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首页> 外文期刊>Journal of mass spectrometry: JMS >Lithium adduct as precursor ion for sensitive and rapid quantification of 20 (S)-protopanaxadiol in rat plasma by liquid chromatography/quadrupole linear ion trap mass spectrometry and application to rat pharmacokinetic study
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Lithium adduct as precursor ion for sensitive and rapid quantification of 20 (S)-protopanaxadiol in rat plasma by liquid chromatography/quadrupole linear ion trap mass spectrometry and application to rat pharmacokinetic study

机译：锂加合物作为前体离子，用于液相色谱/四极杆线性离子阱质谱法快速，灵敏地定量大鼠血浆中的20（S）-原萘并二醇，并用于大鼠药动学研究

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摘要

A novel, rapid and sensitive liquid chromatography/quadrupole linear ion trap mass spectrometry [LC-ESI-(QqLIT)MS/MS] method was developed and validated for the quantification of protopanaxadiol (PPD) in rat plasma. Oleanolic acid (OA) was used as internal standard (IS). A simple protein precipitation based on acetonitrile (ACN) was employed. Chromatographic separation was performed on a Sepax GP-C18 column (50 × 2.1 mm, 5 μM) with a mobile phase consisting of ACN-water and 1.5 μM formic acid and 25 mM lithium acetate (90: 10, v/v) at a flow rate of 0.4 ml/min for 3.0 min. Multiple-reaction-monitoring mode was performed using lithium adduct ion as precursor ion of m/z 467.5/449.4 and 455.6/407.4 for the drug and IS, respectively. Calibration curve was recovered over a concentration range of 0.5-100 ng/ml with a correlation coefficient >0.99. The limit of detection was 0.2 ng/ml in rat plasma for PPD. The results of the intraday and interday precision and accuracy studies were well within the acceptable limits. The validated method was successfully applied to investigate the pharmacokinetic study of PPD after intravenous and gavage administration to rat.
机译：建立了一种新颖，快速，灵敏的液相色谱/四极杆线性离子阱质谱[LC-ESI-（QqLIT）MS / MS]方法，并验证了大鼠血浆中原萘二酚（PPD）的定量方法。齐墩果酸（OA）用作内标（IS）。采用基于乙腈（ACN）的简单蛋白质沉淀法。色谱分离是在Sepax GP-C18色谱柱（50×2.1 mm，5μM）上进行的，流动相由ACN-水和1.5μM甲酸和25 mM乙酸锂（90：10，v / v）组成。流速为0.4 ml / min，持续3.0 min。使用锂加合物离子作为前体离子对药物和IS分别执行m / z 467.5 / 449.4和455.6 / 407.4的多重反应监测模式。在0.5-100 ng / ml的浓度范围内恢复校准曲线，相关系数> 0.99。在PPD大鼠血浆中的检出限为0.2 ng / ml。日内和日间精度和准确性研究的结果均在可接受的范围内。经验证的方法已成功用于研究大鼠静脉内和强饲法对PPD的药代动力学研究。

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