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  

Ultra faster method for the quantification of chlorpromazine in chlorpromazine preparation using UFLC-MS/MS

作　　者：徐丽婷 张娟红[1,2] 孙爱军[1] 王荣[1,2] 谢华[1] 张汝学[1] 张强[1] 黄小玉[1] 贾正平[1,2] 

机构地区：[1]兰州军区兰州总医院药剂科,甘肃兰州730050 [2]兰州军区兰州总医院全军高原环境损伤防治重点实验室,甘肃兰州730050

出　　处：《兰州大学学报（医学版）》2015年第2期46-49,54,共5页Journal of Lanzhou University（Medical Sciences）

基　　金：科技部重大专项(2008ZXJ09004-52);甘肃省科技重大专项(1102FKDA012)

摘　　要：目的建立简单超快速液相色谱一质谱／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（3．0mm×75mm，2．0μn）柱分离，以乙腈-水-甲酸（90：10：0．02，V／V／V）为流动相，流速为O．40mL／min，在3min内完成氯丙嗪定量分析。结果线性范围为1-256ng／mL，最低检测限为1ng／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。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 ionization, using the transitions of m/z 319.0→85.8 of chlorpromazine. Chromatographic separation was achieved using a 3.0 mm×75 mm, 2.0 μm 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 quantified in a single run within 3 mins. Results Linearity was demonstrated over the expected concentratinn 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.

关 键 词：氯丙嗪 制剂 超快速液相色谱-质谱/质谱联用法 

分 类 号：R971[医药卫生—药品]