Quality evaluation of Commelina communis from different origins based on multicomponent content determination combined with chemometrics / 中国中药杂志

This research established a high-performance liquid chromatography(HPLC) method for simultaneous determination of isoorientin, orientin, vitexin, and isovitexin in Commelina communis to conduct content difference analysis and quality evaluation of 62 batches of C. communis from different origins. The HPLC content determination was performed on a Dikma Platisil ODS chromatographic column(4.6 mm×250 mm, 5 μm), with acetonitrile-0.1% formic acid(14∶86) as the mobile phase. The detection wavelength was set at 348 nm, the flow rate was 1.0 mL·min~(-1), and the column temperature was 35 ℃. The differences in origins and quality of 62 batches of C. communis were studied by chemometrics. The results showed that the determination of four components mani-fested a good linear relationship in the range of mass concentration(r>0.999 9), and the average recovery rate was 96.17%-103.0%. The relative standard deviations(RSDs) of precision, stability, and repeatability were all less than 2.0%. The content of four components from high to low was isoorientin>isovitexin>orientin>vitexin. Forty-seven batches of C. communis with clear origins were classified into six categories by chemometrics. C. communis from different origins had different qualities. Generally, C. communis from Western China, Central China, and South of China had superior qualities. The HPLC method established in this study is specific, simple, and efficient, which provides references for the comprehensive evaluation of the quality of C. communis. The chemometrics shows that the qualities of C. communis from different origins are largely different. Isoorientin can be used as an index to determine the content of C. communis, and its content limit should be set no less than 0.023%.

Comprehensive quality evaluation of Tangwei capsule based on HPLC-QAMS multi-index quantitative determination combined with chemometrics and EW-TOPSIS method / 浙江大学学报·医学版

OBJECTIVES@#To detect the contents of Tangwei capsule main components with high performance liquid chromatography-quantitative analysis of multicomponents by single marker (HPLC-QAMS) method and to evaluate the quality with chemometrics and entropy weight-technique for order preference by similarity to an ideal solution (EW-TOPSIS).@*METHODS@#A symmetry C18 column and 0.1% formic acid-acetonitrile as mobile phase were used for HPLC of Tangwei capsule. The contents of 3'-hydroxypuerarin, puerarin, 3'-methoxypuerarin, methylnissolin-3-O-glucoside, calycosin, formononetin, rosmarinic acid, salvianolic acid B, dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ, tanshinone ⅡA and cucurbitacin B in 15 batches of Tangwei capsule were determined simultaneously. The quality differences of 15 batches of samples were analyzed by chemometrics and EW-TOPSIS.@*RESULTS@#The HPLC-UV showed that 13 components had good linear relationships in corresponding concentration ranges (r≥0.9991). The relative standard deviations (RSD) of precision, repeatability and stability were all less than 2.00%. The average recovery rates were between 96.86% and 100.13%, and RSD were all less than 2.00%. Cluster analysis showed that 15 batches of samples were clustered into 3 groups. Partial least squares-discriminant analysis showed that salvianolic acid B, formononetin, puerarin, 3'-methoxypuerarin and rosmarinic acid were the main potential markers affecting the quality of Tangwei capsule. EW-TOPSIS analysis showed that the quality of S12-S15 was superior.@*CONCLUSIONS@#The analytical method established in this study can be used for the comprehensive evaluation of the quality of Tangwei capsule to provide laboratory support for its quality control and overall evaluation.

Dynamic changes of volatile components in Forsythia suspensa at different harvest periods based on GC-MS and chemometrics analysis / 中国中药杂志

Forsythiae Fructus is the dried fruit of Forsythia suspensa and the volatile compounds are its main bioactive components. According to the different harvest periods, F. suspensa can be divided into Qingqiao(mature F. suspensa) and Laoqiao(ripe F. suspensa). To investigate dynamic changes of volatile components in Qingqiao and Laoqiao samples collected at different periods, the present study extracted and analyzed the total volatile oils in Qingqiao and Laoqiao samples(four harvest periods for Qingqiao and two for Laoqiao) by steam distillation method. The results indicated that the content of volatile oils in F. suspensa samples at different harvest periods was significantly different. The content of volatile oils in Qingqiao samples(except those harvested in the first period) was higher than that of Laoqiao, and the content of volatile oils in both Qingqiao and Laoqiao increased with the harvest period. Furthermore, volatile compounds in F. suspensa were qualitatively analyzed by the gas chromatography-mass spectrometry(GC-MS), and 28 volatile compounds were identified. Chemometrics analyses including principal component analysis(PCA) and partial least squares discriminant analysis(PLS-DA) were further applied to explore differential markers and dynamic changes of volatile components in Qingqiao and Laoqiao samples at different harvest periods. Finally, four volatile compounds, including α-pinene, sabinene, β-pinene, and 4-terpenol were selected as potential differential markers. The relative content of α-pinene and 4-terpenol was consistent with that of total volatile oils in the changing trend.

