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