of China Songqin Liu, College of Chemistry and Chemical Engineering, Southeast University, Nanjing, 210009 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Recombinant human erythropoietin (rhEPO) analogues are known to have been used in horse sports for their assumed performance enhancing properties. Recently, several authors have published liquid chromatographic-tandem mass spectrometric (LC-MS/MS) methods for confirming the presence of rhEPO analogues in horse plasma. In the current study, an improved LC-MS/MS confirmatory procedure for rhEPO, darbepoetin (DPO) and continuous erythropoietin receptor activator (CERA) in horse plasma was developed and validated. The method was also adapted for and applied to urine samples for the first time. Similar to previously published plasma assays, the methods utilise size exclusion and immunoaffinity extraction prior to tryptic cleavage, enzymatic deglycosylation and LC-MS/MS analysis of the resulting signature tryptic peptides (rhEPO/CERA T5, rhEPO/CERA/DPO T6 and DPO T9). However, the novel application of UPLC chromatography significantly improves the run time of the method compared to nano- or micro-LC and its robustness compared to nano-LC. Furthermore, recombinant canine EPO was found to serve as an effective internal standard, thus allowing confidence in interpretation of the success/failure of every step in the procedure. Limits of detection for confirming the presence of rhEPO, CERA and DPO in plasma were 0.1, 0.25 and 0.05 ng mL −1 , respectively, which were equal to or lower than limits achieved using previously published LC-MS/MS based methods. Limits of detection for confirming the presence of rhEPO, CERA and DPO in urine were 0.05, 0.15 and 0.025 ng mL −1 and the analysis of urine samples collected from horses administered rhEPO (Eprex™) or DPO (Aranesp™) demonstrated the use of this matrix as a suitable alternative in situations where plasma is not available. Content Type Journal Article Pages 1-16 DOI 10.1007/s10337-011-2119-y Authors James P. Scarth, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Cathrin Seibert, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Pamela R. Brown, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Phil Teale, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Gavin J. Beamon, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Clive M. Pearce, HFL Sport Science (an LGC company), Newmarket Road, Fordham, Cambridgeshire, CB7 5WW UK Richard A. Sams, HFL Sport Science (an LGC company), Alysheba Way, Lexington, KY 40509, USA Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The hydrophobic ionic liquid [BMIM]PF 6 (1-butyl-3-methylimidazolium hexafluorophosphate) can interact with sodium dodecyl sulfate (SDS) micelles in aqueous solution and modify their physicochemical properties to produce a unique separation efficiency in micellar electrokinetic chromatography (MEKC). An MEKC method was developed using [BMIM]PF 6 as a modifier for separating eight fluoroquinolone compounds (ciprofloxacin, enrofloxacin, gatifloxacin, ofloxacin, norfloxacin, enoxacin, pazufloxacin, and tosufloxacin). The effects of several parameters on the separation selectivity, e.g., pH, concentration of background electrolyte, concentration ratio and amount of [BMIM]PF 6 and SDS, were investigated. Under the optimal conditions of 10 mmol L −1 sodium borate, pH 7.1, 1.7% (w/w) SDS, 1.5% (w/w) [BMIM]PF 6 with 18 kV as running voltage, the eight investigated quinolone compounds were baseline separated within 15 min. The selectivity of the developed method differed from that of the simple SDS micelles system containing no ionic liquid. The results suggest that hydrophobic ionic liquids should be promising modifiers in capillary electrophoresis, especially in MEKC analysis. Content Type Journal Article Category Short Communication Pages 1-6 DOI 10.1007/s10337-011-2150-z Authors Zhitao Chen, College of Bioengineering, Chongqing University, 400030 Chongqing, China Zibei Zhong, College of Chemistry and Chemical Engineering, Chongqing University, 400030 Chongqing, China Zhining Xia, College of Bioengineering, Chongqing University, 400030 Chongqing, China Fengqing Yang, College of Chemistry and Chemical Engineering, Chongqing University, 400030 Chongqing, China Xiaojing Mu, College of Chemistry and Chemical Engineering, Chongqing University, 400030 Chongqing, China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Analytical derivatizations (AD) can increase the sensitivity of analyses—including those with mass spectrometric detection—by as much as three orders of magnitude. The extra steps required, however, are a possible impediment to their use. To simplify AD we investigated solid-phase analytical derivatization (SPAD) of compounds with diverse structures by using pentafluorobenzyl bromide (PFBBr) as the reagent. Model compounds were organic acids (e.g. phenols, chlorophenols and carboxylic acids) which were simultaneously extracted and derivatized from 0.1 M NaOH onto a polystyrene–divinylbenzene resin (XAD-4) as their pentafluorobenzyl (PFB) derivatives. Test analytes ranged in molecular weight from 94 for phenol to 266 for pentachlorophenol and octanol–water partition coefficients (log  P ) values ranged from 1.48 for phenol to 7.15 for hexadecanoic acid. Under SPAD conditions, reaction rates rapidly increased with log  P , but yields for less lipophilic compounds, although precise, were unacceptably low. Use of the tetrabutylammonium (TBA) cation as a phase transfer catalyst increased the yield of compounds with low log  P ; but, unexpectedly, as the log  P of the analyte increased, the phase transfer catalyst caused a decrease in yield. The data from this study define the log  P range of compounds that require TBA for optimal yield and the log  P range of compounds for which TBA compromises yield. This insight led to a simple, two-step, one-pot technique that gave high yields of the PFB derivatives for the entire range of analytes studied. SPAD first extracted/derivatized the lipophilic analytes from aqueous solution onto the solid phase. Extraction/derivatization of the polar analytes followed upon addition of TBA to the reaction mixture. The PFB ethers and esters of the entire range of analytes were then eluted from the XAD-4. The two-step procedure was faster, used less reagent and required lower temperature than comparable methods in the literature. With the two-step procedure, pentafluorobenzylation of phenols and carboxylic acids from water gave yields in excess of 88% with the exception of phenol and pentachlorophenol which were recovered in 57 and 44%, respectively. For all analytes, relative standard deviations were below 15%. The effect of matrix on yield varied between zero and a decline in recoveries of approximately 20–30% depending on the analyte and concentrations of NaCl or humic acid. In the presence of matrix components relative standard deviations remained below 20%. Content Type Journal Article Category Original Pages 1-8 DOI 10.1007/s10337-011-2160-x Authors Sanka N. Atapattu, Department of Pathology and Molecular Medicine, McMaster University, 3N26-1280 Main Street West, Hamilton, ON L8S 4K1, Canada Jordan N. Fortuna, Department of Pathology and Molecular Medicine, McMaster University, 3N26-1280 Main Street West, Hamilton, ON L8S 4K1, Canada Jack M. Rosenfeld, Department of Pathology and Molecular Medicine, McMaster University, 3N26-1280 Main Street West, Hamilton, ON L8S 4K1, Canada Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Programmed-temperature retention indices (PTRIs) are useful for the identification and quantification of chemicals by means of GC and GC/MS. To obtain reproducible PTRIs, we studied the influence of average linear velocity and column length under the constant average linear velocity control (CVC) using 55 pesticides and 33 fatty acid methyl esters. The PTRIs decreased with increasing average linear velocity, and the degree of decrease differs with the compounds. The