首页> 外文期刊>Biomedical Chromatography: An International Journal Devoted to Research in Chromatographic Methodologies and Their Applications in the Biosciences >Development of a sensitive LC-MS/MS method for simultaneous quantification of eleven constituents in rat serum and its application to a pharmacokinetic study of a Chinese medicine Shengmai injection
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Development of a sensitive LC-MS/MS method for simultaneous quantification of eleven constituents in rat serum and its application to a pharmacokinetic study of a Chinese medicine Shengmai injection

机译:同时测定大鼠血清中11种成分的灵敏LC-MS / MS方法的建立及其在中药生脉注射液药代动力学研究中的应用

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摘要

A sensitive LC-MS/MS method was developed and validated for simultaneous quantification of 11 constituents, ginsenoside Rg1, Re, Rf, Rg2, Rb1, Rd, Rc, ophiopogonin D, schisandrin, schisandrol B and schizandrin B, in rat serum using digoxin as the internal standard (IS). The serum samples were pretreated and extracted with a two-step liquid-liquid extraction. Chromatographic separation was achieved on a C-18 analytical column with a proper gradient elution using 0.02% acetic acid aqueous solution and 0.02% acetic acid-acetonitrile as mobile phase at a flow rate of 0.5 mL/min. MS detection was performed using multiple reaction monitoring via an electrospray ionization source. Good linearity was observed in the validated concentration range for every analyte (r(2) 0.9929), and the lower limits of quantitation of the analytes were in the range of 0.044-1.190 ng/mL in rat serum. Intra- and inter-day precisions were <14.2%. The accuracy expressed as recovery was within the range of 85.1-112.8%. The extraction recoveries were >75.8%.The validated method was successfully applied to a pharmacokinetic study of all analytes in rats after single intravenous administration of Shengmai injection. Copyright (c) 2014 John Wiley & Sons, Ltd.
机译:开发了一种灵敏的LC-MS / MS方法,并通过地高辛对大鼠血清中人参皂苷Rg1,Re,Rf,Rg2,Rb1,Rd,Rc,ophiopogonin D,五味子素,五味子酚B和五味子素B的11种成分进行了同时定量,并进行了验证作为内部标准(IS)。血清样品经过预处理,并采用两步液液萃取法进行萃取。在C-18分析柱上进行色谱分离,使用0.02%的乙酸水溶液和0.02%的乙酸-乙腈作为流动相,以0.5 mL / min的流速进行适当的梯度洗脱。 MS检测是通过电喷雾电离源使用多反应监测进行的。在每个分析物的验证浓度范围内均观察到良好的线性(r(2)为0.9929),在大鼠血清中分析物的定量下限为0.044-1.190 ng / mL。日内和日间精度为<14.2%。以回收率表示的准确度在85.1-112.8%的范围内。提取回收率> 75.8%。该验证方法成功地应用于生脉注射液单次静脉内给药后大鼠中所有分析物的药代动力学研究。版权所有(c)2014 John Wiley&Sons,Ltd.

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