Determination of Esomeprazole in dog plasma by LC-MS-MS
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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, 5 μm);流动相为乙腈:2 mmol/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0.5~1 200 μg/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0.5 μg/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。Abstract: Objective To establish a method for determining Esomeprazole in dog plasma by LC-MS-MS. Methods Diazepam 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 (esomeprazole)and 285.2→193.2 m/z (diazepam). Results The calibration curve was linear over the range of 0.5~1 200 μg/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 concentration and suitable to the pharmacokinetics study.
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Key words:
- Esomeprazole /
- LC-MS-MS /
- plasma concentration
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[1] 杨 丽,严宝霞.埃索美拉唑的药动学[J].中国新药杂志,2003,13(5):398. [2] 戴歌心,张振南,王贤亲,等.HPLC-MS 联用测定人血浆中埃索美拉唑的浓度[J].中国卫生检验杂志,2011:21(8):1875. [3] 余 勤,梁茂植,赵 焱,等.反相高效液相色谱法测定血浆中埃索美拉唑浓度[J].华西医学,2006:21(1):93.
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