Multi-index components of Scutellariae Barbatae Herba according to UHPLC-QTRAP-MS coupled with chemometrics / 中国中药杂志

The present study developed an ultra-fast liquid chromatography coupled with triple quadrupole-linear ion trap composite mass spectrometry(UHPLC-QTRAP-MS) to simultaneously determine the content of potential active components in Scutellariae Barbatae Herba and also to provide a reference approach for screening out the differential quality control components among different batches of Scutellariae Barbatae Herba. Chromatographic separations were conducted on a Thermo Acclaim~(TM) RSLC 120 C_(18) column(3.0 mm×100 mm, 2.2 μm) in a gradient program. The mobile phase consisted of 0.1% aqueous formic acid and acetonitrile, and the column temperature was maintained at 40 ℃. The flow rate was 0.4 mL·min~(-1) and the injection volume was 2 μL. The targeted compounds were monitored in the multiple reaction monitoring(MRM) mode. The acquired data were processed by hierarchical cluster analysis(HCA) and partial least square discriminant analysis(PLS-DA). Sixteen compounds all showed good linear relationship within the corresponding linear ranges and the R~2 values were all higher than 0.993 2. The RSDs of precision, repeatability, and stability were less than or equal to 3.7%. Mean recovery rates were in the range of 95.67% and 104.8% with RSDs≤3.2%. According to HCA and PLS-DA, all samples were clustered into four categories. Scutellarin, acteoside, scutellarein, and scutebarbatine X(VIP>1) were considered as differential chemical markers in the four categories. In conclusion, the developed method can be used for the simulta-neous determination of the multiple components and quality control of Scutellariae Barbatae Herba.

FT-NIR associado a método quimiométrico para discriminar resíduos de antimicrobianos e antiparasitário no leite / FT-NIR coupled to chemometric method to discriminate antimicrobial and antiparasitic residues in milk

Introdução: O leite é um dos alimentos mais consumidos pelos seres humanos. Proteínas, vitaminas, gordura, carboidratos e sais minerais fazem parte de sua composição e desempenham importantes funções para a nutrição humana. A prática de adulteração no leite é antiga e ainda se faz presente nos dias de hoje em diversos países, inclusive no Brasil. A fim de obter lucro maior, alguns fornecedores costumam adicionar ao leite: água, amido, citrato, ureia, soda cáustica, cloreto de sódio, sacarose, soro do leite, melamina e outros componentes. No entanto, ainda há outro problema, o da contaminação do leite por medicamentos veterinários. Estes podem causar danos à saúde do consumidor e prejuízos para a produção de seus derivados. Objetivo: O presente trabalho propõe uma metodologia que permite detectar de maneira rápida a presença de resíduos de medicamentos veterinários em leites, dentro do limite máximo de resíduos de cada droga. Métodos: Fez-se o uso da espectroscopia no infravermelho próximo por transformada de Fourier associada à análise de componentes principais. A espectroscopia no infravermelho tem sido utilizada não somente para a autenticidade de laticínios, mas para determinar sua qualidade. Resultados: Conseguiu-se detectar resíduos de penicilina, oxitetraciclina e enrofloxacino, e também do antiparasitário ivermectina nas amostras de leites. Conclusão: A metodologia detectou de maneira rápida e precisa os resíduos das drogas analisadas, mesmo em concentrações muito baixas. Assim, é uma opção a outras existentes, já utilizadas para tal objetivo. (AU)

Introduction: Milk is one of the most consumed foods by humans. Proteins, vitamins, fat, carbohydrates and minerals are part of its composition and play important roles in human nutrition. The practice of adulteration in milk is old and is still present today in several countries, including Brazil. In order to obtain a higher profit, some suppliers usually add to the milk: water, starch, citrate, urea, caustic soda, sodium chloride, sucrose, whey, melamine and other components. However, there is still another problem, that of contamination of milk by veterinary medicines. These can cause damage to the health of the consumer and damage to the production of its derivatives. Objective: The present work proposes a methodology that allows to quickly detect the presence of residues of veterinary medicines in milk, within the maximum residue limit of each drug. Methods: The use of spectroscopy in the near infrared by Fourier transform associated with the analysis of principal components was used. Infrared spectroscopy has been used not only for the authenticity of dairy products, but to determine their quality. Results: It was possible to detect residues of penicillin, oxytetracycline and enrofloxacin, and also of the antiparasitic ivermectin in the milk samples. Conclusion: The methodology fastly and accurately detected the residues of the analyzed drugs, even in very low concentrations. Thus, it is an option to other existing ones, already used for this purpose. (AU)

UV-Visible Chemometrics Approach for the Determination of Selected Adulterants in Claimed Premixed Coffee

@#Introduction: Adulterated premixed coffees have turned into an issue in Malaysia lately and have caught the eye of the authorities due to death reports linked to these products. The major cause of this issue is reported that these premixed coffees have passed food inspection test and eventually released to the market for public consumption. These coffees were claimed to be spiked with several sexual enhancers like sildenafil, tadalafil, and vardenafill, which are common drugs used to treat erectile dysfunction. Methods: Chemometrics approach using UV-Vis spectroscopy was developed to detect the selected sexual enhancer drugs found in commercial coffees by employing SIMCA-P software for the multivariate statistical analysis. Seven brands of coffee samples were purchased from local stores, and 30 sachets each were tested, hence totalling to 210 samples. Each sample was named H, J, G, W, N, T, and K, respectively. Results: Three multivariate models were generated, namely principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), and partial least squares discriminant analysis (PLSDA). OPLS-DA was selected as the best model for the overall results as it displayed minimal discriminate. Sildenafil, tadalafil, and vardenafil were detected in sample H, while vardenafil in brand J, and none in samples G, W, N, T, and K. Conclusion: OPLS-DA analysis showed discrimination for the sexual enhancer drugs in two brands of premixed coffee. The UV-Vis spectroscopy-based chemometrics method proved to be reliable and efficient in determining the selected drugs, as well as in saving time and cost.