摘要
目的建立液相色谱联用质谱法(LC-MS-MS)测定犬体内血浆中埃索美拉唑(esomeprazole,EMZ)药物浓度。方法以地西泮为内标,血浆采用蛋白沉淀处理,色谱柱为Shim-pack XR-ODS柱(2 mm×100 mm,5μm);流动相为乙腈:2mmol/L乙酸铵(含0.1%甲酸);流速0.3 ml/min;质谱条件:电喷雾离子化电离源ESI,正离子多反应检测,检测离子分别为346.2→198.2 m/z(埃索美拉唑)和285.2→193.2 m/z(地西泮)。结果埃索美拉唑在0.5~1 200μg/L检测浓度范围内呈良好线性关系(r>0.99),最低定量限(LLOQ)为0.5μg/L,平均绝对回收率在(101.0±6.5)%,低、中、高3种浓度的日内、日间RSD≤15%。结论该方法操作简便、灵敏、准确,适用于埃索美拉唑血药浓度测定及药动学研究。
Objective To establish a method for determining Esomeprazole in dog plasma by LC-MS-MS. Methods Diaze- pam was used as the internal standard ,the samples were precipitated with acetonitril. Analytical column was Shim-pack XR-ODS (2 mm × 100 mm, 5 μm). The mobile phase was acetonitrile:2 mmol/L ammonium acetate( containing 0.1% formic acid) at a flow rate of 0.3 ml/min. Mass spectrum conditions was ESI performing in positive ion MRM mode using target ions 346.2-198.2 m/z( esome- prazole) and 285.2-193.2 m/z(diazepam). Results The calibration curve was linear over the range of 0.5 - 1 200μg/L . The LLOQ of Esomeprazole in plasma was 0.5 μg/L . The average extracted recovery was( 101.0 ± 6.5) %. The RSDs of intra- and inter- day were less than 15%. Conclusion The method was sensitive, simple and accurate to determinate Esomeprazole plasma concentra- tion and suitable to the pharmacokinetics study.
出处
《药学实践杂志》
CAS
2013年第1期61-63,共3页
Journal of Pharmaceutical Practice