QuEChERS-液相色谱-串联质谱法测定蔬菜中的56种农药残留  

Determination of the 56 Pesticide Residues in Vegetables by QuEChERS-ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李欣[1] 孙素群[1] 张卫锋 陈威[3] 

机构地区：[1]广东科贸职业学院生物技术系,广东广州510430 [2]广州市农产品质量安全监督所,广东广州510308 [3]广东省粮食科学研究所,广东广州510050

出　　处：《现代食品科技》2017年第10期245-253,177,共10页Modern Food Science and Technology

基　　金：2013年广东省科技计划项目(2013B020311005);2015年广东省优秀青年教师培养项目(YQ2015188)

摘　　要：为解决蔬菜中农药多残留检测存在的基质复杂、干扰大和浓度低等技术困难,本研究建立了一种新的蔬菜中56种农药多残留的液相色谱-串联质谱的分析方法。蔬菜样品经改良QuEChERS方法前处理,即用含1%(V/V)乙酸的乙腈溶液提取,并加入氯化钠和无水乙酸钠盐析,以N-丙基乙二胺净化,直接进样分析。以乙腈和水溶液(含5 m M的乙酸铵和0.1%(V/V)甲酸)为流动相,经C18色谱柱(4.6×100 mm、2.6μm)分离,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测。结果表明,56种农药在2μg/L^100μg/L有良好线性,其相关系数大于0.99,检出限均低于0.01 mg/kg,在3个添加水平下的回收率为65.8%~114.0%,相对标准偏差为0.1%~14.5%。该方法简单、快速、可靠,可用于蔬菜质量安全风险评估中多种类农药残留的快速筛查分析。A new method for analysis of 56 pesticide residues in vegetables using modified QuEChERS-performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was established to solve the technical difficulties of complex components, interference and low concentration. Vegetable samples were pretreated bymodified QuEChERS, which was extracted with acetonitrile containing 1%（V/V） acetic acid, and then salted out with sodium chloride and anhydrous sodium. purified with primary secondary amine, samples was analyzed by HPLC-MS/MS. The extract was separated on a C18 column（4.6×100 mm, 2.6 μm） using acetonitrile and aqueous solution as the mobile phase（containing 5 m M ammonium acetate and 1%（V/V） acetic acid）, ionized in electrospray ion（ESI＋） mode and then analyzed in multiple-reaction monitoring（MRM） mode. The results showed that the 56 pesticide residues showed good linear correlation in the range of 2.0 μg/L to 100 μg/L with the correlation coefficients over 0.99. The limits of detection were less than 0.01 mg/kg, and the recoveries were ranged of 65.8%~114.0% at three spiked levels in vegetables with the relative standard deviations of0.1%~14.5%. This proposed method is rapid, simple, low-cost and effective, which can be applied to rapid screening and analysis of pesticide residues in vegetables for the risk assessments of quality and safety.

关 键 词：QUECHERS 农药多残留 高效液相色谱-串联质谱法 多反应监测 

分 类 号：O657.63[理学—分析化学]