固相萃取-气相色谱串联质谱法检测牛奶中41种农药残留张月辉（辽宁省检验检测认证中心，辽宁沈阳110032）摘要：目的建立固相萃取-气相色谱串联质谱法（SPE-GC-MS/MS）同时测定牛奶中41种农药残留分析方法。方法采用固相萃取方法对样品进行前处理。样品经乙腈提取、盐析后，提取液经CaptivaEMR-Lipid固相萃取柱净化后上机测定。用气相色谱-三重四极杆串联质谱仪进行多农残检测。结果41种农药在50~1000ng/ml之间呈良好的线性关系，相关系数r均大于0.99。在0.02，0.1，0.2mg/kg加标水平下，41种农药的平均回收率为60.6%~110.6%，相对标准偏差（RSD）为1.3%~16.6%（n=6）。结论该方法选择性好，操作简单安全，快速准确，适用于牛奶中多种农药残留的测定。关键词：固相萃取；气相色谱-串联质谱法；农药残留；牛奶中图分类号：O657.7TS252.41文献标识码：A文章编号：1672-979X（2023）01-0046-06DOI：10.3969/j.issn.1672-979X.2023.01.009SimultaneousDeterminationof41PesticideResiduesinMilkbySolid-phaseExtractionandGasChromatography-tandemMassSpectrometryZHANGYue-hui(LiaoningInspection,ExaminationandCertificationCentre,Shenyang110015,China)Abstract：ObjectiveToestablishamethodforthesimultaneousdeterminationof41pesticideresiduesinmilkbysolid-phaseextractionandgaschromatography-tandemmassspectrometry.MethodsThesamplewaspretreatedbysolid-phaseextraction.Thesamplewasextractedwithacetonitrile,andaftersaltextraction,theextractingsolutionwaspurifiedbyCaptivaEMR-Lipidsolid-phaseextraction.Thepesticideresiduesweredeterminedbygaschromatography-triplequadrupolemassspectrometry.ResultsThereweregoodlinearrelationshipsbetween50-1000ng/mlforthepesticideresiduesandthecorrelationcoefficientsweregreaterthan0.99.At0.02,0.1,0.2mg/kg,theaveragerecoveriesof41pesticideswere60.6%-110.6%,andtherelativestandards(RSDs)were1.3%-16.6%(n=6).ConclusionThemethodisofhighsensitivity,accurate,safe,simpleandsuitablefordeterminationofpesticideresiduesinmilk.KeyWords：solid-phaseextraction;gaschromatography-tandemmassspectrometry;pesticideresidue;milk收稿日期：2021-10-11基金项目：辽宁省自然科学基金指导计划（编号：2019-ZD-0847）作者简介：张月辉，副主任技师，研究方向：食品农残检...
