超快速液相色谱-质谱/质谱联用法测定氯丙嗪制剂中氯丙嗪含量

摘要

Objective To establish a simple and ultra-fast method for the quantification of chlorpromazine in chlorpromazine preparation by liquid chromatography/tandem mass spectrometric (UFLC-MS/MS) method. Methods Sample preparation consisted of extraction by adding ethanol, filtration with microporous membrane and centrifugation of the sample subsequently. LC-MS/MS detection was performed by using a triple-stage quadrupole mass spectrometer working in multiple reaction monitoring mode with positive electrospray ion-ization, using the transitions of m/z 319.0→85.8 of chlorpromazine. Chromatographic separation was achieved using a 3.0 mm × 75 mm, 2.0μm Shim-pack XR-ODS column with isocratic flow and elution with acetonitrile-water-formic acid ( 90∶10∶0.02, V/V/V ) and a flow-rate of 0.4 mL/min. The analyte was quanti-fied in a single run within 3 mins. Results Linearity was demonstrated over the expected concentration range 1~256 ng/mL. The lower limit of quantification was 1 ng/mL, respectively. Intra-day precision expressed as relative standar deviation was 1.34% or less, while inter-day result was 1.89% or less for chlorpromazine. Conclusion The method has good repeatability, high sensitivity and more convenient, and can be successfully applied for the determination of chlorpromazine in chlorpromazine preparation.%目的：建立简单超快速液相色谱—质谱/质谱联用法测定氯丙嗪制剂中氯丙嗪的含量。方法样品以乙醇提取、微孔滤膜滤过、离心后，通过电喷雾离子化（ESI），采用多反应检测方式进行正离子检测，用于定量分析的检测离子为质荷比319.0→85.8。采用Shim-pack XR-ODS （3.0 mm×75 mm,2.0μm）柱分离，以乙腈—水—甲酸（90∶10∶0.02， V/V/V ）为流动相，流速为0.40 mL/min，在3 min内完成氯丙嗪定量分析。结果线性范围为1~256 ng/mL，最低检测限为1 ng/mL；日内、日间测定的相对标准偏差分别小于1.34%、1.89%。结论本方法重复性好，灵敏度高，分析速度快，操作简单，可作为氯丙嗪制剂中氯丙嗪质量控制方法。