PTRIs, however, were almost constant as long as the same average linear velocity was used even if the column length was changed. In addition, the correlation between the variation ratio in PTRI and the increase in average linear velocity was linear. Using the linear relationship between PTRIs and average linear velocities under CVC, highly reproducible PTRIs were obtained even if the capillary column length changes. Furthermore, the PTRIs determined by GC with FID, ECD, and FPD under atmospheric pressure were applied to GC/MS under vacuum or vice versa. From these results, it was confirmed that because CVC provides reproducible retention indices, CVC is advantageous for qualitative and quantitative analysis by GC and GC/MS. Content Type Journal Article Pages 1-11 DOI 10.1007/s10337-011-1956-z Authors H. Miyagawa, SHIMADZU Corporation, 1, Nishinokyo-Kuwabaracho Nakagyo-ku, Kyoto, 604-8511 Japan K. Nakagawa, SHIMADZU Corporation, 1, Nishinokyo-Kuwabaracho Nakagyo-ku, Kyoto, 604-8511 Japan K. Kadokami, Faculty of Environmental Engineering, The University of Kitakyushu, Hibikino, Wakamatsu-ku, Kitakyushu, Fukuoka 808-0135, Japan Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Artificial Neural Networks (ANNs) present a powerful tool for the modeling of chromatographic retention. In this paper, the main objective was to use ANNs as a tool in modeling of atorvastatin and its impurities’ retention in a micellar liquid chromatography (MLC) protocol. Factors referred to MLC were evaluated through 30 experiments defined by the Central Composite Design. In this manner, 5– x –3 topology as a starting point for ANNs’ optimization was defined too. In the next step, in order to set the network with the best performance, network optimization was done. In the first part, the number of nodes in the hidden layer and the number of experimental data points in training set were simultaneously varied, and their importance was estimated with suitable statistical parameters. Furthermore, a series of training algorithms was applied to the current network. The Back Propagation, Conjugate Gradient-descent, Quick Propagation, Quasi-Newton, and Delta-bar-Delta algorithms were used to obtain the optimal network. Finally, the predictive ability of the optimized neural network was confirmed through several statistical tests. The obtained network showed high ability to predict chromatographic retention of atorvastatin and its impurities in MLC. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-1994-6 Authors Anđelija Malenović, Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, Belgrade, Serbia Biljana Jančić-Stojanović, Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, Belgrade, Serbia Nađa Kostić, Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, Belgrade, Serbia Darko Ivanović, Department of Drug Analysis, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, Belgrade, Serbia Mirjana Medenica, Department of Physical Chemistry and Instrumental Methods, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, Belgrade, Serbia Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A sensitive, specific and rapid high performance liquid chromatography–atmospheric pressure chemical ionization source-tandem mass spectrometry (LC-APCI-MS-MS) method for the determination of pilocarpine in human plasma was developed and validated. The method is based on liquid–liquid extraction, followed by a reversed-phase liquid chromatographic separation, and detected by means of tandem mass spectrometry. The linear calibration curve covered a concentration range of 2–500 μg L −1 . The intra- and inter-day precisions for pilocarpine were 〈10% and the accuracies were between 90 and 110%. The method was applied successfully to a pharmacokinetic study involving 20 healthy Chinese male volunteers after oral administration of 6 mg pilocarpine. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1928-3 Authors Peng Yu, School of Pharmaceutical Sciences, Central South University, Changsha, 410013 China Guoping Yang, The Third Xiangya Hospital, Central South University, Changsha, 410013 China Hongyi Tan, The Third Xiangya Hospital, Central South University, Changsha, 410013 China Zeneng Cheng, School of Pharmaceutical Sciences, Central South University, Changsha, 410013 China Ming Song, School of Pharmaceutical Sciences, Central South University, Changsha, 410013 China Zhenkun Gu, School of Pharmaceutical Sciences, Central South University, Changsha, 410013 China Xiao Li, School of Pharmaceutical Sciences, Central South University, Changsha, 410013 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A highly sensitive, precise, and accurate reversed-phase high-performance liquid-chromatography/electrochemical detection method for simultaneous determination of the endogenous free α-lipoic acid and dihydrolipoic acid in biological matrices was developed and validated. The two analytes were extracted from the samples with acetonitrile/10% metaphosphoric acid solution (aqueous) (50/50 v / v ). To determine the total lipoic acid, samples were treated with tris(2-carboxyethyl)phosphine solution in phosphate buffer, pH 2.5 with 85% orthophosphoric acid prior to deproteination. The two analytes were separated on a C 18 (150 × 4.6 mm, 5 μm) analytical column using acetonitrile-50 mM phosphate buffer, pH 2.5 with 85% orthophosphoric acid (35/65 v / v ) as the isocratic mobile phase pumped at a flow rate of 2.0 mL min −1 at the column oven temperature of 35 °C. The column eluents were monitored at a potential of 0.9 V. These analytes were efficiently resolved in 〈7 min. The present method was sufficiently robust and specific for simultaneous determination of the two analytes and demonstrated acceptable values for linearity ( r 2  = 0.999 in the range of 0.1–500 and 0.25–1,000 ng mL −1 for α -lipoic acid and dihydrolipoic acid, respectively), recovery (〉97%), precision (RSD% 〈2), and sensitivity (on column limit of detection, 150 and 375  f g for α-lipoic acid and dihydrolipoic acid, respectively and limit of quantification: 0.5 and 1.25 pg for α-lipoic acid and dihydrolipoic acid, respectively), indicating that the proposed method was more sensitive, precise, economical, and versatile, and has higher throughput than the previously reported methods for simultaneous determination of the two analytes. Content Type Journal Article Pages 1-11 DOI 10.1007/s10337-011-1997-3 Authors Muhammad Imran Khan, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Zafar Iqbal, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Lateef Ahmad, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Yasar Shah, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Shabnam Nazir, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Abbas Khan, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Fazli Nasir, Department of Pharmacy, University of Peshawar, Peshawar, 25120 Pakistan Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A fast, sensitive, and specific LC–MS–MS method for determination of quinine (QN) and doxycycline (DOX) in rat plasma has been developed and validated. QN, DOX, and cimetidine (internal standard, IS) were extracted from the plasma by protein precipitation. The compounds were separated on a C 18 column with methanol–0.1% aqueous formic acid 70:30 ( v / v ) as mobile phase at a flow rate of 0.5 mL min −1 (split 1:3). Detection was by positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, monitoring the transitions 325.0 → 307.0, 445.0 → 428.1, and 252.8 → 159.0, for QN, DOX, and IS, respectively. The analysis was carried out in 2.0 min and the method was linear in the plasma concentration range 5–5,000 ng mL −1 . The mean extraction recoveries for QN, DOX, and IS from plasma were 89.4, 90.5, and 86.3%, respectively. The method was validated for linearity, precision, accuracy, specificity, and stability; the results obtained were within the acceptable range. The proposed method was successfully applied to the determination of QN and DOX in rat plasma samples to support pharmacokinetic studies. