QuEChERS-气相色谱-串联质谱法测定白附子中35种禁用农药的残留量  

Determination of Residues of 35 Prohibited Pesticides in Typhoni Rhizoma by Gas Chromatography-Tandem Mass Spectrometry with QuEChERS

作　　者：钱冲 马博凯 刘珊珊 黄雯雯 勾新磊 王尉[1] 高峡[1,2] 张梅 QIAN Chong;MA Bokai;LIU Shanshan;HUANG Wenwen;GOU Xinlei;WANG Wei;GAO Xia;ZHANG Mei(Beijing Key Laboratory of Organic Materials Testing Technology&Quality Evaluation,Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical&Chemical Analysis),Beijing 100094,China;Beijing Engineering Research Center of Food Safety Analysis,Beijing 100089,China)

机构地区：[1]北京市科学技术研究院分析测试研究所(北京市理化分析测试中心)有机材料检测技术与质量评价北京市重点实验室,北京100094 [2]北京市食品安全分析测试工程技术研究中心,北京100089

出　　处：《理化检验（化学分册）》2023年第8期896-902,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：北京市市级项目(11000022T000000455996);北京市改革与发展专项(2021ZL0122)。

摘　　要：在《中华人民共和国药典》(2020年版)四部通则2341新增第五法的基础上,提出了题示方法,并对前处理、色谱、质谱条件进行优化,解决了同分异构体农药在检测过程中易转化、分解的难题。用乙腈和QuEChERS萃取试剂盒提取样品中的35种禁用农药,用农残专用净化管去除杂质,所得样品提取液经氮吹浓缩和乙腈稀释后,加入磷酸三苯酯内标溶液,采用气相色谱-串联质谱法(GC-MS/MS)分析。用DB-17MS毛细管色谱柱在程序升温条件下分离样品溶液中各禁用农药,配有电子轰击离子(EI)源的三重四极杆质谱仪在多反应监测(MRM)模式下检测,基质匹配法联合内标法定量。结果表明:各禁用农药与内标的质量浓度比值均与对应的峰面积比值在一定范围内呈线性关系,相关系数均不小于0.999 8,检出限(3S/N)为0.16~5.00μg·kg^(-1);按标准加入法进行回收试验,回收率为61.1%~121%;仪器、方法以及中间精密度试验所得各农药测定值的相对标准偏差分别为1.2%~1.8%(n=6)、2.3%~5.5%(n=6)和2.5%~5.7%(n=12)。方法用于实际样品的分析,6批白附子样品中均未检出35种禁用农药。On the basis of the addition of the fifth method in the fourth part general rule 2341 of Pharmacopoeia of the People's Republic of China(2020 edition),the title method was proposed,and conditions of the pre-treatment,chromatography and mass spectrometry were optimized to solve the problems of easy conversion and decomposition of isomeric pesticides in the detection process.The 35 prohibited pesticides were extracted from the sample using acetonitrile and QuEChERS extraction kit.Impurities were removed using dedicated agricultural residue purification tube.The resulting sample extract was concentrated by nitrogen blowing and diluted with acetonitrile,and then mixed with triphenyl phosphate internal standard solution.The sample solution obtained was analyzed by GC-MS/MS.Prohibited pesticides in the sample solution were separated by DB-17MS capillary column under programmed temperature conditions,detected by triple quadrupole mass spectrometer equipped with EI source in MRM mode,and quantified by matrix matching method combined with internal standard method.It was shown that linear relationships between values of the mass concentration ratio and the peak area ratio of each prohibited pesticide to internal standard were kept in definite ranges,with correlation coefficients not less than 0.9998 and detection limits(3S/N)ranging from 0.16μg·kg^(-1) to 5.00μg·kg^(-1).Test for recovery was made by standard addition method,giving results in the range of 61.1%-121%.RSDs of the determined values for each pesticide obtained from tests of the instrument,method and intermediate precision were in the ranges of 1.2%-1.8%(n=6),2.3%-5.5%(n=6)and 2.5%-5.7%(n=12),respectively.The proposed method was applied to the analysis of actual samples,and the 35 prohibited pesticides were not detected in 6 batches of Typhonii Rhizoma samples.

关 键 词：QUECHERS 气相色谱-串联质谱法 禁用农药 残留量 白附子 

分 类 号：O657.63[理学—分析化学]