摘要
目的建立蔬菜中多种农药残留固相萃取-GC-MS分析方法。方法样品切碎匀浆后加乙腈提取,提取液经Envi-18柱和Carb/NH2柱双重净化,浓缩,正己烷定容,经DB-5MS色谱柱GC-MS法测定,外标法定量。结果各农药组分在0.125μg/mL-1.0μg/mL范围线性关系良好,相关系数≥0.995,加标回收率为67.9%-102.7%,RSD为2.1%-6.2%(n=6),检出限为0.003 mg/kg-0.02 mg/kg。结论方法样品前处理简单,定性定量准确灵敏,能够满足蔬菜中多种农药残留的检测。
Objective to establish a method of determining multiple pesticide residues in vegetables by solid phase extraction(SPE) purification coupled with gas chromatography-mass spectrometry(GC-MS).Methods the chopped samples were homogenized and extracted by acetonitrile,purified by Envi-18 column and Carr/NH2 column,concentrated,re-dissolved in 1 mL hexane,analyzed by GC-MS through DB-5 MS chromatographic column,and quantified by external standard method.Results the linear correlativity among all the tested pesticide components between 0.125 μg/mL-1.0 μg/mL was very prominent,which means the correlation coefficient was not less than 0.995.The recovery rate was 67.9%-102.7%,RSD was 2.1%-6.2%(n=6),maximum amount was 0.003 mg/kg-0.02 mg/kg.Conclusions the SPE/GC-MS method can satisfy the need of determining a variety of pesticide residues in vegetables,not only the preparation is convenient,but also the qualification and quantification are accurate and sensitive.
作者
李亚波
朱建中
王林
LI Yabo ZHU Jianzhong WANG Lin Xiangtan(City Center for Disease Control and Prevention, Hunan 411100, China)
出处
《河南预防医学杂志》
2017年第4期263-266,共4页
Henan Journal of Preventive Medicine