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1949-y Authors Liberato Brum Junior, Programa de Pós-Graduação em Ciências Farmacêuticas, Universidade Federal do Rio Grande do Sul, Avenida Ipiranga, 2752, CEP 90610-000 Porto Alegre, RS Brazil Manoela Guerra Leal, Programa de Pós-Graduação em Ciências Farmacêuticas, Universidade Federal do Rio Grande do Sul, Avenida Ipiranga, 2752, CEP 90610-000 Porto Alegre, RS Brazil Flávia de Toni Uchoa, Centro Bioanalítico de Medicamentos da Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS Brazil Moacir Kaiser, Centro Bioanalítico de Medicamentos da Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS Brazil Sílvia Staniçuaski Guterres, Programa de Pós-Graduação em Ciências Farmacêuticas, Universidade Federal do Rio Grande do Sul, Avenida Ipiranga, 2752, CEP 90610-000 Porto Alegre, RS Brazil Teresa Dalla Costa, Programa de Pós-Graduação em Ciências Farmacêuticas, Universidade Federal do Rio Grande do Sul, Avenida Ipiranga, 2752, CEP 90610-000 Porto Alegre, RS Brazil Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    This study aimed to develop an LC-MS/MS assay for the quantitation of S002-857 in plasma, urine and feces to evaluate the pharmacokinetic parameters and elimination pathway for further development of S002-857. A sensitive and selective LC-MS/MS method was developed and validated for estimating a novel antidiabetic flavone derivative, S002-857, synthesized by Central Drug Research Institute, CSIR, Lucknow, India. Plasma and urine samples were prepared by two-step liquid-liquid extraction with diethyl ether and feces by protein precipitation using acetonitrile. The analyte was chromatographed on a cyano column with methanol-ammonium acetate buffer (pH 4.6, 10 mM; 90:10, v/v ). The calibration curves were linear over a range of 0.78–400 ng mL −1 for plasma and 1.56–400 ng mL −1 for urine and feces samples. The accuracy and precision were 〈15% for plasma, urine and feces samples. The recoveries from spiked plasma, urine and feces samples were 〉85%. S002-857 was stable in plasma for 8 h at ambient temperature, 30 days at −60 °C and after three freeze-thaw cycles. The assay was successfully applied to determine the pharmacokinetic parameters and excretion profile in male rats. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1978-6 Authors Nagsen Gautam, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Lucknow, 226001 India Hari Narayan Kushwaha, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Lucknow, 226001 India Hemant Kumar, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Lucknow, 226001 India Ram Pratap, Medicinal and Process Chemistry Division, Central Drug Research Institute, CSIR, Lucknow, 226001 India Shio Kumar Singh, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Lucknow, 226001 India Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Natural prenyloxycinnamic acids were shown to exert in vitro and in vivo remarkable and valuable anti-cancer and anti-inflammatory effects. Among these, 4′-geranyloxyferulic acid [3-(4′-geranyloxy-3′-methoxyphenyl)-2- trans -propenoic acid] was discovered as an efficient orally active chemopreventive agent of several types of cancer, and its structural analogue boropinic acid was shown to exert a valuable inhibitory effect both in vitro and in vivo against the growth of Helicobacter pylori. As a continuation of our chemical, chemico-physical, and pharmacological studies on these secondary metabolites, we report herein the comparison between traditional UV/Vis assays and HPLC–DAD methods for the determination of the molar absorptivity coefficient of 4′-geranyloxyferulic acid ( ε 310  = 12,950 and ε 288  = 11,910 L mol −1  cm −1 ) and boropinic acid ( ε 310  = 13,510 and ε 288  = 12,350 L mol −1  cm −1 ). Ferulic acid was merely used as a reference standard to test the possibility of the application of these two assays to the oxyprenylated compounds. The data reported in the present study will represent an essential aid for future studies aimed to better define the pharmacological profile and the mechanism of action of these compounds and are an important starting point to evaluate other natural products where standard powders are not available. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1979-5 Authors Marcello Locatelli, Dipartimento di Scienze del Farmaco, Università degli Studi “G. D’Annunzio” Chieti-Pescara, Via dei Vestini 31, 66100 Chieti (CH), Italy Giuseppe Carlucci, Dipartimento di Scienze del Farmaco, Università degli Studi “G. D’Annunzio” Chieti-Pescara, Via dei Vestini 31, 66100 Chieti (CH), Italy Salvatore Genovese, Dipartimento di Scienze del Farmaco, Università degli Studi “G. D’Annunzio” Chieti-Pescara, Via dei Vestini 31, 66100 Chieti (CH), Italy Massimo Curini, Dipartimento di Chimica e Tecnologia del Farmaco, Sezione di Chimica Organica, Università degli Studi di Perugia, Via del Liceo, 06123 Perugia (PG), Italy Francesco Epifano, Dipartimento di Scienze del Farmaco, Università degli Studi “G. D’Annunzio” Chieti-Pescara, Via dei Vestini 31, 66100 Chieti (CH), Italy Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Bernd Spangenberg, Colin F. Poole, Christel Weins: Quantitative Thin-Layer Chromatography: A Practical Survey Content Type Journal Article Pages 1-1 DOI 10.1007/s10337-011-1977-7 Authors Ian D. Wilson, Maccesfield, Cheshire, UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The article is intended to introduce and discuss a new quantile regression method for baseline detrending of chromatographic signals. It is compared with current methods based on polynomial fitting, spline fitting, LOESS, and Whittaker smoother, each with thresholding and reweighting approach. For curve flexibility selection in existing algorithms, a new method based on skewness of the residuals is successfully applied. The computational efficiency of all approaches is also discussed. The newly introduced methods could be preferred to visible better performance and short computational time. The other algorithms behave in comparable way, and polynomial regression can be here preferred due to short computational time. Content Type Journal Article Pages 1-11 DOI 10.1007/s10337-011-1962-1 Authors Ł. Komsta, Department of Medicinal Chemistry, Medical University of Lublin, Jaczewskiego 4, 20-090 Lublin, Poland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A method for fast, sensitive, and specific hydrophilic interaction chromatography combined with tandem mass spectrometry (HILIC-MS/MS) was developed for the first time to determine the level of pidotimod in human plasma. With rosiglitazone as internal standard, analysis was carried out on a HILIC column (150 mm × 2.1 mm, 3.5 μm) using a mobile phase consisting of methanol:0.2% formic acid (60:40, v / v ). Detection was carried out by tandem mass spectrometry using electrospray ionization (ESI). Linear calibration curves were obtained in the concentration range of 11.2–1.12 × 10 4  ng mL −1 for pidotimod, with a lower limit of quantification of 11.2 ng mL −1 . The intra- and inter-day precision values were high, with standard deviations lower than 15%, and the accuracy, in terms of relative error, ranged from −10.5 to 9.4% at all quality control (QC) levels. