改进的QuEChERS-凝胶渗透色谱-气相色谱/质谱法测定保健食品中53种农药残留  

Determination of 53 pesticide residues in health food with Modified QuEChERS-gel permeation chromatography-Gas Chromatography/Mass Spectrometry

作　　者：荣维广[1] 季倩 吉文亮[1] 刘华良[1] 宋宁慧[3] RONG Wei-guang;JI Qian;JI Wen-liang;LIU Hua-liang;SONG Ning-hui(Jiangsu Center for Disease Prevention and Control,Nanjing,Jiangsu 210009,China)

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009 [2]南京市疾病预防控制中心,江苏南京210003 [3]环境保护部南京环境科学研究所,江苏南京210042

出　　处：《现代预防医学》2019年第23期4345-4350,共6页Modern Preventive Medicine

基　　金：江苏省医学重点学科-流行病学(课题编号:ZDXKA2016008)

摘　　要：目的建立保健食品中53种农药残留的QuEChERS-凝胶渗透色谱-气相色谱/质谱检测方法。方法样品经QuEChERS提取、凝胶渗透色谱柱净化后,DB-5MS(25 m×0.25 mm,0.25μm)色谱柱分离,质谱检测器检测,外标法定量。结果在0.02 mg/kg添加水平样品的平均回收率除甲胺磷等8种农药在55.7%~77.2%范围内,其余为78.0%~115.2%;相对标准偏差除氧化乐果和甲基毒死蜱大于10%外,其余均小于10%;在0.05 mg/kg添加水平样品的平均回收率除甲胺磷等6种农药在57.7%~77.3%范围内,其余均在78.4%~113.5%范围内;相对标准偏差除氧化乐果外,其余农药均小于10%。速灭威等6种农药的检出限为0.0240~0.0901 mg/kg,其余为0.0012~0.0200 mg/kg。结论该方法消耗试剂少,分析成本低,操作简便快速,适合保健食品中53种农药残留的检测。Objective To develop a method for the determination of 53 pesticides in health food by QuEChERS coupled with on line gel permeation chromatography-Gas Chromatography/Mass Spectrometry(GPC-GC/MS).Methods Samples were exacted by QuEChERS and followed by clean-up treatment with on line GPC,and then separated by DB-5 MS column and the identification and quantification were performed by GC-MS in selected ion monitoring(SIM)mode with the external standard method.Results The average recoveries of 8 pesticides like methamidophos ranged from 55.7%~77.2%,the remaining pesticides were in the range of 78.0%~115.2%,with the relative standard deviations(RSDs,n=6)less than 10%except omethoate,chlorpyrifos methyl,spiked at 0.02 mg/kg.The average recoveries of 6 pesticides like methamidophos ranged from 57.7%~77.3%,the remaining pesticides were in the range of 78.4%~113.5%,with the relative standard deviations(RSDs,n=6)less than 10%except omethoate,spiked at 0.05 mg/kg.The Limits of detection(LODs)of this method ranged from 0.0012~0.0200 mg/kg(S/N=3)except 6 pesticides like Tsumacide were in the range of 0.0240~0.0901 mg/kg.Conclusion The developed method which has proved convenient,time-saving,environmental-friendly,accurate and sensitive is suitable for the determination of 53 pesticide residues in health food.

关 键 词：QUECHERS 气相色谱-质谱法 保健食品 农药残留 

分 类 号：R115[医药卫生—公共卫生与预防医学]