三重四级杆串联气相色谱-质谱联用仪检测黄芪中6种农药残留

Detection of six pesticide residues in astragalus by triple quadrupole gas chromatography-tandem mass spectrometry

目的采用三重四级杆串联气相色谱-质谱联用仪(GC/MS/MS),对药食同源物质黄芪中的克百威、乐果、三氯杀螨醇、乙酰甲胺磷、高效氯氟氰菊酯、辛硫磷6种农药残留量进行分析。方法样品经乙腈超声提取后采用QuECHRS萃取包净化,用VF-1701 ms(30 m×0.25 mm×0.25μm)毛细管色谱柱分离,在电子轰击电离(EI)源下采用选择反应监测模式(MRM)进行测定,基质匹配标准溶液外标法定量分析。结果用本法测定,克百威、乐果、三氯杀螨醇、乙酰甲胺磷、高效氯氟氰、辛硫磷色谱峰得到很好的分离,最重要的是实现了不稳定农药辛硫磷的同时检测,6种农药残留在0.005μg/ml~0.5μg/ml浓度范围内成良好的线性关系。线性相关系数均达到0.9998,方法检出限均为0.003 mg/kg,定量限均为0.010 mg/kg。6种农药残留的加标回收率为87%~117%,相对标准偏差均<6.2%。结论此方法操作简便,准确度、精密度、灵敏度均能满足药食同源物质黄芪中含辛硫磷在内的6种农药残留检测技术要求,为开发含辛硫磷农药的多组分农药残留检测技术提供了新思路。

Objective This paper aims to detect and analyze six pesticide residues in astragalus,including carbofuran,dime⁃thoate,dicofol,acephate,lambda-cyhalothrin and phoxim,by triple quadrupole gas chromatography-tandem mass spectrom⁃etry(GC/MS/MS).Methods The samples were sonicated by acetonitrile and purified by QuECHRS extraction package.Then,the extracts were separated by VF-1701 ms capillary column(30 m×0.25 mm×0.25μm).Selective reaction monito⁃ring mode(MRM)was performed under electron bombardment ionization(EI)source,and matrix matching standard solution external standard method was carried out for quantitative analysis.Results The chromatography-peaks of carbofuran,dime⁃thoate,dicofol,acephate,lambda-cyhalothrin and phoxim were well separated,the determination of phoxim was realized sim⁃ultaneously,and the linear relationship was achieved in the concentration range of 0.005μg/ml-0.5μg/ml.The correlation coefficient(r)was 0.9998,the detection limit was 0.003 mg/kg,and the limit of quantitation was 0.010 mg/kg.The stand⁃ard recoveries of six pesticide residues were within 87%-117%,and the relative standard deviations(RSDs)were all<6.2%.Conclusion It is easy to operate,and the obtained accuracy,precision and sensitivity can meet the detection require⁃ments of six pesticide residues including phoxiphos in astragalus.This study provides a new idea for the development of detection technology for multicomponent pesticide residues containing phoxim.