QuEChERS-气相色谱串联质谱法同时测定番茄中46种农药残留

Simultaneous Determination of 46 Pesticide Residues in Tomatoes by QuEChERS Method Combined with Gas Chromatography-Mass Spectrometry

建立一种QuEChERS结合气相色谱-串联质谱同时检测番茄中46种杀菌剂和杀虫剂残留的分析方法。样品用乙腈提取,经PSA、C18、无水MgSO4净化,HP-5MS色谱柱分离,采用多反映监测(MRM)模式检测,基质匹配外标法定量。结果表明,46种农药在0.005~0.500μg/mL的浓度范围内线性关系良好(R^(2)>0.999),方法检出限和定量限分别在0.07~2.63μg/kg和0.21~8.39μg/kg之间;在0.0025、0.025、0.25 mg/kg的加标水平下,46种农药化合物平均加标回收率在70.40%~115.08%范围内,相对标准偏差为0.22%~4.89%。50批次番茄样品中9批次检出毒死蜱和嘧菌酯残留,含量范围在0.0043~0.0365 mg/kg,均未超出GB 2763-2021标准规定的限量值。本方法快速、简单、灵敏、准确,能够满足番茄中多农药残留的检测。

An analysis method for simultaneous determination of 46 kinds of fungicides and insecticides residues in tomatoes by QuEChERS method combined with gas chromatography-mass spectrometry was established.The samples were extracted with acetonitrile,then purified up with PSA,C18 and anhydrous MgSO4,separated by a HP-5MS chromatographic column,analyzed using multiple reflection monitoring(MRM)mode,and quantified by matrix-matched external standard method.The result showed that,the 46 kinds of pesticides showed good linearity when they were in 0.005~0.500μg/mL(R^(2)>0.999).The limits of detection of the 46 kinds of pesticides were in 0.07~2.63μg/kg,and the limits of quantitation were in 0.21~8.39μg/kg.The average recoveries were 70.40%~115.08%with the relative standard deviations of 0.22%~4.89%at the spiked levels of 0.0025,0.025 and 0.25 mg/kg.Residues of chlorpyrifos and azoxystrobin were detected in 9 of the 50 batches of tomato samples,with the content ranging from 0.0043~0.0365 mg/kg,which did not exceed the limit value specified in GB 2763-2021.The method was rapid,simple,sensitive and accurate,which could meet the detection of multiple pesticide residues in tomato.