Change pattern and correlation analysis of macroscopic characteristics, active components and rancidness degrees of Armeniacae Semen Amarum in deterioration process / 中国中药杂志

To discuss the effect of deterioration on the quality of Armeniacae Semen Amarum by observing the changes of macroscopic characteristics, active components and rancidness degrees of Armeniacae Semen Amarum in deterioration process. The traditional macroscopic identification was used to observe, identify and classify the morphologic and organleptic characteristics of Armeniacae Semen Amarum. The contents of amygdalin and fatty oil(two representatives of active components) were detected by HPLC and general rule 0713 in Chinese Pharmacopoeia, respectively. Acid value and peroxide value of the samples were selected as the representative indices of different rancidness degrees, and the general rule 2303 was adopted as the method for quantitative analysis. Then principal component analysis(PCA), partial least square analysis discrimination analysis(PLS-DA) were further utilized to establish the discriminative models of samples with different rancidness degrees, and also to screen out the largest contribution factors. In sensory evaluation, Armeniacae Semen Amarum samples were divided into three groups: non-rancid, slightly-rancid, and noticeably-rancid. The color of seed coat, cotyledon and surface of noticeably-rancid samples was deepened, and the odor differed much from non-rancid samples. Average content of amygdalin and fatty oil in non-rancid samples was 4.12% and 67.77%, respectively, both meeting the requirements of Chinese Pharmacopoeia; and decreased to some extent in slightly-rancid samples. However, the content of amygdalin sharply dropped to 0.074% in noticeably-rancid samples. The acid value and peroxide value were increased significantly with the intensifying of the rancidness degree, from only 1.363 and 0.016 74 in non-rancid samples to 1.865 and 0.023 70 in slightly-rancid samples, even doubled in noticeably-rancid samples(2.167 and 0.033 82). The discriminative models established by PCA and PLS-DA could complete the task of distinguishing the non-rancid samples from noticeably-rancid ones. The contribution degree of amygdalin content as one of the input attributes of discriminative model was higher than 1. Rancidness affected the quality of Armeniacae Semen Amarum, resulting in appearance changes, decrease in content of active components, and increase in acid value and peroxide value. Obviously, noticeably-rancid samples were non-conforming to Chinese Pharmacopoeia and no longer suitable for medicinal use. Rancidness can significantly reduce the quality of Armeniacae Semen Amarum, and even could possibly produce toxicity, which should attach more attention.

Comparative study on the effect of Danggui-Chuanxiong herb pair on vasoactive substances and adhesion molecules in the serum of acute blood stasis in rats using PLS-DA and multi-attribute comprehensive index methods / 药学学报

We evaluated the effects of Danggui-Chuanxiong (GX) herb pair with different proportions (1∶0, 3∶2, 1∶1, 2∶3, 0∶1) and preparation methods (water extract W, alcohol extract A, and water-alcohol extracts WA) on vasoactive substances and endothelial cell adhesion molecules in the serum of acute blood stasis in rats. An acute blood stasis model was co-replicated by ice water bath and subcutaneous injection of epinephrine hydrochloride in rats. The expressions of vasoactive substances (arachidonic acid metabolites, coagulation-fibrin system index) and adhesion molecules in the serum were detected by enzyme linked immunosorbent assay method; the Spearman method was used to analyze the correlation of those detection indicators; the partial least squares-discriminant analysis and multi-attribute comprehensive index method were used to comprehensively evaluate the total effect of GX herb pair samples with different proportions and preparation methods on vasoactive substances and adhesion molecules. The experimental scheme was approved by the Animal Experimental Ethics Committee of the First Affiliated Hospital of Henan University of Chinese Medicine. The results showed that GX 1∶1_WA had the strongest effect on the improvement of vasoactive substances and adhesion molecules in the serum of acute blood stasis in rats (the total effect value was 6.96). When extraction method was same, the overall effect of GX 1∶1 had better effect than that of other proportions; when the proportion of GX was same, the total effects of GX_WA and GX_A were better than GX_W. The combination of Danggui and Chuanxiong can significantly improve the expressions of vasoactive substances and adhesion molecules in the serum of blood stasis in rats. But the action strength of GX herb pairs was different when the proportions and preparations of GX herb pair were different. These findings provide a basis for clinical rational application of GX herb pair, and lay the foundation for in-depth research on GX herb pair for treatment of blood stasis related diseases.

Quality evaluation of Hugan Tablets based on HPLC fingerprint and chemical pattern recognition / 中草药

Objective: To establish the HPLC fingerprint of Hugan Tablets and provide a scientific basis for the quality control of Hugan Tablets. Methods: HPLC method was adopted and using schizandrin as reference, and 10 batches of Hugan Tablets were determined. Similarity evaluation was performed by using Similarity Evaluation System for Fingerprint Chromatogram of TCM (2004A) to confirm the common peak. Pattern recognition analysis was performed using principal component analysis (PCA) and orthogonal partial least squares-discrimination analysis (OPLS-DA). Results: There were 22 common peaks in HPLC of 10 batches of samples. Schizandrin, saikosaponin a, saikosaponin c, saikosaponin d, schisandrin A, and schizandrin B were identified by chemical identification of the reference substance. The similarity of 10 batches of samples was higher than 0.97, which indicated that the overall quality of the drug was relatively stable. However, there were slight differences between the quality of different batches of drugs found by PCA, and they were mainly divided into two categories. Finally, OPLS-DA was used to screen out two main components that caused the quality differences in the batches, namely peak 12 (saikosaponin D) and peak 22. Conclusion: The construction of fingerprint of Hugan Tablets and chemical pattern recognition provides a practical and theoretical basis for the quality evaluation of Hugan Tablets, which can provide a scientific basis for manufacturers to control drug quality more efficiently and reasonably in drug production.

