犬血浆中氨氯地平和阿托伐他汀的LC-MS/MS测定

Determination of Amlodipine and Atorvastatin in Dog's Plasma by LC-MS/MS

建立了LC-MS/MS法同时测定犬血浆中氨氯地平和阿托伐他汀的含量。用甲醇沉淀血样中的蛋白质,采用C18色谱柱,2mmol/L醋酸胺溶液(含0.5%甲酸)-甲醇(32∶68)为流动相,以地西泮为内标,电喷雾离子化,正离子多反应监测,检测离子分别为m/z409.2→m/z238.1(氨氯地平)、m/z559.2→m/z440.5(阿托伐他汀)和m/z285.1→m/z193.1(地西泮)。结果氨氯地平和阿托伐他汀在0.1～20ng/ml和0.2～50ng/ml浓度范围内线性关系良好,定量限为0.1和0.2ng/ml,方法回收率均大于94%,日内、日间RSD均小于9%。

A LC-MS/MS method was established for the determination of amlodipine and atorvastatin in Beagle dog＇s plasma. The samples were precipitated with methanol. A C18 column was used with the mobile phase of 2 mmol/L ammonium acetate （containing 0.5%formic acid）-methanol （32 ： 68）. Diazepam was used as the internal standard. ESI was applied and operated in positive ion multiple-reaction monitoring mode. The detected ions were m/z 409.2→ m/z 238.1 （amlodipine）, m/z 559.2→ m/z 440.5 （atorvastatin）, and m/z 285.1→m/z 193.1 （diazepam）. The calibration curves of amlodipine and atorvastatin were linear in the concentration ranges of 0.1 -20 ng/ml and 0.2- 50 ng/ml, and the limit of quantification was 0.1 ng/ml （amlodipine） and 0.2 ng/ml （atorvastatin）. The average recoveries were above 94 %. The RSDs of intra- and inter-day were less than 9 %.