UPLC-MS/MS法测定3种兽药制剂中违禁药物氯丙嗪

Determination of Chlorpromazine Illegally Added in 3 Kinds of Veterinary Preparations by UPLC-MS/MS

关键词:  兽药制剂  氯丙嗪  违禁药物  超高效液相色谱-串联质谱

Key words:  veterinary preparations  chlorpromazine  illicit drug  ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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（UPLC-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, 1.7 μm)，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。

Abstract:

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.