超高效液相色谱—串联质谱法测定生牛乳中10种新烟碱类农药残留
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1.上海市农产品质量安全中心,上海 201708;2.农业农村部食品质量监督检验测试中心(上海),上海 201708

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张维谊(1977—),女,上海市农产品质量安全中心推广研究员,硕士。E-mail:zhangharewei@163.com

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上海市奶业优势特色产业集群科研类项目


Simultaneous determination of 10 neonicotinoid pesticides in raw milk by ultra-high performance liquid chromatography tandem mass spectrometry
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Affiliation:

1.Shanghai Center of Agri-product Quality and Safety, Shanghai 201708, China;2.Food Quality Supervision and Inspection Center of Ministry of Agriculture and Rural Affairs (Shanghai), Shanghai 201708, China

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    摘要:

    目的 建立分散固相萃取结合超高效液相—串联质谱(UPLC-MS)同时检测生牛乳中10种新烟碱类农药残留的分析方法。方法 生牛乳样品用乙腈提取,提取液加入QuECHERS盐包盐析,采用分散固相萃取剂净化,净化液以超高效液相色谱—串联质谱测定,通过外标法定量。结果 10种化合物在一定浓度范围内呈现良好的线性关系(R2>0.999),方法检出限为0.2~0.5 μg/kg,定量限为1 μg/kg,生牛乳中1.0,2.5,5.0 μg/kg 3个添加水平的平均加标回收率在75.9%~108.9%,日内精密度为1.8%~7.6%,日间精密度低于11.7%。结论 该方法前处理简便、重现性好、灵敏度高,适用于生牛乳中新烟碱类农药的残留检测。

    Abstract:

    Objective To establish an analysis method for the simultaneous determination of 10 neonicotinoid pesticide residues in raw milk by dispersive solid-phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS).Methods The samples are extracted with acetonitrile, salted out with a QuECHER salt pocket, and purified by the dispersive solid-phase extraction (d-SPE) method. The analytes are detected by UPLC-MS/MS and quantified by the external standard method.Results 10 targeted compounds show a good linear relationship in a certain concentration range with the coefficient of determination (R2) over 0.999. The limits of detection (LODs) are 0.2~0.5 μg/kg, while the limits of quantification (LOQs) are 1.0 μg/kg. At the supplemental levels of 1.0, 2.5, and 5.0 μg/kg, the average recovery rates of standard addition of analytes in raw milk are between 75.9%~108.9%, with the intra-day precision (RSDr) of 1.8%~7.6% and the inter-day precision (RSDR) less than 11.7%.Conclusion The established method is simple for pretreatment and has good repeatability and high sensitivity. It is suitable for the detection of neonicotinoid pesticide residues in raw milk.

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高猛峰,童金蓉,梅博,等.超高效液相色谱—串联质谱法测定生牛乳中10种新烟碱类农药残留[J].食品与机械,2025,(1):74-79.
GAO Mengfeng, TONG Jinrong, MEI Bo, et al. Simultaneous determination of 10 neonicotinoid pesticides in raw milk by ultra-high performance liquid chromatography tandem mass spectrometry[J]. Food & Machinery,2025,(1):74-79.

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  • 收稿日期:2023-04-18
  • 最后修改日期:2024-11-25
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  • 在线发布日期: 2025-03-31
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