QuEChERS-气相色谱-质谱法测定大米中8种农药残留  

Determination of 8 pesticide residues in rice based on QuEChERS gas chromatography-mass spectrometry

作　　者：曲肖华 陈淑梅 孙学景 QU Xiao-hua;CHEN Shu-mei;SUN Xue-jing(Market Supervision and Administration Bureau of Hekou District,Dongying City,Dongying 257200,China;Market Supervision and Administration Bureau of Kenli District,Dongying City,Dongying 257500,China)

机构地区：[1]东营市河口区市场监督管理局,山东东营257200 [2]东营市垦利区市场监督管理局,山东东营257500

出　　处：《粮食与饲料工业》2024年第3期79-83,共5页Cereal & Feed Industry

摘　　要：为更好地检测大米中的农药残留,提高食品安全性,建立了一种基于QuEChERS-气相色谱-质谱法,以快速测定大米中异稻瘟净、异丙草胺、甲霜灵、扑草净、乙草胺、异丙甲草胺、灭绣胺、甲氰菊酯这8种农药残留。在前处理中,将大米试样先经过加速溶剂萃取,再进行QuEChERS净化,其中,氮吹温度应为40℃,复溶试剂为丙酮。再按照设定的气相色谱、质谱参数进行测试。结果表明,8种农药在质量浓度50~1 000 ng/mL,表现出良好的线性关系,线性范围均为0.01~1μg/mL,线性相关系数R~2均大于0.99。同时,在20、50、70μg/kg这3个加标水平下,该检测方法加标回收率为77.2%~123.1%,相对标准偏差RSD为1.0%~6.5%。另外,该检测方法的检出限在6.83~22.09μg/kg,定量限在22.75~73.62μg/kg。综上所述,试验中建立的检测方法有着简单、便捷、回收率高、灵敏度高等优良特点,可以适用于大米中异稻瘟净等8种农药的检测。In order to better detect pesticide residues in rice food and improve food safety,a method based on QuEChERS gas chromatography-mass spectrometry was established for the rapid determination of eight pesticide residues in rice,including isopyrifos,promethazine,methamphetamine,promethazine,acetaminophen,and fenpropathrin.In the pre-treatment,the rice sample was first subjected to accelerated solvent extraction,followed by QuEChERS purification.The nitrogen blowing temperature should be 40 ℃,and the re dissolving reagent was acetone.Then the test was carried out according to the set parameters of gas chromatography and mass spectrometry.The results showed that the 8 pesticides showed a good linear relationship in the mass concentration range of 50-1 000 ng/mL,the linear range was 0.01-1 μg/mL,and the linear correlation coefficient R~2 was greater than 0.99.At 20,50 and 70 μg/kg,the recoveries ranged from 77.2% to 123.1%,and the relative standard deviations(RSD) ranged from 1.0% to 6.5%.In addition,the detection limits of the method were 6.83-22.09 μg/kg,and the limits of quantification were 22.75-73.62 μg/kg.In summary,the detection method established in this experiment has the advantages of simple,convenient,high recovery rate and high sensitivity,and can be applied to the detection of 8 kinds of pesticides in rice.

关 键 词：气相色谱 大米 农药残留 线性相关系数 加标回收率 相对标准偏差 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]