In vivo Breath Analysis by Extractive Electrospray Ionization-Mass Spectrometry for Investigation of Metabolic Responses to Traditional Chinese Medicine Massages / 分析化学

Traditional Chinese Medicine massage is a kind of physiotherapy which affects on specific parts of the body surface by means of training to regulate the function of the body to achieve the therapeutic effect. In this work,under positive detection model, the chemical fingerprint of exhaled breath from volunteers before and after receiving Traditional Chinese Medicine massage within m/z 50-1000 were detected by extractive electrospray ionization-mass spectrometry (EESI-MS). And through high resolution mass spectrometry analysis, the metabolites such as epinephrine (m/z 184. 0889), 3-(3-hydroxyphenyl) propionic acid (m/z 167.0615) and L-tryptophan (m/z 205. 0933) were successfully identified. Besides, chemical fingerprints of volunteers before and after receiving Traditional Chinese Medicine massage under different health condition were clearly differentiated via partial least squares discrimination analysis (PLS-DA). The results showed that Traditional Chinese Medicine massage could significantly change the metabolic process of volunteers. Moreover, it further indicated that the established method could provide a real time fashion to follow metabolic changes caused by Traditional Chinese Medicine massage.

Link between sortase A function and cariogenicity of Streptococcus mutans: a preliminary metabolomics analysis / 华西口腔医学杂志

<p><b>OBJECTIVE</b>This study intends to explore the mechanism underlying the support of sortase A (SrtA) of the cariogenicity of Streptococcus mutans (S. mutans).</p><p><b>METHODS</b>We performed a metabonomics study based on ¹H nuclear magnetic resonance spectroscopy (NMR), in which we compared the extracellular metabolites of wild-type S. mutans UA159 with those of its SrtA-deficient strain. Metabolite differences among strains were identified using a combination of principal component analysis and orthogonality partial least square discriminant analysis.</p><p><b>RESULTS</b>Several differences corresponding mostly to unknown metabolites were identified. Some amino acids such as leucine and valine (δ 0.92×10⁻⁶-1.20×10⁻⁶), lactic acid ( δ1.28×10⁻⁶), oxoglutaric acid (δ 3.00×10⁻⁶), and glycine (δ 3.60×10⁻⁶) differed among strains.</p><p><b>CONCLUSIONS</b>This work establishes the feasibility of using ¹H NMR-based metabonomics to provide leads for research into molecular factors that promote caries. The database of microbial metabolites should be also improved in further studies.</p>

Fingerprint study of Picrorhiza scrophulariiflora by UPLC coupled with chemometrics method / 中草药

Objective To establish the UPLC fingerprint for effective quality control and scientific evaluation of Picrorhiza scrophulariiflora. Methods The analysis was performed on Waters ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm), using acetonitrile-0.5% glacial acetic acid aqueous solution as mobile phase for gradient elution, with the flow rate at 0.3 mL/min, the column temperature at 32 ℃, and the detection wavelength at 295 nm. Total of 25 batches of P. scrophulariiflora and its adulterants were analyzed. Similarity evaluation combined with hierarchical clustering analysis (HCA) and principal components analysis (PCA) were used to evaluate the quality of herbs from different batches. Ultra-performance liquid chromatography- quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS) was used for qualitative analysis in the positive and negative ion modes. Results There were significant differences in fingerprint chromatogram among P. scrophulariiflora and its adulterants. There were 16 common peaks in UPLC fingerprint of 22 batches of P. scrophulariiflora, and 12 peaks among which were carried out for chemical components identification with the similarity at 0.939-0.998. Twenty-two samples could be classified into three clusters. The PCA result was consistent with that of HCA. The four symbolic compounds in samples were verified by PLS-DA analysis, which identified that No.1, 12, 9 peaks were picroside I, picroside III, and scrophenoside C. Conclusion The establishment of UPLC fingerprint and the recognition of chemical pattern of P. scrophulariiflora can provide a more comprehensive reference for the quality control of herbs.

Quality evaluation of Terminalia billerica based on HPLC fingerprint and multi-components simultaneous determination / 中草药

Objective: To establish the HPLC fingerprint and to determin gallic acid, methyl gallate, corilagin, and ellagic acid in Terminalia billerica, in order to provide the scientific foundation for quality control of T. billerica. Methods: The analysis was performed on Atlantic T3 (250 mm × 4.6 mm, 5 μm) C18 column, mobile phase was acetonitrile-0.2% glacial acetic acid aqueous solution with gradient elution, flow rate was 1.0 mL/min, injection size was 20 μL column, and temperature was maintained at 30 oC. The common mode of T. billerica HPLC fingerprint was established, the hidden information was analyzed in the fingerprint by Chemometrics, and the components in T. billerica by HPLC-MSn and quantitative analysis characteristic peaks were identified. Results: There were 21 common peaks in the diagram and the similarity of the fingerprints was over 0.9 in all 11 batches. The information of the 18 common peaks in T. billerica was summarized by HPLC-MSn technology. The samples were broadly divided into three kinds by principal component analysis and clustering analysis. The five key compounds were verified by partial least squares discriminant analysis method in quantitative analysis, and identified that the No.12 peak was chabulagic acid, and the average recoveries were in the range of 97.24%-98.58%. Conclusion: The HPLC fingerprint method and content determination method are reliable, accurate, rapid, simple, and reproducible, and this study could control the quality of T. billerica.