A global quality control method based on high performance liquid chromatography(HPLC)coupled with diode array detection(DAD),single quadrupole mass spectrometry(MS)and time-of-flight mass spectrometry(TOFMS)was develo...A global quality control method based on high performance liquid chromatography(HPLC)coupled with diode array detection(DAD),single quadrupole mass spectrometry(MS)and time-of-flight mass spectrometry(TOFMS)was developed for simultaneous determination of seven major components(mangiferin,neomangiferin,timosaponin E1,timosaponin E,timosaponin BⅡ,timosaponin BⅢ,and timosaponin AⅢ)and identification of most components in extracts of Rhizoma Anemarrhenae(RA).HPLC analysis was performed on an Agilent SB-C18 column(4.6 mm×150 mm,5 μm)by gradient elution using acetonitrile and water-acetic acid(100∶0.05,v/v)as the mobile phase.Seven major components in RA were successfully separated.This quantitative method was fully validated in respect of the following performance criteria:linearity,precision,repeatability,stability,accuracy,limits of detection(LOD)and quantification(LOQ).A formula database of known compounds in RA was established,against which,most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS.This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China.This global quality control method,which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components,is suitable for routine quantification and comprehensive quality control of RA.展开更多
Objective:To investigate the effect of Rhizoma Anemarrhenae extract on glucose and lipid metabolism in diabetic mice,and provide basis for follow-up research.Methods:The method of streptozotocin combined with high-fat...Objective:To investigate the effect of Rhizoma Anemarrhenae extract on glucose and lipid metabolism in diabetic mice,and provide basis for follow-up research.Methods:The method of streptozotocin combined with high-fat diet was used to replicate the diabetes model in this study.After continuous intragastric administration for 6 weeks,the effects of Rhizoma Anemarrhenae extract on body weight,blood sugar,blood lipids,serum insulin and the organ index in diabetic mice were detected.Results:The fasting blood glucose and blood lipids(serum total cholesterol,triglyceride,low density lipoprotein cholesterol levels)of the Rhizoma Anemarrhenae group of mice were significantly decreased,which was statistically significant compared with the model group.The area under the curve of the Rhizoma Anemarrhenae group is significantly smaller than that of the model group,and the result is statistically significant.Rhizoma Anemarrhenae can increase serum insulin levels in diabetic mice,which is statistically significant compared with the model group.Compared with the model group,the liver,spleen,kidney and pancreas indexes of the Rhizoma Anemarrhenae group are significantly reduced.Conclusion:The extract of Rhizoma Anemarrhenae can significantly reduce blood glucose concentration,lower blood lipid levels,promote serum insulin secretion,and protect liver,kidney,spleen,pancreas and other tissues and organs.展开更多
Two novel steroidal saponins（timosaponin BⅢ-a,timosaponin BⅢ-b） together with a known steroidal saponin（timosaponin BⅡ-b） were prepared by the dilute acid hydrolysis of timosaponin BⅢ.Their structures were elu...Two novel steroidal saponins（timosaponin BⅢ-a,timosaponin BⅢ-b） together with a known steroidal saponin（timosaponin BⅡ-b） were prepared by the dilute acid hydrolysis of timosaponin BⅢ.Their structures were elucidated by means of 1D,2D NMR and TOF-MS spectral analysis.展开更多
Objective:Gegen Qinlian decoction(GQD)is a classical traditional Chinese medicine formulation which has been used for almost 2000 years.At Guang'anmen Hospital,Beijing,a modified GQD version(m GQD)with seven inste...Objective:Gegen Qinlian decoction(GQD)is a classical traditional Chinese medicine formulation which has been used for almost 2000 years.At Guang'anmen Hospital,Beijing,a modified GQD version(m GQD)with seven instead of four herbal ingredients has been applied to treat Type 2 diabetes.Quality control is a crucial prerequisite for the therapeutic application of herbal medicines.For the identification of products derived from classical GQD,the Chinese Pharmacopeia requires the analysis of only three marker compounds.Because m GQD is a more complex mixture containing seven herbs and hundreds of constituents,the pharmacopoeia method for GQD is inadequate.Materials and Methods:A more comprehensive characterization of the formula's constituents has been developed using ultra-high-performance liquid chromatography-diode array detection(UHPLC-DAD)-Q-Exactive-mass spectrometry(MS)in electrospray ionization positive and negative mode.Moreover,a new method for the fingerprint analysis of m GQD via high-performance thin-layer chromatography(HPTLC)has been established.Results:Altogether,91 compounds have been assigned to their originating plants and 84 substances were identified either by comparison with authentic references or with data from the literature.The HPTLC method is based on the application of two different mobile phases and is able to detect both lipophilic and hydrophilic constituents of m GQD.Conclusions:The modified GQD was extensively characterized by UHPLC combined with DAD and Q-Exactive Orbitrap high-resolution MS detection,leading to the assignment and identification of compounds present in the decoction.In addition,a new method for the fingerprint analysis of the m GQD using HPTLC was established,which allows fast and simple identification of the herbal ingredients in the mixture.展开更多
基金supported by the National Science and Technology Supporting Program(No.2006BAI08B03-07)the National Natural Science Foundation of China(No.30873196)
文摘A global quality control method based on high performance liquid chromatography(HPLC)coupled with diode array detection(DAD),single quadrupole mass spectrometry(MS)and time-of-flight mass spectrometry(TOFMS)was developed for simultaneous determination of seven major components(mangiferin,neomangiferin,timosaponin E1,timosaponin E,timosaponin BⅡ,timosaponin BⅢ,and timosaponin AⅢ)and identification of most components in extracts of Rhizoma Anemarrhenae(RA).HPLC analysis was performed on an Agilent SB-C18 column(4.6 mm×150 mm,5 μm)by gradient elution using acetonitrile and water-acetic acid(100∶0.05,v/v)as the mobile phase.Seven major components in RA were successfully separated.This quantitative method was fully validated in respect of the following performance criteria:linearity,precision,repeatability,stability,accuracy,limits of detection(LOD)and quantification(LOQ).A formula database of known compounds in RA was established,against which,most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS.This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China.This global quality control method,which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components,is suitable for routine quantification and comprehensive quality control of RA.
