LC/MS/MS测定犬血浆中氯米帕明浓度及体内药动学(1)
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[摘要] 目的：建立液相色谱-串联质谱法测定犬血浆中氯米帕明(Clomipramine)。方法：色谱柱为Zorbax Extend-C18柱(150 mm×4.6 mm，5 μm，美国Agilent公司)；C18 保护柱(4.0 mm×3.0 mm，5 μm，迪马公司)；流动相为乙腈-10 mmol/L醋酸铵-甲酸(60∶40∶0.1，V/V/V)；流速为0.5 ml/min；进样量为20 μl；柱温为20℃；采用三重四极杆串联质谱仪，ESI电离源，以选择反应监测方式进行检测。用于定量分析的离子反应分别为m/z 315.2~86.1(氯米帕明)和m/z 285.1~86.2(内标异丙嗪)。500 μl血浆样品经正己烷液提取后蒸干，流动相复溶，进行分析。结果：测定血浆中氯米帕明的线性范围为1~500 ng/ml，定量下限为1 ng/ml；日内、日间精密度RSD均小于15%，准确度在85%~115%范围内，符合《中国药典》2010年版二部的规定。结论：本方法可用于氯米帕明的犬体内药代动力学研究。
[关键词] 氯米帕明；犬血浆；液相色谱-串联质谱
[中图分类号] R969.1 [文献标识码] A [文章编号] 1673-7210(2011)11(a)-033-03
Study on the concentration and pharmacokinetic of Clomipramine in dog plasma by LC/MS/MS
WANG Haojiang, BAI Kehua, WANG Ruili, ZHANG Shuqiu
College of Pharmacy, Shanxi Medical University, Shanxi Province, Taiyuan 030001, China
[Abstract] Objective: To establish an LC/MS/MS method for the determination of Clomipramine in dog plasma. Methods: The determination was carried on Zorbax Extend-C18 (150 mm×4.6 mm, 5 μm, Amercia agilent) with the mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate solution-formic acid (60∶40∶0.1, V/V/V). Column temperature was set at 20℃, flow rate of mobile phase was 0.5 ml/min, the sample amount was 20 μl. Mass spectrum condition was electrospray ionization (ESI) and SIM mod selected ion mass spectral m/z 315.2-86.1 (Clomipramine) and m/z 285.1-86.2 (internal standard Promethazine). The plasma samples with 500 μl which were extracted with N-hexane and reconstituted with mobile phase were analysed. Results: The calibration curve was established in the concentration range of 1-500 ng/ml. The lowest limit of quantification was 1 ng/ml. RSD of inter-day and intra-day precision were all less than 15%. The method recoveries were within 85%-115% and also met for requirement of Chinese Pharmacopoeia (2010) Vol Ⅱ. Conclusion: The method is successfully used for Clomipramine pharmacokinetic studies in dog.
[Key words] Clomipramine; Dog plasma; LC/MS/MS ......
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