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
曲肖华 1陈淑梅 1孙学景2
作者信息
- 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
- 折叠
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 0.01～1 μg/mL,线性相关系数R2 均大于 0.99.同时,在 20、50、70 μg/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 6.83～22.09 μg/kg,定量限在 22.75～73.62 μg/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.
Abstract
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 sam-ple 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 R2 was greater than 0.99.At 20,50 and 70μg/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 6.83-22.09μg/kg,and the limits of quantification were 22.75-73.62μg/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Key words
gas chromatography/rice/pesticide residues/linear correlation coefficient/standard recovery rate/relative standard deviation引用本文复制引用
出版年
2024
NETL
NSTL
万方数据