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1930-9 Authors H. S. Chen, State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Science, Guangzhou, 510640 China M. Shen, Hygiene Detection Center, School of Public Health and Tropical Medicine, Southern Medical University, Guangzhou, 510515 China L. Y. Chen, Hygiene Detection Center, School of Public Health and Tropical Medicine, Southern Medical University, Guangzhou, 510515 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Acknowledgement to Referees Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1986-6 Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    We present the validation of a multiresidue method for the concurrent SPE of organochlorine (OCP) and phenoxy-acidic pesticides (PA) in river water. The two classes of compounds show very different chemical characteristics. The analyses were performed by gas chromatography–mass spectrometry and by liquid chromatography–electrospray ionization–mass spectrometry. The method was validated at three different concentrations: method limit of quantitation, 0.5 and 5 μg L −1 . The recoveries were in the range 65–135% for all the target compounds and in the range 83–113% with RSD 〈20% for most of them at all the concentrations tested. The method showed good accuracy, precision, and sensitivity, and allowed the analysis of the selected pesticides at a concentration lower than that required by the EU current legislation for surface water [ 1 ]. The single-step procedure reduced artifacts, matrix effects, and speeded up sample preparation. Content Type Journal Article Pages 1-9 DOI 10.1007/s10337-011-1971-0 Authors Achille Cappiello, LC–MS Laboratory, Dipartimento di Scienze della Terra, della Vita e dell’ Ambiente (DiSteVa), Università di Urbino “Carlo Bo”, Piazza Rinascimento 6, 61029 Urbino, Italy Elisabetta Pierini, LC–MS Laboratory, Dipartimento di Scienze della Terra, della Vita e dell’ Ambiente (DiSteVa), Università di Urbino “Carlo Bo”, Piazza Rinascimento 6, 61029 Urbino, Italy Pierangela Palma, LC–MS Laboratory, Dipartimento di Scienze della Terra, della Vita e dell’ Ambiente (DiSteVa), Università di Urbino “Carlo Bo”, Piazza Rinascimento 6, 61029 Urbino, Italy Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In this work, tetrazole-functionalized stationary phase was prepared with nitrile-modified silica by an ammonium-catalyzed (3 + 2) azide-nitrile cycloaddition reaction. The prepared stationary phase was used for separation of nucleobases and nucleosides by hydrophilic interaction chromatography (HILIC) mode. A typical HILIC mechanism was observed at higher content of acetonitrile (〉85%, v / v ) in the mobile phase. The retention mechanism of the column was investigated by the models used for describing partitioning and surface adsorption through adjustment ratio of water in the mobile phase, and by the influence of salt concentration, buffer pH, and temperature on the retention of solutes. The results illustrated that the surface adsorption through hydrogen bonding dominated the retention behavior of nucleobases/nucleosides under HILIC mode. From the separation ability, the tetrazole-functionalized stationary phase could become a valuable alternative for the separation of the compounds concerned. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-011-1985-7 Authors Xiaojun Dai, Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Material Science, Northwest University, Xi’an, 710069 People’s Republic of China Xiaolei Qian, Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Material Science, Northwest University, Xi’an, 710069 People’s Republic of China Bolin Gong, Key Laboratory of Energy and Chemical Engineering, Ningxia University, Yinchuan, 750021 People’s Republic of China Yinmao Wei, Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Material Science, Northwest University, Xi’an, 710069 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The nature of ionic liquids (ILs) facilitates their analysis by ion chromatography which, unlike conventional high-performance liquid chromatography, enables analysis both of cations and anions. This paper describes a pioneering ion-chromatographic investigation of IL cations and statistical evaluation of quantitative structure–retention relationships with the objective of predicting the molecular mechanism responsible for retention. Eleven ionic liquid imidazolium and pyridinium cations were analyzed on a CS15 cation-exchange column by isocratic elution with acetonitrile–methanesulfonic acid mixtures. Structural descriptors of the cations obtained from molecular modeling were used to describe their hydrophobicity as determined by chromatography. The most statistically significant were three-term QSRR regression equations relating log k w to analyte n -octanol–water partition coefficient (log P ), dipole moment ( μ ), solvent accessible surface area ( A SAS ), and hydration energy (HE). They indicate the important role of both hydrophobic and polar the retention of ILs on the CS15 column. Content Type Journal Article Pages 1-10 DOI 10.1007/s10337-011-1960-3 Authors S. Studzińska, Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin St., 87-100 Toruń, Poland M. Molíková, Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 532 10 Pardubice, Czech Republic P. Kosobucki, Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin St., 87-100 Toruń, Poland P. Jandera, Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 532 10 Pardubice, Czech Republic B. Buszewski, Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin St., 87-100 Toruń, Poland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A comparative quantitative structure–retention relationship (QSRR) study has been carried out to predict the retention time of nitrobenzene derivatives using original molecular descriptors and multivariate image analysis (MIA) descriptors. First, original molecular descriptors were generated from molecular structures and applied to construct QSRR models using multiple linear regression (MLR), partial least squares (PLS), and artificial neural network (ANN) modeling methods. Then, multivariate image analysis (MIA) descriptors were generated from pixels of images and analyzed using correlation ranking–principal component regression (CR–PCR) and correlation ranking–principal component–artificial neural network (CR–PC–ANN) methods. In this paper, the CR–PC–ANN method presented better results than the other methods for predicting the retention time of the studied compounds. Coefficients of determination ( R 2 ) using the CR–PC–ANN method for the training, test, and validation sets were 0.989, 0.999, and 0.999, respectively. Content Type Journal Article Pages 1-10 DOI 10.1007/s10337-011-1969-7 Authors Zahra Garkani-Nejad, Chemistry Department, Faculty of Science, Vali-e-Asr University, Rafsanjan, Iran Mohammad Ahmadvand, Chemistry Department, Faculty of Science, Vali-e-Asr University, Rafsanjan, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In the present work, six nonionic block copolymer surfactants consisting of poly(ethylene glycol) (PEG), polyethylene (PE), and poly(propylene glycol) (PPG) were exploited to extract total proteins from maize ( Zea mays L.) roots within a water–organic solvent system. After the treatment, proteins were partitioned into aqueous phase, interphase, and organic phase. The total yield was increased by up to 30% after adding PE-PEG block polymer surfactant compared with control. Two-dimensional electrophoresis (2-DE) was further used to evaluate proteins in water phase and interphase; the results revealed that the spot numbers and density were all improved, and well-focused electrophoretic patterns were achieved with higher density and without excess Joule heating problem after adding nonionic block polymer surfactants. Among the six investigated block polymers, PE-PEG extracted the largest amount of proteins. Content Type Journal Article Pages 1-10 DOI 10.1007/s10337-011-1961-2 Authors Hongbo Ma, Department of Plant Nutrition, College of Resources and Environmental Sciences, China Agricultural University, Beijing, 100193 People’s Republic of China Yufeng Hu, Department of Plant Nutrition, College of Resources and Environmental Sciences, China Agricultural University, Beijing, 100193 People’s Republic of China Futong Yu, Department of Plant Nutrition, College of Resources and Environmental Sciences, China Agricultural University, Beijing, 100193 People’s Republic of China Xueqin Ren, Department of Plant Nutrition, College of Resources and Environmental Sciences, China Agricultural University, Beijing, 100193 People’s Republic of China Fusuo Zhang, Department of Plant Nutrition, College of Resources and Environmental