目的建立蒙药三臣丸中同时测定紫丁香苷,羟基红花黄色素A,芦丁,山柰酚-3-O-芸香糖苷,脱水红花黄色素B,胆酸和猪去氧胆酸共7种成分的一测多评技术方法(quantitative analysis of multi-components by single marker,QAMS)。方法以羟基红...目的建立蒙药三臣丸中同时测定紫丁香苷,羟基红花黄色素A,芦丁,山柰酚-3-O-芸香糖苷,脱水红花黄色素B,胆酸和猪去氧胆酸共7种成分的一测多评技术方法(quantitative analysis of multi-components by single marker,QAMS)。方法以羟基红花黄色素A为内参物,计算相对于其他6种成分的相对校正因子(relative correction factor,RCFs),并通过所得相对校正因子计算各个成分的含量,同时采用外标法测定该6种成分的含量,并比较2种方法所得计算结果的差异,以验证一测多评法的技术可行性和方法准确性。结果 10批三臣丸中7种成分含量的校正因子法与外标法计算结果无显著性差异。结论 QAMS可以作为一种简便准确的质量评价模式用于三臣丸中多种成分的定量测定,为蒙药三臣丸的质量控制提供新的参考依据。展开更多
In the present study, we developed a rapid, sensitive and efficient ultra high-performance liquid chromatography-tandem mass spectrometric(UPLC-Q-Exactive-MS) method, and six bioactive constituents in San-Chen-pill(SC...In the present study, we developed a rapid, sensitive and efficient ultra high-performance liquid chromatography-tandem mass spectrometric(UPLC-Q-Exactive-MS) method, and six bioactive constituents in San-Chen-pill(SCP), including cholic acid(CA), hyodeoxycholic acid(HDCA), hydroxysafflor yellow A(HSYA), kaempferol-3-O-rutinoside(KFR), anhydrosafflor yellow B(AHSYB) and syringin(SRG), in rat plasma after oral administration of San-Chen-pill, were simultaneously determined. Plasma samples were pretreated with methanol for protein precipitation. Chromatography separation was performed on a SHIMADZU of shim-pack GIST C18 column using a gradient mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution. A tandem mass spectrometric detection with an electrospray ion source(HESI) interface was conducted in negative ionization mode. For all the six analytes of interest, the calibration curves were linear within the concentration rage of 0.50–1280 ng/m L with r≥0.99. The intra-day and inter-day precisions(in terms of relative standard deviation, RSD) were all below 12.7% for all six analytes. Extraction recovery, matrix effect and stability data all met the acceptance criteria of FDA guideline for bioanalytical method validation. In addition, San-Chen-pill is a traditional Mongolian herbal medicine that has been prepared with three medicinal herbs, Calculus bovis, Carthamus tinctorius L. and Concretio silicea bambusae, and it shows potent anti-anginal activity in all preparations with in a ratio of 1:1:1. The pharmacokinetic parameters of San-Chen-pill were reported herein for the first time, and this developed method was successfully used in a pharmacokinetic study for San-Chen-pill.展开更多
文摘目的建立蒙药三臣丸中同时测定紫丁香苷,羟基红花黄色素A,芦丁,山柰酚-3-O-芸香糖苷,脱水红花黄色素B,胆酸和猪去氧胆酸共7种成分的一测多评技术方法(quantitative analysis of multi-components by single marker,QAMS)。方法以羟基红花黄色素A为内参物,计算相对于其他6种成分的相对校正因子(relative correction factor,RCFs),并通过所得相对校正因子计算各个成分的含量,同时采用外标法测定该6种成分的含量,并比较2种方法所得计算结果的差异,以验证一测多评法的技术可行性和方法准确性。结果 10批三臣丸中7种成分含量的校正因子法与外标法计算结果无显著性差异。结论 QAMS可以作为一种简便准确的质量评价模式用于三臣丸中多种成分的定量测定,为蒙药三臣丸的质量控制提供新的参考依据。
基金Natural Science Foundation of Inner Mongolia(Grant No.2017BS0806)Science Fund of Inner Mongolia Education Department(Grant No.NJZZ19089)
文摘In the present study, we developed a rapid, sensitive and efficient ultra high-performance liquid chromatography-tandem mass spectrometric(UPLC-Q-Exactive-MS) method, and six bioactive constituents in San-Chen-pill(SCP), including cholic acid(CA), hyodeoxycholic acid(HDCA), hydroxysafflor yellow A(HSYA), kaempferol-3-O-rutinoside(KFR), anhydrosafflor yellow B(AHSYB) and syringin(SRG), in rat plasma after oral administration of San-Chen-pill, were simultaneously determined. Plasma samples were pretreated with methanol for protein precipitation. Chromatography separation was performed on a SHIMADZU of shim-pack GIST C18 column using a gradient mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution. A tandem mass spectrometric detection with an electrospray ion source(HESI) interface was conducted in negative ionization mode. For all the six analytes of interest, the calibration curves were linear within the concentration rage of 0.50–1280 ng/m L with r≥0.99. The intra-day and inter-day precisions(in terms of relative standard deviation, RSD) were all below 12.7% for all six analytes. Extraction recovery, matrix effect and stability data all met the acceptance criteria of FDA guideline for bioanalytical method validation. In addition, San-Chen-pill is a traditional Mongolian herbal medicine that has been prepared with three medicinal herbs, Calculus bovis, Carthamus tinctorius L. and Concretio silicea bambusae, and it shows potent anti-anginal activity in all preparations with in a ratio of 1:1:1. The pharmacokinetic parameters of San-Chen-pill were reported herein for the first time, and this developed method was successfully used in a pharmacokinetic study for San-Chen-pill.
