Wang Xianqin, Zhu Jiayin, Xu Renai, Yang Xuezhi, Wu Haiya, Lin Dan, Ye Faqing, Hu Lufeng
Analytical and Testing Center, Wenzhou Medical College, Wenzhou 325035, China.
Biomed Chromatogr. 2010 Oct;24(10):1108-12. doi: 10.1002/bmc.1412.
A sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of piracetam in rat plasma was developed and validated over the concentration range of 0.1-20 µg/mL. After addition of oxiracetam as internal standard, a simplified protein precipitation with trichloroacetic acid (5%) was employed for the sample preparation. Chromatographic separation was performed by a Zorbax SB-Aq column (150 × 2.1 mm, 3.5 µm). The mobile phase was acetonitrile-1% formic acid in water (10:90 v/v) delivered at a flow rate of 0.3 mL/min. The MS data acquisition was accomplished in multiple reaction monitoring mode with a positive electrospray ionization interface. The lower limit of quantification was 0.1 µg/mL. For inter-day and intra-day tests, the precision (RSD) for the entire validation was less than 9%, and the accuracy was within the 94.6-103.2% range. The developed method was successfully applied to pharmacokinetic studies of piracetam in rats following single oral administration dose of 50 mg/kg.
建立了一种灵敏且选择性好的液相色谱-串联质谱法,用于测定大鼠血浆中吡拉西坦的含量,该方法在0.1 - 20μg/mL的浓度范围内经过了验证。加入奥拉西坦作为内标后,采用简化的5%三氯乙酸蛋白沉淀法进行样品制备。色谱分离采用Zorbax SB-Aq柱(150×2.1mm,3.5μm)。流动相为乙腈-1%甲酸水溶液(10:90 v/v),流速为0.3 mL/min。质谱数据采集采用正电喷雾电离接口的多反应监测模式。定量下限为0.1μg/mL。在日间和日内测试中,整个验证过程的精密度(RSD)小于9%,准确度在94.6 - 103.2%范围内。所建立的方法成功应用于大鼠单次口服50mg/kg剂量吡拉西坦后的药代动力学研究。