液质联用法测定盐酸氯丙嗪的浓度 - 第三军医大学学报.doc

液质联用同时测定盐酸氯丙嗪与氨基比林的研究 杨丹，王章阳，向荣风，杨波（第三军医大学西南医院药学部,重庆 400038） [摘要] 目的 建立同时测定细胞培养液中微量盐酸氯丙嗪与氨基比林的含量测定方法。nertsil ODS柱(5μm,2.1mm×100mm)、 柱温40℃甲醇2mmol/L乙酸铵溶液(4) =90:10 为流动相流速0.2 /min，质谱检测采用电喷雾离子源ESI)，正离子模式m/z86.2、氨基比林的分子离子m/z232.1及内标地西泮碎片离子m/z192.9。结果在优化的液相色谱与质谱检测条件下，各离子峰分离良好，可同时对盐酸氯丙嗪与氨基比林进行测定，其线性范围为0.005mg/L～0.32mg/L，回收率分别为87.5%～116.4%和92%～109.8%，所测药物的日内、日间精密度均小于8%。结论 所建立的高效液相色谱与双极质谱联用同时测定盐酸氯丙嗪Study on the Simultaneous Determination of Chlorpromazine Hydrochloride and Aminopyrine by HPLC MS/MS YANG Dan，W Zhang-yang,XIANG Rong-feng,YANG Bo（Department of Pharmacy , The Affiliated Southwest Hospital of Third Military Medical University, Chongqing 400038 , China） [Abstract] Objective To develop a method to simultaneously determine the low concentration of chlorpromazine hydrochloride(CPZ) and aminopyrine(AMP) in cell culture solution. Methods: The high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) method was adopted and evaluated . HPLC was carried out by using Inertsil ODS column(5μm, 2.1mm×100mm) as analytical column, methanol:2mmol/L aceticamind solution(pH 7.4) as mobil phase with velocity of flow 0.2ml/min, the column temperture was 40℃. The mass spectrometer was operated in the positive ion mode and the electrospray ionization (ESI) source as part of the tandem mass spectrometer system, simultaneous selective reaction monitoring (SRM) of multi-analytes were used for the quantitative determination of the analytes. The fragment ion m/z86.2 were selected to moniter CPZ, m/z192.9 to internal standard Diazepam ,but paren ion m/z232.1 to AMP. Results: Bouth calibration curves were linear in the range from 0.005mg/L to 0.32mg/L . The mean recovery was 87.5%～116.4%for CPZ ,92%～109.8% for AMP，and RSD of intra-day and inter-day were less than 8% for bouth. Conclusion: This method is sensitive, specific, simple, rapid and accurate, and is suitable for the determination of CPZ and AMP in cell culture solution. [Key words] chlorpromazine hydrochloride;