超高效液相串联质谱法测定水产品中乙酰甲喹及其代谢物

Determination of mequindox and its metabolites in aquatic products by ultra liquid chromatography tandem mass spectrometry

目的建立一种超高效液相串联质谱法(ultra liquid chromatography tandem mass spectrometry,ULPC-MS/MS)测定水产品中乙酰甲喹及其代谢物的方法。方法组织样品经二氯甲烷/乙酸乙酯提取,正己烷去除脂肪过滤处理后,采用Waters ACQUITY HSS T3色谱柱进行分离,乙腈-5mmol/L乙酸铵水溶液+0.1%甲酸水(V:V)溶液作为流动相进行梯度洗脱,正离子扫描方式下多反应监测模式测定。结果乙酰甲喹及其5种代谢物在1~50 ng/mL线性范围内线性良好,相关系数为0.9991~0.9996;该方法的检出限和定量限分别为0.03μg/kg和0.1μg/kg;鳗鲡、青蛾、虾、蟹肌肉样品中,乙酰甲喹及代谢物在0.1、0.2、1.0μg/kg的加标水平的平均回收率为66.6%~106.6%,日内精密度范围为2.1%~11.1%,日间精密度范围为1.3%~13.2%。结论本方法稳定、准确、灵敏、快速,能够满足水产品中乙酰甲喹及其代谢物残留分析的需求。

Objective To establish a method for determination of mequindox and its metabolites in aquatic products by ultra liquid chromatography tandem mass spectrometry(ULPC-MS/MS).Methods The tissue samples were extracted with dichloromethane/ethyl acetate and filtered with n-hexane to remove fat,separated with Waters ACQUITY HSS T3 column by gradient elution using acetonitrile-5 mmol/L ammonium acetate solution+0.1%formic acid solution(V:V)as mobile phase,the contents were determined by multi-reaction monitoring mode under positive ion scanning mode.Results Mequindox and its 5 metabolites had good linearity in the linear range of 1-50 ng/mL,with correlation coefficients of 0.9991-0.9996,the limit of detection was 0.03μg/kg,and the limit of quantitation was 0.1μg/kg.In eel,moth,shrimp and crab muscle samples,the average recoveries of mequindox and its metabolites at the spiked levels of 0.1,0.2,and 1.0μg/kg were 66.6%-106.6%,and the daily precision range was 2.1%-11.1%,the daytime precision range was 1.3%-13.2%.Conclusion The method is stable,accurate,sensitive and fast,and can meet the needs of analysis of mequindox and its metabolites in aquatic products.