分散固相萃取-GC-MS/MS联用法测定大米中13种农药残留  

Determination of 13 pesticide residues in rice by disperse solid phase extraction and GC-MS/MS

作　　者：王金鑫 杨清华[2] 施逸岚[2] 仇倩颖 于春梅[1] WANG Jin-xin;YANG Qing-hua;SHI Yi-lan;QIU Qian-ying;YU Chun-mei(Department of Physical and Chemical Laboratory,Nantong Center for Disease Control and Prevention,Nantong,Jiangsu 226000,China;不详)

机构地区：[1]南通大学公共卫生学院,江苏南通226000 [2]南通市疾病预防控制中心理化检验科,江苏南通226000

出　　处：《现代预防医学》2023年第17期3223-3228,共6页Modern Preventive Medicine

基　　金：南通市科技局项目(JC2020111);南通市卫健委面上基金(MB2021074)。

摘　　要：目的建立大米中13种农药残留的分散固相萃取-气相色谱-串联质谱(GC-MS/MS)同时测定方法。方法样品经乙酸乙酯-二氯甲烷(1:1,v/v)提取,无水MgSO4和改性Al2O3分散固相萃取净化,净化液经氮吹浓缩后复溶,过0.22μm膜后,进GC-MS/MS分析,多反应监测模式(MRM)扫描,内标法定量。结果13种农药在0.05~2.5μg/ml范围内线性相关系数均大于0.996;加标回收率在75.6%~105.2%,相对标准偏差在2.44%~4.86%,检出限和定量限分别为1.0~3.5μg/kg和3.0~10.5μg/kg。结论本法回收率高、成本低、灵敏度高、重现性好,可满足大米中多种农药残留的测定。Objective To establish a method for simultaneous determination of 13 pesticide residues in rice by disperse solid phase extraction-gas chromatography-tandem mass spectrometry(GCMS/MS).Methods The samples were extracted by ethyl acetate-dichloromethane(1:1,v/v)and purified by solid phase extraction with anhydrous MgSO4 and modified Al2O3.The purified solution was concentrated by nitrogen blowing and then re-dissolved.After passing through 0.22μm membrane,the sample was analyzed by GC-MS/MS,scanned by multiple reaction monitoring mode(MRM)and quantified by internal standard method.Results The linear correlation coefficients of 13 pesticides were more than 0.996 in the range of 0.05 to 2.5μg/ml,the recovery was 75.6%to 105.2%,the relative standard deviation was 2.44%to 4.86%,and the detection limit and quantitative limit were 1.0 to 3.5μg/kg and 3.0 to 10.5μg/kg,respectively.Conclusion This method has the advantages of high recovery,low cost,high sensitivity,and good reproducibility,which thus can be used for the determination of various pesticide residues in rice.

关 键 词：乙烯基三(2-甲氧基乙氧基)硅烷 GC-MS/MS 农药残留 大米 

分 类 号：R657.63[医药卫生—外科学] TS210.7[医药卫生—临床医学]