Sciences, China Agricultural University, Beijing, 100193 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Erratum to: LC–MS Method for Determination of Amphotericin B in Rabbit Tears and Its Application to Ocular Pharmacokinetic Study Content Type Journal Article Pages 1-1 DOI 10.1007/s10337-011-1953-2 Authors Rabi Sankar Bhatta, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Post box 173, Lucknow, 226001 India Chetan Rathi, Department of Pharmaceutics, National Institute of Pharmaceutical Education and Research (NIPER), Raebareli, 229010 India Hardik Chandasana, Department of Pharmaceutics, National Institute of Pharmaceutical Education and Research (NIPER), Raebareli, 229010 India Devendra Kumar, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Post box 173, Lucknow, 226001 India Yashpal Singh Chhonker, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Post box 173, Lucknow, 226001 India Girish Kumar Jain, Pharmacokinetics and Metabolism Division, Central Drug Research Institute, CSIR, Post box 173, Lucknow, 226001 India Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A new extraction technique, ionic liquid-assisted extraction (ILAE), has been developed. The ILAE process was further optimized by varying different parameters such as pretreatment time and temperature, ionic liquid/sample ratio, particle size and solvents. Under the optimum conditions, the extraction yield of ILAE was higher than that of Soxhlet extraction. The results of bioassay test showed that crude extract of ILAE was almost the same with that of Soxhlet extraction. The results in this study can serve as a reference for the ILAE of effective constituents in medicinal plants. Content Type Journal Article Pages 1-6 DOI 10.1007/s10337-010-1865-6 Authors Ronghua Jin, School of Chemistry and Chemical Engineering, South China University of Technology, Wushan Road, Tianhe District, Guangzhou, 510640 China Ling Fan, College of Science, South China Agricultural University, Guangzhou, 510642 China Xiaoning An, School of Chemistry and Chemical Engineering, South China University of Technology, Wushan Road, Tianhe District, Guangzhou, 510640 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    As over 70% of pharmaceutical compounds are bases, the analysis of these basic compounds by high performance liquid chromatography (HPLC) continues to be of great value and interesting. Acetyl cholinesterase inhibitors (AChEIs), which contain the basic compounds like Rivastigmine tartrate, Galantamine hydrobromide and Donepezil with different polarities, were chosen for the study. A rapid screening of the volatile ion-pairing reagents was performed using modern techniques like ultra high performance liquid chromatography (UHPLC). The experiments were planned using the ‘Design of Experiments’ (DoE) approach to identify the LC–MS compatible ion-pair reagent. In this study, Heptafluorobutyric acid (HFBA) has given a very good peak shape with tailing factor at 1.4 and theoretical plates up to ~5,000 were observed, compared to tailing factor at 1.9 and theoretical plates up to ~3,000 with non-volatile ion-pair reagent sodium heptane sulphonate (SHS). Similarly retention with HFBA was optimum as ~5 min in short run time method compared to ~13 min with SHS. This ion-pair reagent has proved to be good replacement of sodium alkyl sulphonate modifiers. HFBA can also be used for semi-preparative work for isolation of impurities by just evaporating the solvents. It avoids the extraction of other inorganic modifiers. Content Type Journal Article Pages 1-10 DOI 10.1007/s10337-011-1970-1 Authors Girish R. Deshpande, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, Hyderabad, AP 500055, India Amrendra K. Roy, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, Hyderabad, AP 500055, India N. Someswara Rao, Department of Inorganic and Analytical Chemistry, Andhra University, Visakhapatnam, 530 003 India B. Mallikarjuna Rao, Department of Inorganic and Analytical Chemistry, Andhra University, Visakhapatnam, 530 003 India J. Rudraprasad Reddy, Department of Inorganic and Analytical Chemistry, Andhra University, Visakhapatnam, 530 003 India Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A rapid and precise LC-ESI-MS-MS method for the parallel identification and quantification of dopamine, serotonin and their metabolites (homovanillic acid, 3-methoxytyramine, 3,4-dihydroxyphenylacetic acid and 5-hydroxyindolacetic acid) from rat brain tissue without any pre-analysis adjustment of the sample such as pre-concentration or derivatization has been developed. In particular, the reaction-monitoring mode was selected for its extremely high degree of selectivity and the stable-isotope-dilution assay for its high precision of quantification. Alternation the ionization polarity in the course of mass spectrometry detection enabled to determine substances susceptible to various ionization modes in only one analysis run. This fact, in combination with an easy pre-treatment step, constitutes the method straightforward and time undemanding. The developed method was characterized with a high precision (≤19.5%, determined as RSD), an acceptable accuracy (≥82.0%, determined as recovery), a low limit of detection (≤0.40 ng/100 mg brain tissue) and a low limit of quantification (≤0.42 ng/100 mg brain tissue). The method has been applied in a recent animal study. The levels of the studied neurotransmitters have been determined in the rat brain hippocampus, prefrontal cortex, and striatum in an animal model of schizophrenia induced by an acute dose of a dizocilpine. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1959-9 Authors Věra Najmanová, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6, Czech Republic Lukáš Rambousek, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6, Czech Republic Kamila Syslová, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6, Czech Republic Věra Bubeníková, Department of Biochemistry and Brain Pathophysiology, Prague Psychiatric Center, Ustavni 91, 181 03 Prague 8, Czech Republic Romana Šlamberová, Department of Normal Pathological and Clinical Physiology, Third Faculty of Medicine, Charles University, Ruska 87, 100 00 Prague 10, Czech Republic Karel Valeš, Institute of Physiology, Videnska, 1083 142 20 Prague 4, Czech Republic Petr Kačer, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6, Czech Republic Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Nano-baskets of calixarenes have been subject to extensive research in the construction of liquid chromatographic phases, extractants, transporters, electrode ionophores, and optical and electrochemical sensors over the past 4 decades. There has long been interest in calixarene-based liquid chromatographic phases. Owing to the recent rapid growth in the number of publications on calixarene-based liquid chromatographic phases, this review paper focuses on their different applications in the main fields of molecular and ionic species as well as liquid chromatographic mobile and stationary phases. Although the recent reports have focused on the optimization and application of one kind or a unique group of calixarenic mobile or stationary phases, this review is a collection and comparison of a variety of research data dealing with the synthesis, preparation and behavior of calixarene-based liquid chromatographic phases. Content Type Journal Article Pages 1-19 DOI 10.1007/s10337-011-1954-1 Authors Bahram Mokhtari, Phase Separation & FIA Lab, Department of Chemistry, Faculty of Science, Zanjan University, Zanjan, 45195-313 Iran Kobra Pourabdollah, Department of Chemical Engineering, Islamic Azad University, Shahreza Branch, Shahreza, Iran Nasser Dalali, Phase Separation & FIA Lab, Department of Chemistry, Faculty of Science, Zanjan University, Zanjan, 45195-313 Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    An isocratic reversed-phase HPLC method with ultraviolet detection at 205 nm has been developed for analysis of cyclosporine A (CyA) in rabbit ocular samples. Neither internal standard nor extraction was needed for sample preparation. Acetonitrile (ACN; 1 mL) was added to 250 μL aqueous and vitreous samples to precipitate proteins. The supernatant was dried and the residue was reconstituted in mobile phase and injected for HPLC analysis. Chromatography was performed on an octadecyl silane-A (ODSA) C 18 (4.6 × 250 mm, 5 μm) column. The column temperature was fixed at 70 °C and the mobile phase was ACN 65%, methanol 20% and water 15% at a flow rate of 1.5 mL min −1 . The calibration curve for CyA in rabbit ocular samples was linear over the concentration range 0.2 and 10 μg mL −1 with a correlation coefficient of 0.9992. Intra-day and inter-day precision were 4.61–7.83% and 5.27–10.70%, respectively. Intra-day and inter-day accuracy were 89.2–108% and 83.4–111%, respectively. The limits of detection (LOD) and quantification (LOQ) were 5.7 and 38 ng mL −1 , respectively. The method was successfully used for analysis of CyA in real aqueous and vitreous humor samples from New Zealand albino rabbits. The method is therefore suitable for analysis of CyA in ocular samples. