高效液相色谱—串联质谱法测定乳制品中9种国际关注除草剂残留量
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1.广州检验检测认证集团有限公司,广东 广州 511447;2.华南农业大学,广东 广州 510642;3.国家粮食和物资储备局广东局,广东 广州 510050

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黄嘉乐(1988—),女,广州检验检测认证集团有限公司质量高级工程师,硕士。E-mail: 673510691@qq.com

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广州市市场监督管理局科技项目(编号:2023kj47)


Determination of residues of 9 herbicides of international concern in dairy products by high performance liquid chromatography-tandem mass spectrometry
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1.Guangzhou Inspection and Testing Certification Group Company Limited, Guangzhou, Guangdong 511447, China;2.South China Agricultural University, Guangzhou, Guangdong 510642, China;3.Guangdong Bureau of the National Food and Strategic Reserves Administration, Guangzhou, Guangdong 510050, China

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    摘要:

    目的 针对乳制品中9种国际关注而中国暂未设定残留限量的除草剂(黄草灵、环嗪酮、茚嗪氟草胺、达草灭、磺酰草吡唑、砜吡草唑、磺酰磺隆、特丁塞隆和吡喃草酮)的精准检测,建立一种快速测定方法。方法 采用乙腈—丙酮混合试剂(体积比8∶2)超声提取目标物,提取液经分散固相萃取吸附剂氟罗里硅土(Florisil)、N-丙基乙二胺(PSA)和无水MgSO4净化后,建立一种高效液相色谱—串联质谱(HPLC-MS/MS)方法进行测定。结果 9种除草剂在7 min内完全分离,在2.00~100 μg/L范围内线性关系良好(r≥0.997),检出限为0.02~0.30 μg/kg,加标回收率为71.6%~104.1%,相对标准偏差为0.4%~10.3%。结论 该方法操作简便、灵敏度高、重现性好,可用于乳制品中9种除草剂残留的快速测定。

    Abstract:

    Objective To establish a rapid and precise determination method for 9 herbicides (asulam, hexazinone, indaziflam, norflurazon, pyrasulfotole, pyroxasulfone, sulfosulfuron, tebuthiuron, and tepraloxydim) in dairy products that are of international concern but without established maximum residue limits (MRLs) in China.Methods The samples are ultrasonically extracted with acetonitrile-acetone mixed reagent (vv=8∶2), and the extract is purified by the dispersed solid-phase extraction adsorbents Florisil, N-propylethylenediamine (PSA), and anhydrous MgSO4. A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method is established for determination.Results The nine herbicides are completely separated within 7 min. Their linear relationships are good within the range of 2.00~100 μg/L (r≥0.997). Their detection limits are 0.02~0.30 μg/kg, spiked recoveries are 71.6%~104.1%, and relative standard deviations are 0.4%~10.3%.Conclusion This method is simple to operate, has high sensitivity and good reproducibility, and can be used for rapid determination of residues of the 9 herbicides in dairy products.

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严婉盈,何敏恒,黎明明,等.高效液相色谱—串联质谱法测定乳制品中9种国际关注除草剂残留量[J].食品与机械,2026,42(1):50-57.
YAN Wanying, HE Minheng, LI Mingming, et al. Determination of residues of 9 herbicides of international concern in dairy products by high performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2026,42(1):50-57.

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  • 收稿日期:2025-05-27
  • 最后修改日期:2025-12-29
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  • 在线发布日期: 2026-01-23
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