LC-MS/MS测定大鼠血浆中虎杖苷浓度
投稿时间:2011-02-10  修订日期:2011-12-21  点此下载全文
引用本文:丁雪鹰,侯晓丽,孙铭学,肖凯.LC-MS/MS测定大鼠血浆中虎杖苷浓度[J].药学实践杂志,2012,30(1):45~48
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作者单位E-mail
丁雪鹰 第二军医大学药学院药剂学教研室,上海 200433  
侯晓丽 第二军医大学海医系毒物药物研究室,上海 200433  
孙铭学 第二军医大学海医系毒物药物研究室,上海 200433  
肖凯 第二军医大学海医系毒物药物研究室,上海 200433 kaixiaocn@gmail.com 
基金项目:上海市科委中药现代化项目(08DZ1971504);国家自然科学基金(20872179,30472141).
中文摘要: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1.0
中文关键词:虎杖苷  LC-MS/MS  血药浓度
 
Determination of polydatin in rats plasma by LC-MS/MS
Abstract: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.
keywords:polydatin  LC-MS/MS  plasma drug concentration
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