目的通过高效液相色谱-二极管阵列检测-串联质谱（HPLC-DAD-MS/MS）法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料（金胺O、金橙Ⅱ、胭脂红等）。方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomen...目的通过高效液相色谱-二极管阵列检测-串联质谱（HPLC-DAD-MS/MS）法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料（金胺O、金橙Ⅱ、胭脂红等）。方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomenon Luna C18色谱柱（250 mm×4.6 mm,5μm）;以乙腈-0.05 mol/L醋酸铵为流动相,梯度洗脱;体积流量1 m L/min;柱温40℃;检测波长400~700 nm。MS分析采用ESI电离源;干燥气温度350℃,体积流量10 L/min;雾化气压力241.3 k Pa;源电压4 k V。结果所有样品均检测出合成染料,谱库匹配度均大于99.8。结论该方法准确快速,可用于中药中合成染料筛查。展开更多
建立止咳平喘类中药制剂中非法添加的12种化学药品的快速筛选方法。采用液相色谱-串联质谱法,以Kromasil100-5C18(250 mm×4.6 mm,5μm)为分析柱,流动相采用0.3%甲酸铵(用甲酸调至p H 2.97)和甲醇进行梯度洗脱,电喷雾电离(ESI)、全...建立止咳平喘类中药制剂中非法添加的12种化学药品的快速筛选方法。采用液相色谱-串联质谱法,以Kromasil100-5C18(250 mm×4.6 mm,5μm)为分析柱,流动相采用0.3%甲酸铵(用甲酸调至p H 2.97)和甲醇进行梯度洗脱,电喷雾电离(ESI)、全扫描一级质谱和全扫描二级质谱扫描方式,对止咳平喘类中药制剂中非法添加的12种化学药品进行筛选分析。建立了快速分离、检测止咳平喘类中药制剂中非法添加的12种化学药品的方法,检测限低于50 ng。该方法专属性强、灵敏度高,适用于止咳平喘类中药制剂中非法添加化学药品的筛选及确证工作。展开更多
Objective To evaluate the quality of Psoralea corylifolia collected from 12 provinces of China. Methods An HPLC-DAD-MS/MS method was used to identify, determine, and estimate 14 representative bioactive compounds in P...Objective To evaluate the quality of Psoralea corylifolia collected from 12 provinces of China. Methods An HPLC-DAD-MS/MS method was used to identify, determine, and estimate 14 representative bioactive compounds in P. corylifolia. Then on the basis of the content data, the chemometrics method was used to differentiate 20 samples from different regions. Results The quality of P. corylifolia from 12 different provinces of China was evaluated by this method. Though the samples showed similar profiles, content of the detected markers varied significantly in different regions and batches. According to the results of the hierarchical cluster analysis and principle component analysis, it can be concluded that the samples from different origins could be clustered reasonably into two groups, as well as successfully distinguished. Conclusion A simple and reliable new method which used HPLC-DAD-MS/MS and chemometrics has been developed to characterize, classify, and control the quality of P. corylifolia.展开更多
Objectives To develop a high-performance liquid chromatography （HPLC） tandem mass spectrometry method for screening and identifying the multiple constituents in the complex Chinese materia medica （CMM） formulation...Objectives To develop a high-performance liquid chromatography （HPLC） tandem mass spectrometry method for screening and identifying the multiple constituents in the complex Chinese materia medica （CMM） formulation Sini Decoction. Methods The chemical constituents in Sini prescription as an entirety were isolated and analyzed by HPLC coupled with electrospray ionization ion-trap mass spectrometry （ESI-IT-MS） in order to clarify the chemical components of Sini Decoction and explore the chemical methods of studying CMM prescriptions. Results Twenty-five compounds were isolated from the water extract of this decoction. Through chemical and spectral analyses, the structures of 20 compounds were elucidated, including 15 flavonoids, one triterpene, two coumarins, and two other types of compounds. By using HPLC-DAD-MSn technique, the MSn cleavage behaviors of the flavonoids have been summarized as well as the origin of the isolated compounds was assigned. Conclusion The phytochemical compositon of Sini prescription is tentatively characterized by HPLC-DAD-ESI-IT-MS.. The results of the experiments demonstrate that the combination of HPLC and ESI-MSn is a sensitive and effective tool for rapidly investigating the complex CMM formulations.展开更多
文摘目的通过高效液相色谱-二极管阵列检测-串联质谱（HPLC-DAD-MS/MS）法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料（金胺O、金橙Ⅱ、胭脂红等）。方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomenon Luna C18色谱柱（250 mm×4.6 mm,5μm）;以乙腈-0.05 mol/L醋酸铵为流动相,梯度洗脱;体积流量1 m L/min;柱温40℃;检测波长400~700 nm。MS分析采用ESI电离源;干燥气温度350℃,体积流量10 L/min;雾化气压力241.3 k Pa;源电压4 k V。结果所有样品均检测出合成染料,谱库匹配度均大于99.8。结论该方法准确快速,可用于中药中合成染料筛查。
基金Ministry of Science and Technology of China (No 973: 2005CB523404)
文摘Objective To evaluate the quality of Psoralea corylifolia collected from 12 provinces of China. Methods An HPLC-DAD-MS/MS method was used to identify, determine, and estimate 14 representative bioactive compounds in P. corylifolia. Then on the basis of the content data, the chemometrics method was used to differentiate 20 samples from different regions. Results The quality of P. corylifolia from 12 different provinces of China was evaluated by this method. Though the samples showed similar profiles, content of the detected markers varied significantly in different regions and batches. According to the results of the hierarchical cluster analysis and principle component analysis, it can be concluded that the samples from different origins could be clustered reasonably into two groups, as well as successfully distinguished. Conclusion A simple and reliable new method which used HPLC-DAD-MS/MS and chemometrics has been developed to characterize, classify, and control the quality of P. corylifolia.
文摘Objectives To develop a high-performance liquid chromatography （HPLC） tandem mass spectrometry method for screening and identifying the multiple constituents in the complex Chinese materia medica （CMM） formulation Sini Decoction. Methods The chemical constituents in Sini prescription as an entirety were isolated and analyzed by HPLC coupled with electrospray ionization ion-trap mass spectrometry （ESI-IT-MS） in order to clarify the chemical components of Sini Decoction and explore the chemical methods of studying CMM prescriptions. Results Twenty-five compounds were isolated from the water extract of this decoction. Through chemical and spectral analyses, the structures of 20 compounds were elucidated, including 15 flavonoids, one triterpene, two coumarins, and two other types of compounds. By using HPLC-DAD-MSn technique, the MSn cleavage behaviors of the flavonoids have been summarized as well as the origin of the isolated compounds was assigned. Conclusion The phytochemical compositon of Sini prescription is tentatively characterized by HPLC-DAD-ESI-IT-MS.. The results of the experiments demonstrate that the combination of HPLC and ESI-MSn is a sensitive and effective tool for rapidly investigating the complex CMM formulations.