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1963-0 Authors Bizhan Malaekeh-Nikouei, Nanotechnology Research Center, School of Pharmacy, Mashhad University of Medical Sciences, Mashhad, Iran Toka Banaee, Khatam-al-Anbia Eye Hospital and Eye Research Center, Mashhad University of Medical Sciences, Mashhad, Iran Javad Aghamohammadian, Pharmaceutical Research Center, School of Pharmacy, Mashhad University of Medical Sciences, Mashhad, Iran Navid Mosallaei, Nanotechnology Research Center, School of Pharmacy, Mashhad University of Medical Sciences, Mashhad, Iran Seyed Ahmad Mohajeri, Pharmaceutical Research Center, School of Pharmacy, Mashhad University of Medical Sciences, Mashhad, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A sensitive and specific liquid chromatography electrospray ionisation–tandem mass spectrometry method for determination of new non-imidazole histamine H 3 receptor antagonist 1-[3-(4- tert -butylphenoxy)propyl]piperidine (DL76) in rat serum has been developed and validated. Chromatography was performed on a XBridge™ C18 analytical column (2.1 × 30 mm, 3.5 µm, Waters, Ireland) with gradient elution using a mobile phase containing acetonitrile and water with an addition of 0.1% of formic acid. Detection was achieved by an Applied Biosystems MDS Sciex (Concord, Ontario, Canada) API 2000 triple quadrupole mass spectrometer. Electrospray ionization (ESI) was used for ion production. The limit of detection in the SRM mode was found to be 0.5 ng mL −1 . The limit of quantification was 1 ng mL −1 . The precision and accuracy for both intra- and inter-day determination of DL76 ranged from 1.65 to 15.09% and from 88.74 to 113.43%. The results of this analytical method validation allow to carry out pharmacokinetic studies in rats. The method was used for the pilot study of the pharmacokinetic behavior of DL76 in rats after intravenous administration. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1983-9 Authors Malgorzata Szafarz, Department of Pharmacokinetics and Physical Pharmacy, Faculty of Pharmacy, Jagiellonian University Medical College, Medyczna 9, 30-688 Krakow, Poland Joanna Szymura-Oleksiak, Department of Pharmacokinetics and Physical Pharmacy, Faculty of Pharmacy, Jagiellonian University Medical College, Medyczna 9, 30-688 Krakow, Poland Dorota Lazewska, Department of Technology and Biotechnology of Drugs, Faculty of Pharmacy, Jagiellonian University Medical College, Medyczna 9, 30-688 Krakow, Poland Katarzyna Kiec-Kononowicz, Department of Technology and Biotechnology of Drugs, Faculty of Pharmacy, Jagiellonian University Medical College, Medyczna 9, 30-688 Krakow, Poland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A β -cyclodextrin ( β -CD) and a hydroxypropyl- β -cyclodextrin (HP- β -CD) bonded chiral stationary phase (CSP) were prepared. Comparative evaluations of these two CSPs for the enantioseparation of hydrobenzoin, benzoin and α -phenethyl alcohol by reversed-phase liquid chromatography were presented. The effects of buffer composition in the mobile phase on the retention and enantioseparation were investigated. The borate buffer had a significant influence on the retention and enantioseparation of hydrobenzoin. Linear solvent strength retention model was used to fit the chromatographic data. Good linearity existed between the logarithm of retention factor ( k ) and the volume fraction of organic modifier ( φ ). Another retention model, stoichiometric displacement theory for retention, was also tried to fit the chromatographic data. The results showed that not only acetonitrile, but also water molecules participated in the displacing process of the solute. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1995-5 Authors Guangyan Yu, Department of Chemistry and Environmental Science, Zhangzhou Normal University, 36 Xianqian Straight Street, Xiangcheng District, Zhangzhou, 363000 China Lizhen Guo, Department of Chemistry and Environmental Science, Zhangzhou Normal University, 36 Xianqian Straight Street, Xiangcheng District, Zhangzhou, 363000 China Feiyun Xie, Department of Chemistry and Environmental Science, Zhangzhou Normal University, 36 Xianqian Straight Street, Xiangcheng District, Zhangzhou, 363000 China Bixia Yao, Department of Chemistry and Environmental Science, Zhangzhou Normal University, 36 Xianqian Straight Street, Xiangcheng District, Zhangzhou, 363000 China Qingle Zeng, College of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, 1 Dongsanlu, Erxianqiao, Chenghua District, Chengdu, 610059 China Wen Weng, Department of Chemistry and Environmental Science, Zhangzhou Normal University, 36 Xianqian Straight Street, Xiangcheng District, Zhangzhou, 363000 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    An ion exchange-reversed-phase two-dimensional liquid chromatography (2D-LC) system was developed based on a newly designed interface. The interface was constructed by alternately connecting tandem columns to one of the parallel separation columns to increase the separation efficiency. Separation on the tandem column does not affect the switching frequency; the valve switching could be maintained at high frequency. The constructed interface could be used in both ambient and elevated temperature modes. Under high-temperature mode, only the tandem column was heated, which simplified the operation, decreased the backpressure, improved the solvent compatibility, and speeded up the separation. Tryptic digestion of four proteins was used to evaluate the performance of the developed system. The peak capacity of the 2D-LC system reached 650 under ambient conditions and 890 under high temperature conditions. When compared with the traditional parallel column interface constructed in this paper, the new interface produced a 60% higher peak capacity. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1974-x Authors Duxin Li, Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai, 200237 People’s Republic of China Lingyi Zhang, Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai, 200237 People’s Republic of China Zhicong Wang, Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai, 200237 People’s Republic of China Azeem Intisar, Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai, 200237 People’s Republic of China Weibing Zhang, Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai, 200237 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    The objectives of this study were to investigate the molecular mechanisms of retention of selected fungicides and to classify stationary phases used for RP-HPLC. Chromatographic measurements were made using eight physicochemically diverse HPLC columns which were evaluated for analysis of nine biologically active compounds (strobilurins and triazoles). QSRRs were derived for the logarithms of the retention factors normalized to a hypothetical zero percent organic modifier in the mobile phase, log  k W . Structural descriptors of the pesticides were used to describe their chromatographic retention behaviour under the given LC conditions. The next step was the correlation between retention data, log  k W , and the structural descriptors of the analytes from molecular modelling. