QuEChERS-UPLC-MS/MS法快速测定苹果中304种农药残留

Rapid Determination of 304 Pesticides Residues in Apple by QuEChERS-UPLC-MS/MS

建立了QuEChERS-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)快速筛查和确证苹果中304种农药残留的分析方法。苹果样品经粉碎后用乙腈提取, QuEChERS试剂净化, UPLC-MS/MS测定,基质匹配标准曲线定量。304种农药在10~500 ng/mL范围线性关系良好,相关系数均大于0.995。304种化合物在3个添加水平(10,40和80μg/kg)的平均回收率为73.7%~115.9%,相对标准偏差(SRSD)均小于17.9%(n=6),定量限为10μg/kg。将该方法应用于中国检验检疫科学院(CAIQ)组织的2020年高通量非靶向农药筛查能力验证,定性和定量结果均满足能力验证的要求。该方法前处理简单、定性准确、定量可靠,可为水果和蔬菜中多农药残留的快速检测提供参考。

A method for simultaneous rapid screening and accurate confirmation of 304 pesticide residues in apple was established by QuEChERS-ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(QuEChERS-UPLC-MS/MS). The prepared samples were extracted with acetonitrile, then purified with QuEChERS package,and determined by UPLC-MS/MS with matrix-matched standard calibration for quantitation. The results demonstrated that the compounds showed good linearity in the range of 10-500 ng/mL, and the linear correlation coefficients(R) of the 304pesticides in apple were greater than 0.995. At the addition levels of 10, 40 and 80 μg/kg, the recoveries were in the ranges of 73.7%-115.9%, with the relative standard deviations(SRSD) less than 17.9%(n=6), respectively. In addition, the limits of quantification(SLOQ) of 304 pesticides were no more than 10 μg/kg. The method was applied to detect pesticide residues in the apple sample provided by the 2020 Chinese Academy of Inspection and Quarantine(CAIQ) test project for unknown pesticide screening and accurate quantitation. The results demonstrated that the method was accurately and reliable. This analytical method was simple, accurate and reliable, which could be used for rapid detection of multi pesticide residues in fruits and vegetables.