利用QuEChERS(quick, easy, cheap, effective, rugged, safe)结合超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)建立同时检测禽蛋及其制品中42种农药及其代谢物残留的检测方法。以体积分数1%的乙酸乙腈为提取溶剂,加入NaCl除水后,经多功能针式过滤器至进样小瓶中,以体积分数为0.1%甲酸水溶液和5 mmol/L甲酸铵甲醇溶液作为流动相,采用UPLC-MS/MS方法检测。结果表明,各农药及代谢物在0.5~100 μg/L范围内线性关系良好,相关系数大于0.990 0,检出限为0.01~0.5 μg/kg,样品加标回收率为74.13%～113.22%,相对标准偏差(relative standard deviation, RSD)为0.98%～14.29%(n=6)。建立的QuEChERS-UPLC-MS/MS方法可同时检测42种目标物,回收率好、精密度高、检出限低、且分析时间短,能够满足禽蛋及其制品中多种农药及其代谢物的同时检测。
A method was established for the determination of 42 pesticides and their metabolites in eggs and products on the basis of QuEChERS (quick, easy, cheap, effective, rugged, safe) combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by acetonitrile (containing 1% acetic acid), dewatered by sodium chloride, and then uniformly passed through a multi-functional needle filter into the sampling vial. 0.1% formic acid aqueous solution and 5 mmol/L ammonium formatting methanol solution were used as the mobile phase solution, and UPLC-MS/MS was used as a detection method. 42 pesticides and their metabolites showed good linear in the range of 0.5-100 μg/L, respectively, with the correlation coefficients above 0.990 0. The limits of detection (LOD) were 0.01~0.5 μg/kg, the recoveries of spiked samples were between 74.13%-113.22% and the relative standard deviations (RSD) were between 0.98%-14.29% (n=6). The QuEChERS-UPLC-MS/MS can detect 42 kinds of targets simultaneously with good reproducibility, high accuracy, low detection limit and short analysis time. The method could be widely used for simultaneous detection of pesticide residues in poultry eggs and products.
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