Melton Laura M, Taylor Michael J
Chemistry Branch, SASA, Roddinglaw Road, Edinburgh EH12 9FJ, United Kingdom.
MethodsX. 2020 Dec 10;8:101180. doi: 10.1016/j.mex.2020.101180. eCollection 2021.
The quantitative determination of multiple pesticide residues in food is an iterative process given the frequent changes in monitoring specifications set by regulatory authorities, introduction of new pesticide active ingredients, variety of commodities encountered and advances in the capability of analytical instrumentation and software platforms. The method described here:•replaces our previous methodology [1] that was based on an ethyl acetate extraction [2], two different sample extract clean-up regimes depending on the commodity; either Gel Permeation Chromatography (GPC) or Solid Phase Extraction (SPE) and GC/MSMS analysis using cool on-column injection and permits higher throughput using the same QuEChERS extraction method used for LCMS/MS analysis [3]•uses PTV injection incorporating a deactivated (baffled) injection liner required to improve performance for 'difficult to analyse' pesticides e.g. captan, dichlofluanid, folpet, tolylfluanid.•has been validated for the quantitative determination of 113 different pesticides and their metabolites in a range of fruit and vegetables of high water content and high acid and high water content i.e. cabbage, lemon, pepper, plum and spinach and complies with requirements of European Commission guidance document on Analytical Quality Control and Method Validation Procedures for Pesticides Residues Analysis in food and feed - SANTE/12682/2019 [4].
鉴于监管机构设定的监测规范不断变化、新农药活性成分的引入、所遇到商品的多样性以及分析仪器和软件平台能力的进步,食品中多种农药残留的定量测定是一个迭代过程。此处所述方法:
•取代了我们之前基于乙酸乙酯萃取[2]的方法[1],根据商品不同采用两种不同的样品提取物净化方案;即凝胶渗透色谱法(GPC)或固相萃取法(SPE),以及使用冷柱上进样的气相色谱/串联质谱分析,并采用与用于液相色谱-质谱/质谱分析[3]相同的QuEChERS萃取方法实现更高的通量
•采用程序升温汽化进样(PTV),并配有去活(带折流板)进样衬管,以提高对“难分析”农药(如克菌丹、抑菌灵、福美双、甲苯氟磺胺)的分析性能。
•已针对一系列高水分含量、高酸和高水分含量的水果和蔬菜(即卷心菜、柠檬、辣椒、李子和菠菜)中113种不同农药及其代谢物的定量测定进行了验证,并且符合欧盟委员会关于食品和饲料中农药残留分析的分析质量控制和方法验证程序的指导文件-SANTE/12682/2019[4]的要求。