ALBERT

Description: The quality control of Saussurea involucrata has been greatly improved by macroscopic and microscopic identification and chemical profiling described in Chinese Pharmacopoeia since 2005. However, these methods have their own limitations, e.g., their dependence on personal experience and expertise, and it is a huge challenge to identify closely related species that share similar or identical morphological characteristics and chemical profiles. A novel and generally accepted identification strategy is urgently needed as a complement to regulations for protecting the public health interests. In this work, a comprehensive chromatographic fingerprint method was developed and tested on 43 samples from four haplotypes of S. involucrata according to DNA barcoding. Three common patterns consisting of 20, 14, and 7 common peaks were generated by frequency filters of median, upper quartile, and 100%, respectively. Based on two formerly screened patterns, S. involucrata can be effectively identified from its five easily confused snow lotus species, including the most closely related plant (S. orgaadayi) in the orthogonal partial least-squares discriminant analysis (OPLS-DA) models. The model is supported by good R and Q coefficients. In addition, different haplotypes of S. involucrata can be discriminated in the OPLS-DA model using the 20 common peaks. Among them, peaks 9, 11, 16 (zaluzanin C), and 18 (dehydrocostus lactone) have been identified as fingerprint markers of S. involucrata via S-plots and VIP values (〉1). Additionally, peaks 19 and 20 were identified as linolenic acid and linoleic acid with anti-inflammatory activity, and they were isolated from the herb for the first time. Collectively, the chromatographic fingerprint of S. involucrata can be an effective and integrated method for the identification of authentic herbs from adulterant species or related plants, and discrimination of its different haplotypes provides an objective and reliable tool for quality control.

Description: Qing’e pills is clinically used for treating osteoporosis in postmenopausal women in China. Eucommiae Cortex and Psoraleae Fructus are the main herbs of Qing’e pills and are both required to be salt-processed. In order to study the influence of salt-processing on the tissue distribution of Qing’e pills, a UPLC-MS/MS method was established for studying the tissue distribution of 12 main bioactive ingredients of Qing’e pills in rats. The linear relationships of the 12 compounds in each tissue were good. The method was fully validated for its selectivity, accuracy, precision, stability, matrix effect, and extraction recovery. Then, the validated method was successfully applied for simultaneous determination of the 12 chemical components in Qing’e pills in tissues for the first time. Areas under the curve (AUC) results showed that, except for pinoresinol diglucoside, psoralen, and isopsoralen, the distribution of the other components was increased in the kidney, uterus, ovary, and testes. Relative targeting efficiency (RTE) results showed that all 12 chemical components targeted the kidney and sexual organs. The results indicated that the Eucommiae Cortex and Psoraleae Fructus after salt-processing could significantly increase the distribution of components to the kidney and generative organs.

Description: Dendrobe (Dendrobium spp.) is a traditional medicinal and edible food, which is rich in nutrients and contains biologically active metabolites. The quality and price of dendrobe are related to its geographical origins, and high quality dendrobe is often imitated by low quality dendrobe in the market. In this work, near-infrared (NIR) spectroscopy sensor combined with porphyrin and chemometrics was used to distinguish 360 dendrobe samples from twelve different geographical origins. Partial least squares discriminant analysis (PLSDA) was used to study the sensing performance of traditional NIR and tera-(4-methoxyphenyl)-porphyrin (TMPP)-NIR on the identification of dendrobe origin. In the PLSDA model, the recognition rate of the training and prediction set of the TMPP-NIR could reach 100%, which was higher than the 91.85% and 91.34% of traditional NIR. And the accuracy, sensitivity, and specificity of the TMPP-NIR sensor are all 1.00. The mechanism of TMPP improving the specificity of NIR spectroscopy should be related to the π-π conjugated system and the methoxy groups of TMPP interact with the chemical components of dendrobe. This study reflected that NIR spectrum with TMPP sensor was an effective approach for identifying the geographic origin of dendrobe.

Description: The widespread use of silver nanoparticles (AgNPs) and gold nanoparticles (AuNPs) in a wide variety of industrial as well as medical sectors is indisputable. This leads to a new concern about their presence in various environmental compartments. Since their negative effect and potential toxicity impact have been confirmed, analytical chemists focus on the development of different procedures for their reliable detection, identification, characterization, and quantification, not only in homogenous and simple matrices but also in complex environmental matrices. However, nanoparticles and their ionic species can coexist and their toxicity may differ; therefore, novel analytical approaches are necessary to monitor not only the nanoparticles but also their ionic species. The aim of this article is to bring a review of recent works where magnetic solid-phase extraction (MSPE) procedures in connection with spectrometric methods were used for separation/preconcentration and quantification of (1) silver and gold ions in various environmental samples, (2) AgNPs and AuNPs in real water samples in the presence of various coexisting ions, and (3) both species (it means Ag ions and AgNPs; Au ions and AuNPs) in real water samples. The results presented herein show the great analytical potential of MSPE procedures in connection with spectrometric methods used in these fields and can be helpful in guiding analytical chemists who aim to work on this subject.

Description: Objective. To establish a method for extraction and determination of antioxidant 264 (2,6-di-tert-butyl-4-methylphenol) in the brominated butyl rubber stopper for injection and migration study in recombinant potent antitumor and antivirus protein injection (Novaferon). Methods. Dichloromethane-ethanol was adopted as the extraction solvent during the process of reflux extraction of antioxidant 264 in the brominated butyl rubber stopper. High-performance liquid chromatography (HPLC) was used for the determination of the migration of antioxidant 264 to Novaferon. The mobile phase consisted of acetonitrile-water (80 : 20, v/v). The flow rate was 1.5 mL/min. The detection wavelength was 280 nm. Results. The linearity range was from 4.003 to 200.150 μg/mL (r2 = 0.99996), and the average recovery of antioxidant 264 was 97.8%. The applicability of the methodology was good, which can be used for the determination of antioxidant 264. The results indicated that antioxidant 264 was not detected in Novaferon after the accelerated test and three months of long-term test. Conclusion. The established validated method in this study can be used for the determination of antioxidant 264 in the rubber stopper, and the brominated butyl rubber stopper has good compatibility with Novaferon.

