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

中文关键词:  超高效液相色谱串联质谱  水产品  乙酰甲喹  代谢物

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  aquatic products  mequindox  metabolites

中文摘要:

      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-5 mmol/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 0.03 μg/kg和0.1 μg/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、1.0 μg/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。

英文摘要:

      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 150 ng/mL, with correlation coefficients of 0.99910.9996, the limit of detection was 0.03 μg/kg, and the limit of quantitation was 0.1 μg/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 1.0 μg/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.