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
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.