基金This study was supported by the Key Laboratory of Pharmacology and Toxicology of Traditional Chinese Medicine in Gansu Province(ZDSYS-KJ-2018-007)the 2020 Gansu Provincial Higher Schools Industry Support and Guidance Project(2020C-9)Gansu University of Chinese Medicine Introduced Talent Research Startup Fund Project(2016YJRC-03,2016YJRC-06).
文摘Objective:To investigate the effect of Rhizoma Anemarrhenae extract on glucose and lipid metabolism in diabetic mice,and provide basis for follow-up research.Methods:The method of streptozotocin combined with high-fat diet was used to replicate the diabetes model in this study.After continuous intragastric administration for 6 weeks,the effects of Rhizoma Anemarrhenae extract on body weight,blood sugar,blood lipids,serum insulin and the organ index in diabetic mice were detected.Results:The fasting blood glucose and blood lipids(serum total cholesterol,triglyceride,low density lipoprotein cholesterol levels)of the Rhizoma Anemarrhenae group of mice were significantly decreased,which was statistically significant compared with the model group.The area under the curve of the Rhizoma Anemarrhenae group is significantly smaller than that of the model group,and the result is statistically significant.Rhizoma Anemarrhenae can increase serum insulin levels in diabetic mice,which is statistically significant compared with the model group.Compared with the model group,the liver,spleen,kidney and pancreas indexes of the Rhizoma Anemarrhenae group are significantly reduced.Conclusion:The extract of Rhizoma Anemarrhenae can significantly reduce blood glucose concentration,lower blood lipid levels,promote serum insulin secretion,and protect liver,kidney,spleen,pancreas and other tissues and organs.
基金the National Science & Technology Major Project"Key New Drug Creation and Manufacturing Program",China(Nos2009ZX09301-001,2009ZX09102-121,and 2009ZX09501-030)the State Key Program of National Natural Science Foundation of China(Nos81030065 and 20805054)
文摘Two novel steroidal saponins（timosaponin BⅢ-a,timosaponin BⅢ-b） together with a known steroidal saponin（timosaponin BⅡ-b） were prepared by the dilute acid hydrolysis of timosaponin BⅢ.Their structures were elucidated by means of 1D,2D NMR and TOF-MS spectral analysis.
基金financially supported by the Austrian Federal Ministry of Education,Science and Research(402.000/00012-WF/V/6/2016),Vienna,Austriaby the China Academy of Chinese Medical Sciences as a“Belt and Road”special international cooperation project(GH2017-03-06),Beijing,Chinaby the Key Project of the National Natural Science Foundation(No.81430097),Beijing,China。
文摘Objective:Gegen Qinlian decoction(GQD)is a classical traditional Chinese medicine formulation which has been used for almost 2000 years.At Guang'anmen Hospital,Beijing,a modified GQD version(m GQD)with seven instead of four herbal ingredients has been applied to treat Type 2 diabetes.Quality control is a crucial prerequisite for the therapeutic application of herbal medicines.For the identification of products derived from classical GQD,the Chinese Pharmacopeia requires the analysis of only three marker compounds.Because m GQD is a more complex mixture containing seven herbs and hundreds of constituents,the pharmacopoeia method for GQD is inadequate.Materials and Methods:A more comprehensive characterization of the formula's constituents has been developed using ultra-high-performance liquid chromatography-diode array detection(UHPLC-DAD)-Q-Exactive-mass spectrometry(MS)in electrospray ionization positive and negative mode.Moreover,a new method for the fingerprint analysis of m GQD via high-performance thin-layer chromatography(HPTLC)has been established.Results:Altogether,91 compounds have been assigned to their originating plants and 84 substances were identified either by comparison with authentic references or with data from the literature.The HPTLC method is based on the application of two different mobile phases and is able to detect both lipophilic and hydrophilic constituents of m GQD.Conclusions:The modified GQD was extensively characterized by UHPLC combined with DAD and Q-Exactive Orbitrap high-resolution MS detection,leading to the assignment and identification of compounds present in the decoction.In addition,a new method for the fingerprint analysis of the m GQD using HPTLC was established,which allows fast and simple identification of the herbal ingredients in the mixture.
