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建立了蔬菜干制品中18种有机磷农药和拟除虫菊酯农药残留的在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析方法。样品以乙腈为提取剂超声波高速匀浆提取,提取液经ENVI-Carb固相萃取柱净化,除去样品中大部分的色素等干扰基质,再经在线GPC进一步净化除去大分子干扰物质,有效降低了样品基质带来的背景干扰。采用外标法定量,在质量浓度为0.02 mg/kg~0.5mg/kg有良好的线性关系,加标水平为0.4 mg/kg时,18种农药的回收率基本都在80%~130%,相对标准偏差小于10%,检出限为0.001mg/kg~0.026 mg/kg。经实验证明,该方法是一种快速,准确,灵敏度高的同时检测梅菜干中多种农药残留的检测方法。
An online gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC / MS) method was developed for the determination of 18 organophosphorus pesticides and pyrethroid pesticide residues in vegetable dried products. The sample was extracted by high speed ultrasonic homogenization with acetonitrile as extractant. The extract was purified by ENVI-Carb solid phase extraction (SPE) column to remove most of the pigment and other interfering substrates in the sample, and then further purified by on-line GPC to remove macromolecular interfering substances, effectively reducing Background interference from the sample matrix. The external standard method was used for quantification. The calibration curves were linear in the range of 0.02 mg / kg to 0.5 mg / kg. The spiked recoveries of 18 pesticides ranged from 80% to 130% at the spiking level of 0.4 mg / kg. The relative standard deviation was less than 10%, and the limit of detection was 0.001 mg / kg ~ 0.026 mg / kg. The experimental results show that this method is a rapid, accurate and sensitive method for the simultaneous detection of various pesticide residues in dried plum.