食品科学 ›› 2023, Vol. 44 ›› Issue (22): 373-379.doi: 10.7506/spkx1002-6630-20230219-172

• 安全检测 • 上一篇    

基于大气压化学电离的GC-MS/MS法测定动物源性食品中8 种酰胺类除草剂残留

杨志金, 林彬彬, 黄旭良, 陈倩妮, 林小莲, 蓝燕珊   

  1. (厦门市食品药品质量检验研究院,福建 厦门 361013)
  • 出版日期:2023-11-25 发布日期:2023-12-13
  • 基金资助:
    福建省市场监督管理局科技项目(FJMS2020046)

Determination of Eight Amide Herbicide Residues in Animal-derived Foods by Gas Chromatography-Atmospheric Pressure Chemical Ionization-Tandem Mass Spectrometry

YANG Zhijin, LIN Binbin, HUANG Xuliang, CHEN Qianni, LIN Xiaolian, LAN Yanshan   

  1. (Xiamen Institute for Food and Drug Quality Control, Xiamen 361013, China)
  • Online:2023-11-25 Published:2023-12-13

摘要: 建立基于大气压化学电离的气相色谱-串联质谱法,测定动物源性食品中8 种酰胺类除草剂(甲草胺、乙草胺、丙草胺、丁草胺、敌草胺、吡唑草胺、二甲吩草胺、异丙甲草胺)。采用乙腈提取、EMR-Lipid材料净化作为前处理方法,使用乙酸乙酯稀释乙腈净化液代替溶剂转换,大气压化学电离正离子模式多反应监测测定。结果表明,在猪肉、猪肝、鸡蛋、牛奶基质中,8 种酰胺类除草剂的平均加标回收率为63.3%~108%,相对标准偏差为2.51%~13.8%,检出限为0.029~1.3 µg/kg,定量限为0.095~4.2 µg/kg,基质效应为-11%~12%。本方法可有效降低基质效应,简便、高效、准确、灵敏,可用于动物源性食品中8 种酰胺类除草剂的快速定量测定。

关键词: 大气压化学电离;气相色谱-串联质谱法;酰胺类除草剂;动物源性食品

Abstract: A gas chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (GC-APCI-MS/MS) method was established for the determination of the residues of eight amide herbicides (alachlor, acetochlor, propichlor, butachlor, dichlorochlor, pyrazolam, dimethochlor and metolachlor) in animal-derived foods. The sample pretreatment process involved acetonitrile extraction and enhanced matrix removal (EMR)-lipid cleanup, and ethyl acetate was used to dilute the purified acetonitrile extract instead of solvent conversion. The detection was performed with APCI in the positive ion mode using multi-reaction monitoring (MRM). The results showed that the average recoveries of the eight amide herbicides in spiked pork, pig liver, egg and milk matrices were 63.3%–108%, with relative standard deviation (RSD) 2.51%–13.8%. The limit of detection (LOD) was 0.029–1.3 µg/kg, the limit of quantitation (LOQ) was 0.095–4.2 µg/kg, and the matrix effect was −11%–12%. This method can effectively reduce the matrix effect, and is simple, efficient, accurate, sensitive, and suitable for the rapid quantitative determination of the eight amide herbicides in animal-derived foods.

Key words: atmospheric pressure chemical ionization; gas chromatography-tandem mass spectrometry; amide herbicides; animal-derived food

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