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目的建立LC-MS/MS同时测定大鼠血浆中氯维地平和其主要代谢产物H152/81的浓度。方法大鼠血浆样品用液液萃取后,以尼莫地平为内标,选用ZORBAX SB C18(2.1 mm×100 mm,3.5μm)色谱柱,以乙腈-0.1%甲酸为流动相梯度洗脱,梯度流速恒定为0.3 m L·min-1,柱温为30℃,进样量10μL,总分析时间为3.5 min,采用电喷雾离子化源,正离子方式,多反应监测(MRM)扫描方式进行监测。结果血浆中氯维地平和代谢产物H152/81的线性范围为1.0~200μg·L-1(r>0.99),定量下限为1.0μg·L-1;平均回收率95.2%~109.8%;日内、日间RSD均小于15%;提取回收率在71.3%~82.6%。结论该方法快速、灵敏、准确,专属性强,重复性好,适用于大鼠血浆中同时测定氯维地平及其代谢产物浓度。
Objective To establish a LC-MS / MS method for the simultaneous determination of clevidipine and its major metabolite H152 / 81 in rat plasma. Methods The plasma samples of rats were extracted with liquid and liquid, then nimodipine was used as the internal standard. The chromatographic column of ZORBAX SB C18 (2.1 mm × 100 mm, 3.5 μm) was used and the mobile phase of acetonitrile-0.1% formic acid was eluted. The gradient The flow rate was constant at 0.3 m L · min-1, the column temperature was 30 ℃, the injection volume was 10 μL and the total analysis time was 3.5 min. Electrospray ionization, positive ion and MRM scanning were used to monitor . Results The linear range of clevidipine and metabolite H152 / 81 was 1.0 ~ 200μg · L-1 (r> 0.99) and the lower limit of quantitation was 1.0μg · L-1. The average recovery was 95.2% -109.8% Daytime RSDs were less than 15%; extraction recovery was 71.3% ~ 82.6%. Conclusion The method is rapid, sensitive, accurate, specific and reproducible. It is suitable for simultaneous determination of clevidipine and its metabolites in rat plasma.