职业与健康 ›› 2023, Vol. 39 ›› Issue (9): 1197-1201.

• 论著 • 上一篇    

QuEChERS-气相色谱-质谱法检测火腿中敌敌畏的残留量

朱鹏静, 刘建辉, 李彦生, 张婷, 段毅宏   

  1. 云南省疾病预防控制中心卫生检验中心,云南 昆明 650022
  • 收稿日期:2022-08-11 修回日期:2022-09-06 发布日期:2026-03-13
  • 通信作者: 段毅宏,副主任技师,E-mail:363664164@qq.com
  • 作者简介:朱鹏静,女,技师,主要从事卫生理化检验、食品风险监测与食品安全工作。

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

ZHU Peng-jing, LIU Jian-hui, LI Yan-sheng, ZHANG Ting, DUAN Yi-hong   

  1. Health Inspection Center,Yunnan Center for Disease Control and Prevention,Kunming Yunnan 650022,China
  • Received:2022-08-11 Revised:2022-09-06 Published:2026-03-13
  • Contact: DUAN Yi-hong,Deputy chief technician,E-mail:363664164@qq.com

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0.01~1.00 μg/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0.7 μg/kg,定量限为2 μg/kg,当添加浓度在5~50 μg/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14.82~157.53 μg/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。

关键词: QuEChERS, 气相色谱-质谱法, 火腿, 敌敌畏

Abstract: 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 0.01-1.00 μg/mL with the correlation coefficient(r) was 0.999 9. The limit of detection was 0.7 μg/kg,and the limit of quantitation was 2 μg/kg. When the addition concentration was 5-50 μg/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 14.82-157.53 μg/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.

Key words: QuEChERS, gas chromatography-mass spectrometry, ham, dichlorvos

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