建立同时快速测定动物源性食品中17种农药的在线凝胶渗透色谱-气相色谱-质谱联用法
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(1.惠州出入境检验检疫局综合技术中心,广东 惠州 516006;2.岛津企业管理(中国)有限公司,广东 广州 510010)

作者简介:

吕飞 女 工程师 研究方向为食品中农兽药残留分析 E-mail:lvfei1026@163.com

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广东省惠州市科技计划项目(2012G024)


Establishment of a method for the simultaneous and rapid detection of 17 pesticide residues in animal derived foods using on-line GPC-GC-MS
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(Comprehensive Technology Center of Huizhou Entry-Exit Inspection and Quarantine Bureau, Guangdong Huizhou 516006,China)

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    摘要:

    建立猪肉、鸡蛋、牛奶、猪脂肪等动物源性食品中同时检测17种农药残留的在线凝胶渗透色谱-气相色谱-质谱联用法(GPC-GC-MS)。方法 样品用正己烷饱和乙腈溶液均质提取,加入氯化钠盐析,离心分层,取部分乙腈层经固相萃取(NH2)柱净化,利用在线GPC-GC-MS测定。结果 在0.85~30 μg/L范围内相关系数均在0.95以上,回收率在61.2%~126%之间。17种农药残留最低检出限范围(以信噪比S/N≥3计)为0.25~3.00 μg/L,定量限范围(以信噪比S/N≥10计)为0.85~10.0 μg/L。结论 该法有效、耐用、快速、灵敏,符合法规残留限量检测要求。

    Abstract:

    To establish an on-line GPC-GC-MS analytic method to determine 17 pesticide residues simultaneously and rapidly in animal derived foods including pork, egg, milk and fat.Methods The pesticide residues were extracted from samples with acetonitrile assisted by n-hexane, salting-out with NaCl and separated through acentric. The supernatant liquid was cleaned up by SPE (NH2), and detected with on-line GPC-GC-MS system. Results The calibration curves of 17 pesticide residues were linear in the range of 0.85-30 μg/L with correlation coefficients above 0.95. The recoveries of the method ranged from 61.2% to 126%. The limits of detection and the limits of quantification were 0.25-3.00 μg/L (S/N≥3) and 0.85-10.0 μg/L (S/N≥10). Conclusion The method was effective, rapid, sensitive, and suitable for the monitoring of the maximum residue limits (MRLs) of 17 pesticide residues in animal derived foods.

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吕飞,李华东,叶英,卓晓娟,朱事康,黄刚.建立同时快速测定动物源性食品中17种农药的在线凝胶渗透色谱-气相色谱-质谱联用法[J].中国食品卫生杂志,2016,28(1):69-75.

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  • 收稿日期:2015-08-03
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  • 在线发布日期: 2016-02-19
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