QuEChERS-气相色谱-质谱法检测火腿中敌敌畏的残留量  

Detection of dichlorvos residues in ham by QuEChERS-gas chromatography-mass spectrometry

作　　者：朱鹏静 刘建辉[1] 李彦生[1] 张婷 段毅宏[1] ZHU Peng-jing;LIU Jian-hui;LI Yan-sheng;ZHANG Ting;DUAN Yi-hong(Health Inspection Center,Yunnan Center for Disease Control and Prevention,Kunming Yunnan,650022,China)

机构地区：[1]云南省疾病预防控制中心卫生检验中心,云南昆明650022

出　　处：《职业与健康》2023年第9期1197-1201,共5页Occupation and Health

摘　　要：目的 采用QuEChERS技术与气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)进行检测,建立一种测定火腿中敌敌畏的分析方法。方法 将粉碎后的火腿样品用乙腈提取,经QuEChERS净化处理后,在全扫Full Scan和单离子监测(single ion monitoring,SIM)模式下检测火腿中的敌敌畏。结果 火腿中的敌敌畏分离度较好,在0.01~1.00μg/mL浓度范围内线性关系良好,相关系数(r)为0.999 9,检出限为0.7μg/kg,定量限为2μg/kg,当添加浓度在5~50μg/kg时,加标回收率在85.2%~105.4%,相对标准偏差为2.68%~7.41%。用本方法对95件火腿进行检测,有24件样品被检出,检出率为25.3%,阳性样品检出浓度为14.82~157.53μg/kg。结论 该方法操作简洁、稳定性和重现性好,能满足火腿中敌敌畏的定性、定量检测。Objective By using QuEChERS-gas chromatography-mass spectrometry(GC-MS),to establish an analytical method for the determination of dichlorvos in ham.Methods The crushed ham samples were extracted with acetonitrile,and purified by QuEChERS.The dichlorvos in ham was analyzed by gas chromatography-mass spectrometry under Full Scan and SIM(single ion monitoring)mode.Results The resolution of dichlorvos in ham was good,and the linear relationships was good in the range of 0.01-1.00μg/mL with the correlation coefficient(r)was 0.9999.The limit of detection was 0.7μg/kg,and the limit of quantitation was 2μg/kg.When the addition concentration was 5-50μg/kg,the recovery of standard addition was 85.2%-105.4%,and the relative standard deviation was 2.68%-7.41%.95 ham samples were tested by this method,the dichlorvos was detected in 24 samples,the detection rate was 25.3%,and the detection concentration of positive samples was 14.82-157.53μg/kg.Conclusion The method is simple in operation,stable and reproducible,and can be used for the qualitative and quantitative determination of dichlorvos in ham.

关 键 词：QUECHERS 气相色谱-质谱法 火腿 敌敌畏 

分 类 号：R115[医药卫生—公共卫生与预防医学]