分散固相萃取—超高效液相色谱—串联质谱法测定乳制品中8种杀虫剂
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严婉盈,女,广州检验检测认证集团有限公司工程师,学士

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广州市市场监督管理局科技项目(编号:2022kj49)


Determination of eight kinds of insecticides in dairy products by dispersed solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry
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    摘要:

    目的:快速测定乳制品(纯乳、发酵乳、乳粉)中8种杀虫剂残留量。方法:建立分散固相萃取—超高效液相色谱—串联质谱(UPLC-MS/MS)法,样品经乙腈—丙酮溶液(V乙腈∶V丙酮=80∶20)超声提取,提取液使用吸附剂氟罗里硅土、N-丙基乙二胺和无水MgSO4净化,净化后样液进入UPLC-MS/MS进行检测,在多反应检测扫描模式下进行定性和定量分析。结果:苯线磷、吡虫啉、多杀霉素、呋虫胺、甲氨基阿维菌素苯甲酸盐、灭多威、噻虫啉、杀线威8种杀虫剂在2.00~100μg/L的线性范围内相关系数(r)均大于0.99,检出限为0.010~0.30μg/kg,回收率为82.6%~97.5%,相对标准偏差(RSDs)为1.2%~4.6%(n=6)。结论:该方法简便快捷、灵敏度高、重现性好,适用于乳制品中杀虫剂的快速测定。

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    Objective: To detect eight kinds of insecticides in dairy products (pure milk, fermented milk, milk powder) rapidly. Methods: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method based on dispersive solid phase extraction pre-treatment technology was established. The samples were extracted with acetonitrile-acetone solution (Vacetonitrile∶Vacetone=80∶20) in ultrasonic way, and the extraction solution was purified by Florisil, primary secondary amine and anhydrous MgSO4.After purification, the samples were analyzed by HPLC-MS/MS qualitatively and quantitatively in multi reaction monitoring (MRM) mode. Results: The correlation coefficient (r) of fenamiphos, imidacloprid, spinosad, dinotefuran, emamectin benzoate, methomyl, thiacloprid and oxamyl in the linear range of 2.00~100 μg/L was greater than 0.99,the limits of detection were 0.010~0.30 μg/kg, the recoveries of method were 82.6%~97.5%, and the relative standard deviations (RSDs) were 1.2%~4.6% (n=6). Conclusion: The method is simple, rapid, sensitive and reproducible. It is suitable for the rapid screening of insecticides in dairy products.

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严婉盈,何敏恒,温恒,等.分散固相萃取—超高效液相色谱—串联质谱法测定乳制品中8种杀虫剂[J].食品与机械,2022,(12):44-49.
YAN Wan-ying, HE Min-heng, WEN Heng, et al. Determination of eight kinds of insecticides in dairy products by dispersed solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2022,(12):44-49.

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  • 在线发布日期: 2023-02-28
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