摘要
目的:建立一种均质提取,凝胶色谱净化(GPC),三重四级杆气相色谱质谱(GC-MS)检测蔬菜中多种农药残留的方法。根据MRM全扫描模式(SCAN)结果中的离子丰度比和保留时间定性,离子扫描模式(SIM)定量。方法:采用均质提取,GPC净化,气质联用对蔬菜中的13种农药进行定性及定量分析。结果:GPC对农残测量中干扰物具有更加彻底的净化作用,降低了分析背景,进而改善质谱峰的峰形,提高结果准确度。对13种农药的回收率在76.7%~112.4%之间,RSD<10.5%。结论:本实验建立的均质提取,GPC净化,气质联用测定农残的方法操作简便、提取均匀、净化更彻底、灵敏度更高,符合分析要求。对7个品种共计20个蔬菜样品中13种农药进行测定发现有不同程度的农残检出。
Objective:To establish a method to detect 13 pesticide residues in vegetables by using homogeneous extraction,gel chromatography purification(GPC),and triple quadrupole gas chromatography mass spectrometry(GC-MS).Based on the qualitative ion abundance ratio and retention time in the results of the MRM full scan mode(SCAN),the ion scan mode(SIM) was quantified.Methods:The qualitative and quantitative analysis of 13 pesticides in vegetables was performed by homogeneous extraction,GPC purification and GC-MS.Results:GPC has a more thorough purification effect on the interferences in the measurement of pesticide residues,reduces the analysis background,and then improves the peak shape of the mass spectrum peaks and improves the accuracy of the results.The recoveries of 13 pesticides ranged from 76.7% to 112.4%,and the RSD was less than 10.5%.Conclusion:The method of homogeneous extraction,GPC purification,and GC-MS determination of agricultural residues established in this experiment is simple and convenient,with uniform extraction,more thorough purification,and higher sensitivity,which meets the analytical requirements.Thirteen pesticides in 20 vegetable samples of 7 varieties were measured and found to have different levels of pesticide residues detected.
作者
封丽娟
周文梅
冯琦
FENG Li-juan;ZHOU Wen-mei;FENG Qi(Lianyungang Comprehensive Inspection and Testing Center for Quality and Technology;Lianyungang Inspection and Testing Center For Food and Drug)
出处
《中国标准化》
2019年第S02期98-102,共5页
China Standardization
关键词
农药残留
均质提取
凝胶净化
GC-MS检测
pesticide residues
homogenized extraction
gel permeation chromatography clean up method
GC-MS
作者简介
封丽娟,高级工程师,主要从事食品安全研究;周文梅,工程师,主要从事食品安全检测研究;冯琦,工程师,主要从事食品安全检测研究
