The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, whi...The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, which is based on a data-dependent acquisition of isotope ions and result verified by full scan mass spectrum. The distinguished advantage of data-dependent scan is rapidness because it requires minimum sample preparation, and all the necessary data can be obtained in one chromatographic run. In addition, it is highly sensitive and selective, allowing detection of trace metabolites even in the presence of complex biomatrix. As a result, four phase-Ⅰ（M1--M4） and four Phase-Ⅱ（M5--M8） metabolites of brodimoprim were identified in urine after the oral administration of hrodimoprim to Wistar rats. Their chemical structures were proposed based on the interpretation of their CID fragmentation characterizations and the metabolic pathway was exhibited in this article.展开更多
Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently...Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently further identified by nuclear magnetic resonance(NMR).Thin layer chromatography(TLC)was optimized based on the previous methods reported in the Chinese Pharmacopeia(2015 edition).Results The major compound was isolated from the natural material and identified as linoleic acid.A high performance liquid chromatography(HPLC)method with robust linearity(R2=0.9997),specificity,precision,stability,repeatability and recovery was developed for linoleic acid determination.TLC chromatogram was improved significantly after optimization for qualitative analysis.Conclusions The optimized TLC method is practical and can be adopted for quality control of Polygonati Rhizoma(Huang Jing,黄精).The levels of linoleic acid vary between species of Polygonati Rhizoma(Huang Jing,黄精),with Polygonatum cyrtonema Hua(Jiang Xing Huang Jing,姜型黄精)showing the highest contents.This study provides valuable information for quality control of Polygonati Rhizoma(Huang Jing,黄精).展开更多
Objective In order to analyze the active components in the extracts from Kaki Folium(KF),quantitative metabolomics approach was adopted to investigate the number of active components existing among the different extra...Objective In order to analyze the active components in the extracts from Kaki Folium(KF),quantitative metabolomics approach was adopted to investigate the number of active components existing among the different extracts and their variation.Methods LC-MS method was established for the quantitative determination of the active components taking the mixture with reference substance as tested sample.Results In terms of the number of active components and amount presented in the different tested samples of KF extracted by many types of solvents,variation was observed.But rutin,astragalin,and kaempferol were presented in all samples.Difference was found between the samples extracted from the products on market and from the raw materials of KF processed by polar solvents with different recipes.However,the three active components were found in all samples examined.Conclusion These results might be valuable as all information and could be used for the optimization of raw materials extraction procedure to enhance the productivity.展开更多
基金the National Natural Science Foundation of China(Nos.30630075 and 20675056)Natural Science Founda-tion of Tianjin City,China(No.07JCYBJC01600)
文摘The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, which is based on a data-dependent acquisition of isotope ions and result verified by full scan mass spectrum. The distinguished advantage of data-dependent scan is rapidness because it requires minimum sample preparation, and all the necessary data can be obtained in one chromatographic run. In addition, it is highly sensitive and selective, allowing detection of trace metabolites even in the presence of complex biomatrix. As a result, four phase-Ⅰ（M1--M4） and four Phase-Ⅱ（M5--M8） metabolites of brodimoprim were identified in urine after the oral administration of hrodimoprim to Wistar rats. Their chemical structures were proposed based on the interpretation of their CID fragmentation characterizations and the metabolic pathway was exhibited in this article.
基金We thank for the funding support from the National Standardization Construction in TCMs of China(No.ZYBZH-Y-HUN-23)National Key Research and Development Projects of China(No.2018YFC1707903)Key Research and Development Projects of Hunan Province(No.2018SK2119).
文摘Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently further identified by nuclear magnetic resonance(NMR).Thin layer chromatography(TLC)was optimized based on the previous methods reported in the Chinese Pharmacopeia(2015 edition).Results The major compound was isolated from the natural material and identified as linoleic acid.A high performance liquid chromatography(HPLC)method with robust linearity(R2=0.9997),specificity,precision,stability,repeatability and recovery was developed for linoleic acid determination.TLC chromatogram was improved significantly after optimization for qualitative analysis.Conclusions The optimized TLC method is practical and can be adopted for quality control of Polygonati Rhizoma(Huang Jing,黄精).The levels of linoleic acid vary between species of Polygonati Rhizoma(Huang Jing,黄精),with Polygonatum cyrtonema Hua(Jiang Xing Huang Jing,姜型黄精)showing the highest contents.This study provides valuable information for quality control of Polygonati Rhizoma(Huang Jing,黄精).
基金National Basic Research Plan (973 Plan) Foundation of China (2010CB735602)National Innovation Plan for New Drugs (2011ZX09304-002)
文摘Objective In order to analyze the active components in the extracts from Kaki Folium(KF),quantitative metabolomics approach was adopted to investigate the number of active components existing among the different extracts and their variation.Methods LC-MS method was established for the quantitative determination of the active components taking the mixture with reference substance as tested sample.Results In terms of the number of active components and amount presented in the different tested samples of KF extracted by many types of solvents,variation was observed.But rutin,astragalin,and kaempferol were presented in all samples.Difference was found between the samples extracted from the products on market and from the raw materials of KF processed by polar solvents with different recipes.However,the three active components were found in all samples examined.Conclusion These results might be valuable as all information and could be used for the optimization of raw materials extraction procedure to enhance the productivity.
