Determination of polydatin in rats plasma by LC-MS/MS
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摘要: 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1.0Abstract: 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.
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Key words:
- polydatin /
- LC-MS/MS /
- plasma drug concentration
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