LC-MS/MS测定大鼠血浆中虎杖苷浓度

目的 建立测定大鼠血浆中虎杖苷浓度的LC-MS/MS方法。 方法 采用LC-MS/MS测定大鼠血浆中虎杖苷的浓度,以二苯乙烯苷为内标,血浆样品用乙腈沉淀蛋白,色谱柱为Agilent Zorbax SB-C₁₈ (100 mm×2.1 mm, 3.5 μm),流动相为甲醇-乙腈-0.1%甲酸水溶液(18∶15∶67),流速0.3 ml/min,柱温30 ℃。 结果 虎杖苷的线性范围为1.0~5 000.0 ng/ml (r=0.998 4),最低定量检测浓度为1.0

Determination of polydatin in rats plasma by LC-MS/MS

Objective To establish a LC-MS/MS method for determination of polydatin concentration in rats plasma.Methods The plasma concentration of polydatin was determined by LC-MS/MS.Using stilbene glucoside as internal standard,after precipitation of the plasma proteins with methanol,the analytes were separated on an agilent zorbax SB-C18 reversed-phase column with methanol-acetonitrile-0.1% formic acid(18:15:67,v/v) and detected by electrospray ionization(ESI) mass spectrometry in negative multiple reaction monitoring(MRM) mode.The flow rate was 0.3 ml/min.Column temperature was maintained at 30 ℃.Results The calibration curves with good linearity(r=0.998 4 for plasma sample) were obtained in the range of 1.0～5000.0 ng/ml for polydatin.The lower limit of quantification(LLOQ) was 1.0 ng/ml.Recoveries were around 78% for the extraction from rats plasma,and good precision and accuracy were achieved.The intra-day and inter-day RSD were both less than 15.0%.This method was feasible for the evaluation of pharmacokinetic profiles of polydatin in rats.Conclusion This method was simple,selective and sensitive.It′s suitable for the pharmacokinetic research of polydatin in rats plasma.