摘要
建立了气相色谱-静电场轨道阱质谱(GC-Exactive Orbitrap MS)同时测定牛乳中71种农药残留的检测方法。牛乳样品以1.0%甲酸-乙腈为提取溶剂,采用改进的QuEChERS法进行前处理,净化液氮吹浓缩复溶后,在全扫描(Full MS)模式下测定,基质匹配内标法定量。71种农药的线性关系良好,相关系数(r)均不低于0.99,精确质量数偏差均不大于2.55×10^(-6),方法检出限为1.0~2.0µg/kg,在0.01、0.02、0.10 mg/kg加标浓度下的平均回收率为59.6%~117%,相对标准偏差(RSD)为1.9%~13%。对122份牛乳样品的检测结果表明,共2份超高温灭菌乳检出p,p'-滴滴伊,检出值均低于方法定量下限。该方法简单高效,可用于牛乳中71种农药残留的检测。
A gas chromatography-exactive orbitrap mass spectrometry(GC-Exactive Orbitrap MS)method was established to simultaneous determination of 71 kinds of pesticide residues in milk.The sample was extracted with 1.0%formic acid-acetonitrile solution and pretreated with modified QuEChERS method.The purified liquid was dried,re-dissolved,measured by Full MS mode of GC-Exactive Orbitrap MS and quantified by matrix matching internal standard method.The 71 kinds of pesticides showed good linear relationships within the respective concentration ranges,and the corre-lation coefficients(r)were not less than 0.99.The deviations for each accurate mass number were not more than 2.55×10^(-6),and the detection limits were 1.0-2.0µg/kg.The average recoveries were 59.6%-117%at 0.01,0.02,0.10 mg/kg spiked concentrations,with the relative standard devia-tions(RSDs)of 1.9%-13%.4,4'-DDE was detected in two of ultra-high temperature sterilized milk,and the detected values were all lower than LOQ.The method is simple and efficient,which is suitable for the analysis of 71 kinds of pesticide residues in milk.
作者
张申平
周静
ZHANG Shen-ping;ZHOU Jing(Key Laboratory of Mik and Dairy Products Detection and Monitoring Technoogy for State Market Reguation Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第10期1301-1308,共8页
Journal of Instrumental Analysis
基金
国家市场监督管理总局科技计划项目(2021MK035)。