Description: Numerous countries have shown signs of environmental pollution to prioritize economic growth and benefits, leading to seriously contaminated waters. This work indicated the method to synthesize a green material, which could remove contaminants to protect the natural environment. The porosity and functionality effects of amine-functionalized activated carbon (AFAC) enhanced the removal of toxic heavy metals (THMs) in aqueous solution. The raw activated carbon (RAC) was thermally modified with ultrahigh pure nitrogen (UHPN) at 500°C and 1000°C and then amine-functionalized with coupling agent of aminopropyltriethoxysilane (APS). They were denoted as AFAC-5 and AFAC-10, respectively. The data showed an enhanced metal adsorption capacity of the AFACs, because the modification produced more desired porosity and increased amine functional groups. AFAC-10, modified at a higher temperature, showed much higher THM adsorption capacity than AFAC-5, modified at a lower temperature, and RAC. The adsorption capacity decreased in the following order: Ni 〉 Cd 〉 Zn, which was in good agreement with the increasing electronegativity and ionic potential and the decreasing atomic radius. The maximum THM adsorption capacity of AFAC-10 for Ni, Cd, and Zn was 242.5, 226.9, and 204.3 mg/g, respectively.

Description: Zinc is an essential trace element for animals in several biological processes, particularly in energy production, and it is acquired from food ingestion. In this context, a microplate-based fluorimetric assay was developed for simple, fast, and low-cost determination of zinc in pet food using 2,2′-((4-(2,7-difluoro-3,6-dihydroxy-4aH-xanthen-9-yl)-3-methoxyphenyl)azanediyl)diacetic acid (FluoZin-1) as fluorescent probe. Several aspects were studied, namely, the stability of the fluorescent product over time, the FluoZin-1 concentration, and the pH of reaction media. The developed methodology provided a limit of detection of 1 μg L−1 in sample acid digests, with a working range of 10 to 200 μg L−1, corresponding to 100–2000 mg of Zn per kg of dry dog food samples. Intraday repeatability and interday repeatability were assessed, with relative standard deviation values 

Description: A microfluidic chip with a microvalve based on a microhole array is proposed in this paper for the POCT of tumor marker proteins. In order to control the biochemical reaction time accurately and obtain a higher testing sensitivity, the parameters of the microhole array are optimized basing on the investigation of the effects of the variation of those parameters on the fluid rate and the residual liquid value in the microvalve region. By conducting liquid flow experiments using microvalves based on microhole arrays with varying microstructural parameters, the residual rate of reaction products is demonstrated to be proportional to the depth and diameter of the microholes and inversely proportional to the distance between the microhole centers. A comprehensive analysis indicates that a microhole depth of 95 μm, a microhole diameter of 230 μm, and a distance between microhole centers of 250 μm not only ensure a sufficiently long delay time, but also reduce the residual rate of reaction products, thereby providing an optimum microvalve performance that maximizes the detection efficiency and accuracy of microfluidic chips.

Description: Angelica Sinensis Radix (Danggui, DG) is one of the most commonly prescribed traditional Chinese medicines. The organic components include phthalides and phenolic acids. Meanwhile, inorganic elements play an important role in clinical effect. DG and its different parts have different effects. There is no relevant report on the analysis of organic compounds and inorganic elements among them. Therefore, ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry was developed for the simultaneous determination of 13 organic components (8 phthalides and 5 phenolic acids), and 8 inorganic elements were determined by inductively coupled plasma mass spectrometry. The contents of 32 samples were analyzed by orthogonal partial least squares discrimination analysis, hierarchical cluster analysis, and least-significant difference of one-way analysis of variance. The results showed that the differences were significant among DG and its different parts. 11 difference markers (Ca, Z-ligustilide, Mg, Mn, Fe, Na, K, Cu, Zn, coniferyl ferulate, and senkyunolide A) were obtained by variable importance for the project. These difference markers were some different among DG and its different parts, especially Z‐ligustilide, coniferyl ferulate, Mg, Zn, the differences were significant. This study can provide a reference for DG research.

Description: Athletes usually take nutritional supplements and perform the specialized training to improve the performance of sport. A quick assessment of their athletic status will help to understand the current physical function of athletes’ status and the effect of nutritional supplementation. Human urine, as one of the most important body indicators, is composed of many metabolites, which can provide effective monitoring information for physical conditions. In this study, temperature-dependent near-infrared spectroscopy (NIRS) technology was used to collect the spectra of athlete’s urine for evaluating the feasibility of rapidly detecting the exercise state of the basketball player. To obtain the detection results accurately, several chemometrics methods including principal component analysis (PCA), variables selection method of variable importance in projection (VIP), continuous 1D wavelet transform (CWT), and partial least square-discriminant analysis (PLS-DA) were employed to develop a classifier to distinguish the physical status of athletes. The optimal classifying results were obtained by wavelet-PLS-DA classifier, whose average precision, sensitivity, and specificity are all above 0.95, and the overall accuracy of all samples is 0.97. These results demonstrate that temperature-dependent NIRS can be used to rapidly assess the physical function of athlete’s status and the effect of nutritional supplementation is feasible. It can be believed that temperature-dependent NIR spectroscopy will obtain applications more widely in the future.