摘要
目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测蔬菜、水果中百菌清残留的方法。方法样品称量后加入乙酸钠缓冲液-乙腈提取液,经振荡、离心后吸取上清液用分散固相萃取净化、离心,后取上清液氮吹至近干;用0.01%甲酸化乙酸乙酯复溶残渣,过滤后采用GC-MS/MS的多反应监测(multi reaction monitoring,MRM)模式进行检测。结果百菌清在0.005~0.500 mg/L质量浓度范围内的相关系数达到0.9983及以上,检出限为0.001~0.002 mg/kg,定量限为0.010 mg/kg。百菌清在3个不同水平的平均加标回收率为70.5%~105.5%,相对标准偏差为1.9%~7.7%,满足农药残留分析的要求。结论本研究建立了GC-MS/MS测定蔬菜、水果中百菌清残留量的检测方法,该方法具有快速、准确优势,可作为蔬菜、水果中百菌清残留检测分析提供有效技术依据。
Objective To establish a method for the determination of chlorothalonil residues in vegetables and fruits by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods Samples were weighed and extracted with an acetonitrile solution containing sodium acetate buffer.After vortexing and centrifugation,the supernatant was collected.The extract was purified using dispersive solid-phase extraction,followed by centrifugation.The supernatant was then concentrated to near dryness under a nitrogen stream.The residue was reconstituted with 0.01%formic acid in ethyl acetate,filtered through a membrane filter,and analyzed by GC-MS/MS using multi reaction monitoring(MRM)mode.Results The correlation coefficient reached 0.9983 or above in the mass concentration range of 0.005-0.500 mg/L,with limits of detection of 0.001-0.002 mg/kg and limits of quantitation of 0.010 mg/kg of chlorothalonil.The average recoveries at 3 different spiked levels were 70.5%-105.5%,with relative standard deviations of 1.9%-7.7%,meeting the requirements for pesticide residue analysis.Conclusion This study successfully establishes a GC-MS/MS method for determining chlorothalonil residues in vegetables and fruits.The method offers rapid and accurate advantages,serving as an effective technical basis for detecting and analyzing chlorothalonil residues in vegetables and fruits.
作者
刘帅
肖泽苗
鄢韬
陈志廷
王威利
万凯
LIU Shuai;XIAO Ze-Miao;YAN Tao;CHEN Zhi-Ting;WANG Wei-Li;WAN Kai(Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences,Guangzhou 510640,China;Guangdong Provincial Key Laboratory of Quality&Safety Risk Assessment for Agro-products,Guangzhou 510640,China;Key Laboratory of Testing and Evaluation for Agro-product Safety and Quality,Ministry of Agriculture and Rural Affairs,People’s Republic of China,Guangzhou 510640,China;Guangdong Agricultural Sciences Monitoring Technology Co.,Ltd.,Guangzhou 510640,China)
出处
《食品安全质量检测学报》
2025年第24期23-28,共6页
Journal of Food Safety and Quality
基金
农业农村部风险评估项目(GJFP20240501)
广东农科院质标所-所长基金项目(DWJJ-202104)。
