The present study was designed to develop and validate a rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with tandem mass spectrometry(UHPLC-MS/MS) method for the simultaneous deter...The present study was designed to develop and validate a rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with tandem mass spectrometry(UHPLC-MS/MS) method for the simultaneous determination of five major active constituents in the traditional Chinese medicinal preparation Xingxiong injection(XXI) in rat plasma, including quercetin 3-O-rutinoside(QCR), kaempferol 3-O-rutinoside(KFR), isorhamnetin 3-O-rutinoside(ISR), bilobalide(BB), and ligustrazine(LGT). The plasma samples were pretreated by protein precipitation with acetonitrile. The chromatographic separation was achieved on a Waters Symmetry C18 analytical column(2.1 mm × 100 mm, 3.5 mm) with a mobile phase of 0.1% aqueous formic acid(A)-acetonitrile(B). Quantitation of the five bioactive constituents was achieved. Naringin was used as the internal standard(IS). All the calibration curves showed good linearity(r > 0.996) over the concentration range, with the lowest limit of quantification(LLOQ) between 2-18 ng·m L^(-1). The intraand inter-day accuracy and precision of the analytes were both within acceptable limits. Moreover, satisfactory extraction recoveries(90.92%-104.03%) were obtained by protein precipitation. The validated method was successfully applied to a pharmacokinetic study of XXI in rats after intravenous administration at three doses. The pharmacokinetic parameters of the five compounds varied in a dose-dependent manner within the tested dosage range. The present study was the first report of pharmacokinetic study for XXI.展开更多
基金financially supported from National Natural Science Foundation of China(Nos.81673569,and 81473343)Program for New Century Excellent Talents in University(No.NECT-13-1034)a Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions
文摘The present study was designed to develop and validate a rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with tandem mass spectrometry(UHPLC-MS/MS) method for the simultaneous determination of five major active constituents in the traditional Chinese medicinal preparation Xingxiong injection(XXI) in rat plasma, including quercetin 3-O-rutinoside(QCR), kaempferol 3-O-rutinoside(KFR), isorhamnetin 3-O-rutinoside(ISR), bilobalide(BB), and ligustrazine(LGT). The plasma samples were pretreated by protein precipitation with acetonitrile. The chromatographic separation was achieved on a Waters Symmetry C18 analytical column(2.1 mm × 100 mm, 3.5 mm) with a mobile phase of 0.1% aqueous formic acid(A)-acetonitrile(B). Quantitation of the five bioactive constituents was achieved. Naringin was used as the internal standard(IS). All the calibration curves showed good linearity(r > 0.996) over the concentration range, with the lowest limit of quantification(LLOQ) between 2-18 ng·m L^(-1). The intraand inter-day accuracy and precision of the analytes were both within acceptable limits. Moreover, satisfactory extraction recoveries(90.92%-104.03%) were obtained by protein precipitation. The validated method was successfully applied to a pharmacokinetic study of XXI in rats after intravenous administration at three doses. The pharmacokinetic parameters of the five compounds varied in a dose-dependent manner within the tested dosage range. The present study was the first report of pharmacokinetic study for XXI.
