UP LC－MS／MS法测定3种兽药制剂中违禁药物氯丙嗪

摘要

建立了3种兽药制剂中违禁药物氯丙嗪的超高效液相色谱－串联质谱（ UP LC－MS／MS ）检测方法。用无水乙醇超声提取试样中违禁药物氯丙嗪，采用Waters ACQUITY UPLC BEH C18柱（50 mm×2．1 mm，1．7μm），乙腈和10 mmol／L乙酸铵＋0．1％甲酸溶液流动相，梯度洗脱，电离喷雾电离方式（ESI＋），多反应监测（MRM）定量。该方法线性关系良好，相关系数r2达到0．9956，回收率在88．3％～96．7％之间，相对标准偏差（ RSD）介于3．7％～8．1％。方法的检出限为0．003 mg／kg。本方法适用于兽药制剂中氯丙嗪违法添加的定性、定量分析。%A method of determination of chlorpromazine illegally added in 3 kinds of veterinary preparations by ultra-performance liquid chromatography -tandem mass spectrometry ( UPLC -MS/MS ) was developed. Chlorpromazine was extracted with ethanol by ultrasonic wave and separated on the Waters ACQUITY UPLC BEH C18 column (50 mm×2.1 mm, 1.7μm) using the mobile phase of acetonitrile/mixture of 10 mmol/L ammonium acetate and 0.1%formic acid with gradient elution. Chlorpromazine was detected in electrospray ionization ( ESI+) mode using multiple reaction monitoring ( MRM ) . There was a good linear relationship with the correlation rate more than 0. 9956. The average recoveries ranged from 88. 3% to 96. 7%. The standard deviation was between 3.7% and 8.1%. The limit of detection was 0.003 mg/kg. The method was rapid, simple, sensitive and accurate. It was suitable for qualitative and quantitative analysis of the illicit drug chlorpromazine in veterinary preparations.