HPLC-MS法测定茯苓中4种氨基甲酸酯类农药残留
Determination of Four Carbamate Pesticide Residues in Poria cocos by HPLC-MS
甄达贵 1石芬 2唐树冬 1张和春 1蒋世双1
作者信息
- 1. 靖州苗族侗族自治县质量计量检验检测中心,湖南 怀化 418400
- 2. 中南粮油食品科学研究院有限公司,湖南 长沙 410000
- 折叠
摘要
目的:建立QuEChERS样品前处理结合高效液相色谱-串联质谱法检测茯苓中氨基甲酸酯类农药的检测方法.方法:茯苓样品用含 1%醋酸的乙腈溶液提取,盐析剂盐析后加入MgSO4、PSA和C18 进行萃取、净化,高效液相色谱-串联质谱仪检测,根据色谱峰的保留时间及特征离子对定性,基质匹配标准曲线外标法定量.结果:在2.0～100.0 μg·L-1 时,各目标物线性关系良好,相关系数R2＞0.998;在0.015 mg·kg-1、0.060 mg·kg-1和 0.600 mg·kg-1 添加水平下,回收率在 77.3%～117.2%,相对标准偏差为 0.2%～3.1%(n=6);方法检出限在0.60～1.00 μg·kg-1.结论:该方法准确度高、灵敏度好、高效快速,可用于茯苓中 4 种氨基甲酸酯类农药残留量的质量控制.
Abstract
Objective:To establish a method for the detection of carbamate pesticides in Poria cocos by QuEChERS sample preparation combined with high performance liquid chromatography tandem mass spectrometry.Method:Poria cocos samples were extracted with acetonitrile solution containing 1%acetic acid,salting out agent and then salting out with MgSO4,PSA and C18 were added for extraction and purification,detected by high performance liquid chromatography tandem mass spectrometry,qualitative according to the retention time and characteristic ion pairing of chromatographic peaks,and quantified by matrix matching standard curve.Result:In 2.0～100.0 μg·L-1,the correlation coefficient was good,R2＞0.998;when the addition levels of 0.015 mg·kg-1,0.060 mg·kg-1 and 0.600 mg·kg-1,the recoveries were 77.3%～117.2%,the relative standard deviation was 0.2%～3.1%(n=6);the detection limit was 0.60～1.00 μg·kg-1.Conclusion:This method has high accuracy,sensitivity,efficiency and rapidity,and can be used for quality control of four carbamate pesticide residues in Poria cocos.
关键词
茯苓/克百威/灭多威/丁硫克百威/丙硫克百威/高效液相色谱串联质谱法Key words
Poria cocos/carbofuran/methomyl/carbosulfan/benfuracarb/high performance liquid chromatography tandem mass spectrometry引用本文复制引用
基金项目
湖南省市场监督管理局科技计划项目(2023KJJH45)
出版年
2024
NETL
NSTL
万方数据