分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量
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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. 国家加工食品质量检验检测中心〔广东〕,广东 广州 511447)

作者简介:

黄曼谷(1996—),女,广州检验检测认证集团有限公司助理工程师。E-mail: 1498513699@qq.com

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广州市市场监督管理局科技项目(编号:2022kj49)


Determination of 11 kinds of pesticide residues in liquid milk by dispersive solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry
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(1. Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou, Guangdong 511447, China; 2. National Quality Inspection and Testing Center for Processed Foods 〔Guangdong〕, Guangzhou, Guangdong 511447, China)

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    摘要:

    目的:评估液态乳中农药残留量的安全性。方法:建立同时测定11种农药残留的超高效液相色谱—串联质谱法。待测样品经乙腈提取,C18和PSA固相萃取剂净化,经色谱柱Xbridge BEH C18 (100 mm×2.1 mm,1.7 μm)分离,多反应监测模式进行测定,并使用响应曲面法优化前处理参数。结果:前处理的最佳条件为乙腈用量10 mL,C18用量50 mg,PSA用量30 mg。11种农药在1.0~100.0 μg/L的浓度范围内线性关系良好,相关系数(R2)均>0.999。在10,20,100 μg/kg添加水平内,11种农药的平均回收率为82.7%~102.0%,相对标准偏差为2.89%~8.87%,检出限和定量限分别为2.0~3.0,5.0~10.0 μg/kg。结论:该方法操作简便,分析时间短,回收率高,重现性好,能够准确定性定量分析液态乳中11种农药残留量。

    Abstract:

    Objective: This study aimed to evaluate the safety of pesticide residues in liquid milk. Methods: A method for simultaneous determination of 11 kinds of pesticide residues by ultra-high-performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted by acetonitrile, purified by C18 and PSA solid phase extractants, separated on a column Xbridge BEH C18 (100 mm×2.1 mm, 1.7 μm), determined in multi-reaction monitoring mode, and optimized for pre-treatment parameters using response surface method. Results: The optimal conditions for pretreatment were 10 mL acetonitrile, 50 mg C18 and 30 mg PSA. The linear relationships of 11 kinds of pesticides were good in the concentration range of 1.0~100.0 μg/L, and the correlation coefficients (R2) were all > 0.999. With addition of 10, 20, 100 μg/kg, the average recoveries were 82.7%~102.0%, the relative standard deviations were 2.89% to 8.87%, and the limits of detection (LOD) and limits of quantitation (LOQ) were 2.0~3.0 μg/kg and 5.0~10.0 μg/kg, respectively. Conclusion: The method is simple, convenient, rapid, high recovery rate and high reproducibility, which could accurately determine 11 kinds of pesticide residues in liquid milk.

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黄曼谷,罗永浩,严婉盈,等.分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量[J].食品与机械,2023,39(12):48-54,87.
HUANG Mangu, LUO Yonghao, YAN Wanying, et al. Determination of 11 kinds of pesticide residues in liquid milk by dispersive solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2023,39(12):48-54,87.

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  • 收稿日期:2022-11-17
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  • 在线发布日期: 2024-01-30
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