固相萃取-气相色谱-质谱法测定牛乳中54种农药残留  

Determination of 54 Pesticide Residues in Milk by Solid-Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

作　　者：白晓云 马晓冲 齐晓茹 苏运聪 张耀广 李飞 BAI Xiaoyun;MA Xiaochong;QI Xiaoru;SU Yuncong;ZHANG Yaoguang;LI Fei(Key Laboratory of Dairy Quality and Safety Control,Ministry of Agriculture and Rural Affairs,Junlebao Dairy Group Co.Ltd.,Shijiazhuang 050021,China)

机构地区：[1]君乐宝乳业集团股份有限公司,农业农村部乳品质量安全控制重点实验室,河北石家庄050021

出　　处：《乳业科学与技术》2024年第5期12-19,共8页JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY

基　　金：“十四五”国家重点研发计划重点专项(2021YFE0115500);石家庄市科技计划项目(221170243A)。

摘　　要：建立牛乳中54种农药残留的高通量气相色谱-质谱分析方法。采用乙腈振荡提取样品,提取液浓缩后经C18固相萃取柱净化,用乙腈洗脱54种农药,采用气相色谱-质谱法测定,外标法定量。结果表明:54种农药在质量浓度0~1.00μg/m L范围内线性良好,相关系数(R2)均大于0.990,回收率在43.33%~113.87%之间,相对标准偏差1.8%~19.8%(n=6)。该方法准确度高、操作简便快捷,可用于批量检测牛乳中的农药残留,有效节约检测时间。A high-throughput gas chromatography-mass spectrometry method was established for the analysis of 54 pesticide residues in milk.Samples were extracted with acetonitrile while shaking,and the extract was concentrated and purified using solid-phase extraction(SPE)on a C18 column using acetonitrile as the eluent.The external standard method was used for quantification.The results showed that good linearity was observed over the concentration range from 0 to 1.00μg/mL,with correlation coefficient(R2)greater than 0.990.Recoveries were between 43.33%and 113.87%with a relative standard deviation(RSD)of 1.8%–19.8%(n=6).This method is accurate,simple and suitable for large numbers of milk samples.

关 键 词：气相色谱-质谱法 固相萃取 牛乳 农药残留 高通量 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]