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1931-8 Authors Sylwia Noga, Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin Street, 87-100 Toruń, Poland Monika Michel, Plant Protection Institute, Pesticide Residue Laboratory, 20 W Węgorka Street, 60-318 Poznan, Poland Bogusław Buszewski, Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, 7 Gagarin Street, 87-100 Toruń, Poland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    In this study, dispersive liquid–liquid microextraction (DLLME) combined with ultra high pressure liquid chromatography (UHPLC)–tunable ultraviolet detection (TUV), was developed for pre-concentration and determination of trace levels of tetracyclines, including 4-epitetracycline, 4-epichlortetracycline, doxycycline, chlortetracycline oxytetracycline, tetracycline, 4-epianhydrotetracycline and anhydrotetracycline, in aqueous samples. La (III) was used as the chelating agent to form a hydrophobic complex compound with tetracyclines, followed by extraction with ionic liquids. Some important parameters that may affect extraction efficiencies were examined and optimized. Under the optimum conditions, linearity of the method was observed in the range of 0.1–200 μg L −1 , with correlation coefficients ( r 2 ) 〉0.992. The limits of detection and quantification were 0.031–0.079 and 0.10–0.26 μg L −1 , respectively. The spiked recoveries of eight target compounds in river water, fishpond water and hog leachate were achieved in the range of 62.6–96.3, 58.9–94.5, 55.1–86.1%, respectively. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1992-8 Authors Dekun Hou, College of Chemistry and Chemical Engineering, Inner Mongolia University, No.235, Daxue Xi Road, Hohhot, 010021 Inner Mongolia China Yan Guan, College of Chemistry and Chemical Engineering, Inner Mongolia University, No.235, Daxue Xi Road, Hohhot, 010021 Inner Mongolia China Xiaowei Di, College of Chemistry and Chemical Engineering, Inner Mongolia University, No.235, Daxue Xi Road, Hohhot, 010021 Inner Mongolia China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Gottfried Glöckner (1925–2010) Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-1972-z Authors Klaus Rissler, Solvias AG, Römerpark 2, 4303 Kaiseraugst, Switzerland Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A simple and repeatable liquid chromatography method with UV detection is described for the determination of pyrroloquinoline quinone in DNA binding studies first. Binding of pyrroloquinoline quinone to DNA was measured indirectly by determining unbound pyrroloquinoline quinone. Pyrroloquinoline quinone was chromatographed on a reversed-phase column using gradient elution with mobile phases of 0.1% trifluoroacetic acid (TFA) in deionized water and 0.1% TFA in acetonitrile at a flow-rate of 0.8 mL min −1 and detected at 249 nm. The mean content of unbound pyrroloquinoline quinone to three DNA in (hydroxymethyl) aminoethane(Tris–HCl) media were dropped from 99.3 to 80.3% in 250 min, and than to 64.8% at 1200 min, but the binding remained constant in deionized water. The method precision were validated with RSD 1.05 and 0.69% for peak areas and retention times. Validation of the method showed that the assay was linear from 25 to 2,000 μM and 5 to 2,000 μM pyrroloquinoline quinone in Tris–HCl and deionized water, respectively. The accuracy for three concentrations of pyrroloquinoline quinone with different types DNA in two media were within the given range of 80.9–113.6%. Content Type Journal Article Pages 1-4 DOI 10.1007/s10337-011-1993-7 Authors Xingqin Zhou, Key Laboratory of Nuclear Medicine, Ministry of Health, Jiangsu Key Laboratory of Molecular Nuclear Medicine, Jiangsu Institute of Nuclear Medicine, Wuxi, 214063 Jiangsu China Jiankang Zhang, Key Laboratory of Nuclear Medicine, Ministry of Health, Jiangsu Key Laboratory of Molecular Nuclear Medicine, Jiangsu Institute of Nuclear Medicine, Wuxi, 214063 Jiangsu China Xiaofeng Qin, Key Laboratory of Nuclear Medicine, Ministry of Health, Jiangsu Key Laboratory of Molecular Nuclear Medicine, Jiangsu Institute of Nuclear Medicine, Wuxi, 214063 Jiangsu China Xindai Hu, East China Normal University, Shanghai, 200241 China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A novel water-holding adsorbent was synthesized by introducing a zwitter-ionic polymer to a hydrophilic methacrylate base resin. The retention abilities of the hydrophilic compounds on the adsorbents with and without cross-link in the zwitter-ionic functional groups were examined. The amount of held water on the non-cross-linked adsorbent was higher than that of the cross-linked one. The extraction efficiencies of the hydrophilic solutes on the adsorbents were evaluated by the solid phase extraction method. These adsorbents showed high affinity for nucleosides and glycosides, and good recoveries for such hydrophilic compounds in the solid-phase extraction were obtained. Furthermore, the retention properties of the hydrophilic solutes on the adsorbents were also evaluated by LC. The hydrophilic solutes were retained on these adsorbents by a partition mode based on a hydrophilic interaction. The retention factors of the hydrophilic solutes showed good correlation to their log  P o/w (logarithm of octanol–water partition coefficient) and good separation based on hydrophilic interaction was obtained for nucleobases and nucleosides. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-1965-y Authors Yoshinori Inoue, Products Planning & Development Department, R&D Center, Nippon Filcon Co., Ltd., 2220 Ohmaru, Inagi-shi, Tokyo 206-8577, Japan Waka Kamichatani, Products Planning & Development Department, R&D Center, Nippon Filcon Co., Ltd., 2220 Ohmaru, Inagi-shi, Tokyo 206-8577, Japan Mitsuru Saito, Products Planning & Development Department, R&D Center, Nippon Filcon Co., Ltd., 2220 Ohmaru, Inagi-shi, Tokyo 206-8577, Japan Yasuyuki Kobayashi, College of Bioscience and Biotechnology, Chubu University, 1200 Matsumoto-cho, Kasugai-shi, Aichi 487-8501, Japan Atsushi Yamamoto, College of Bioscience and Biotechnology, Chubu University, 1200 Matsumoto-cho, Kasugai-shi, Aichi 487-8501, Japan Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    This review details the contribution of ion chromatography (IC) to environmental analysis. With reference to the problems usually encountered in environmental analysis (low concentrations to be detected and matrix interference), applications of IC in the analysis of inorganic cations in water and in the analysis of the platinum group elements (PGEs) in air particulate matter, and the advantages of this technique over more traditionally accepted analytical techniques will be discussed. Other current environmental topics, for example the occurrence of haloacetic acids (HAAs) in drinking water, will be covered, highlighting the importance of IC as an emerging powerful tool for monitoring HAAs, recognized also by the EPA that recently adopted it in a regulated method (Method 557). Content Type Journal Article Pages 1-14 DOI 10.1007/s10337-011-1967-9 Authors M. C. Bruzzoniti, Department of Analytical Chemistry, University of Torino, Via P. Giuria 5, 10125 Turin, Italy R. M. De Carlo, Department of Analytical Chemistry, University of Torino, Via P. Giuria 5, 10125 Turin, Italy C. Sarzanini, Department of Analytical Chemistry, University of Torino, Via P. Giuria 5, 10125 Turin, Italy Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A sensitive matrix solid-phase dispersion (MSPD)/gas chromatography-electron capture detector (GC-ECD) method was developed to determine cypermethrin residues in three tissues (muscle, liver, and gill) of crucian carp. Cypermethrin was simultaneously extracted by MSPD and determined by GC-ECD. The main parameters affecting extraction yield and selectivity, such as the type of solid adsorbent material, choice of elution solvents and their volume, were investigated to obtain interference-free extracts and quantitative cypermethrin recovery. Fortified recoveries in muscle, liver, and gill samples ranged from 84.9% to 106.1%, and relative standard deviations were 〈8% with fortification levels of 0.05–1 mg kg −1 . Detection limits were 1.4–2.1 μg kg −1 , and quantitation limits were 5.8–7.8 μg kg −1 . The proposed method was successfully applied to determination of cypermethrin in fish tissue samples. Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1921-x Authors Dongdong Zhao, College of Food Science and Techonolgy, Huazhong Agricultural University, Wuhan, 430070 People’s Republic of China Xiaoyu Liu, College of Food Science and Techonolgy, Huazhong Agricultural University, Wuhan, 430070 People’s Republic of China Wangrong Shi, College of Food Science and Techonolgy, Huazhong Agricultural University, Wuhan, 430070 People’s Republic of China Rongfei Liu, College of Food Science and Techonolgy, Huazhong Agricultural University, Wuhan, 430070 People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Increased throughput in medicinal chemistry has substantially increased the production of new chiral chemical entities with diverse structural features, requiring fast chiral screening strategies. In an effort to explore screening methods we have developed and evaluated gradients in polar organic and normal phase modes on three popular chiral stationary phases using a sample set of 19 racemic compounds. When compared, gradients performed on par with the isocratic methods besides proving to be advantageous in terms of speed of analysis and elution capacity. MS detection was successfully applied to the analysis of a pooled sample consisting 19 compounds to speed-up the screening process. Content Type Journal Article Pages 1-8 DOI 10.1007/s10337-011-1980-z Authors Mahesh Kumar Mone, Drug Discovery Facility, Advinus Therapeutics, Quantum Towers, Plot-9, Rajiv Gandhi Infotech Park, Phase-I Hinjewadi, Pune, 411 057 India K. B. Chandrasekhar, Department of Chemistry, Jawaharlal Nehru Technological University, College of Engineering, Anantapur, 515 002 India Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Alain Berthod (ed.): Chiral Recognition in Separation Methods. Mechanisms and Applications Content Type Journal Article Pages 1-2 DOI 10.1007/s10337-011-1976-8 Authors Colin F. Poole, Wayne State University, Detroit, MI USA Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description: Sanjay Kumur Sharma and Ackmez Mudhoo (Eds): Green Chemistry for Environmental Sustainability Content Type Journal Article Pages 1-1 DOI 10.1007/s10337-011-1942-5 Authors Ken Jones, Knutsford, Cheshire UK Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A rapid and simple quantitative method for the simultaneous determination of the four aflatoxins (AFs) B1, B2, G1 and G2 was developed using reverse homogeneous liquid–liquid extraction (RHLEE) and HPLC post-column derivatization-fluorescence (HPLC-FL) detection. The method based on the rapid extraction of AFs from a methanolic sample into chloroform after addition of water containing KBr, with a method we called reverse homogeneous liquid–liquid extraction. Recoveries were in the range of 88–125% and the limits of detection were between 0.001–0.042 ng g −1 for different AFs. Wheat and pistachio were chosen for the analysis of real samples and the method was also successfully applied to a FAPAS ® TEST MATERIAL (T04151). Content Type Journal Article Pages 1-4 DOI 10.1007/s10337-011-1981-y Authors Jalal Hassan, Department of Toxicology, Faculty of Veterinary Medicine, University of Tehran, Tehran, Iran Shahoo Habibi, International Goods Inspection Company, Tehran, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    Ultrasound-assisted headspace solid-phase microextraction (UA-HS-SPME) coupled to gas chromatography–mass spectrometry (GC–MS) has been used for analysis of volatile compounds in dry Tagetes minuta L. The highest extraction efficiency was achieved with a 100-μm polydimethylsiloxane (PDMS) fiber. Different experimental conditions, for example, type of fiber coating, sonication time, extraction time and temperature, and desorption time, were investigated. Thirty compounds were identified by use of this UA-HS-SPME–GC–MS method. Comparison of the method with the commonly used hydrodistillation (HD) method showed that the proposed method is simpler, needs much less sample, requires shorter extraction time and lower temperature, has high trapping ability, and extracts more volatile and thermally sensitive compounds. The major components identified by use of the method were e -ocimenone (10.3%), cis -β-ocimene (4.8%), α-terpinolene (8.4%), trans -caryophyllene (19.7%), germacrene- d (10.0%), and camphor (3.6%). Content Type Journal Article Pages 1-5 DOI 10.1007/s10337-011-1955-0 Authors Ali Reza Ghiasvand, Department of Chemistry, Lorestan University, Khoramabad, Iran Morasaalsadat Nasseri, Department of Chemistry, Lorestan University, Khoramabad, Iran Sara Farsizaeh, Department of Chemistry, Lorestan University, Khoramabad, Iran Mohammad Hadi Meshkatalsadat, Department of Chemistry, Lorestan University, Khoramabad, Iran Reza Sadeghi-Sarabi, Department of Chemistry, Lorestan University, Khoramabad, Iran Shahriar Shadabi, Department of Chemistry, Lorestan University, Khoramabad, Iran Mohammad Borzoei, Department of Chemistry, Lorestan University, Khoramabad, Iran Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893

Description:    A sensitive and specific liquid chromatography–electrospray ionization–tandem mass spectrometry method has been developed and validated for the identification and quantification of brivudine in human plasma using diclofenac as an internal standard. The method involves extraction with ethyl acetate. The analyte was separated on a C 18 column and analyzed in multiple reaction monitoring mode with a negative electrospray ionization interface using the [M–H] − ions, m / z 332.8→ m / z 80.9 for brivudine, m / z 293.6→ m / z 249.5 for diclofenac. The method was validated over the concentration range of 5.54–2,836 μg L −1 for brivudine. The intra-and inter-day precisions were less than 8.91% in terms of relative standard deviation (RSD), and the accuracy was within −4.22% in terms of relative error (RE). The lower limit of quantification (LLOQ) was 5.54 μg L −1 with acceptable precision and accuracy. There were almost no matrix effects. Recovery of brivudine spiked in drug-free plasma was higher than 77.17%. The method was used to study the pharmacokinetic profile of brivudine in human plasma after oral administration of brivudine tablets. Content Type Journal Article Pages 1-7 DOI 10.1007/s10337-011-2001-y Authors Xiang-Dong Peng, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Zhi-Rong Tan, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Hui-Zi Wu, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Gan Zhou, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Chen-Xian Guo, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Qi Pei, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Shan Cao, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Xiang-Guang Meng, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Yi-Cheng Wang, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Yao Chen, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Dong Guo, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Lan Fan, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Wei Zhang, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Hong-Hao Zhou, Pharmacogenetics Research Institute, Institute of Clinical Pharmacology, Central South University, Changsha, 410078 Hunan People’s Republic of China Journal Chromatographia Online ISSN 1612-1112 Print ISSN 0009-5893