超高效液相色谱-串联质谱法测定食用猪油中氯酚类物质
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(广西-东盟食品药品安全检验检测中心,广西 南宁 530001)

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莫迎 女 副主任药师 研究方向为食品质量安全 E-mail:812381259@qq.com通信作者:┣┣(中)通信作者┫┫蒋湘 女 主管药师 研究方向为食品质量安全 E-mail:61513303@qq.com

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广西食品药品监督管理局研究项目(桂食药办科评[2017]8号-9);食品安全地方标准制定(修订)项目(桂地标食2017003号)


Determination of chlorophenols in edible lard by ultra performance liquid chromatography-tandem mass spectrometry
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(Guangxi-ASEAN Food and Drug Safety Inspection and Testing Center,Guangxi Nanning 530001,China)

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    摘要:

    目的 应用超高效液相色谱-串联质谱技术,建立同时测定食用猪油中2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸和五氯酚3种物质的方法。方法 样品用80%乙腈提取,固相萃取(SPE)和正己烷净化萃取后,以Atlantis T3(2.1 mm×150 mm,3 μm)为分析柱,乙腈-5.0 mmol/L乙酸铵溶液为流动相,以电喷雾离子源在负离子多反应监测模式下进行测定,基质匹配外标法定量。结果 2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸和五氯酚在2.0~100.0 μg/L范围内线性关系良好,相关系数(r)均大于0.999,方法检出限分别为0.09、1.59、0.90 μg/kg,定量限分别为0.29、5.28、3.00 μg/kg,回收率为71.9%~109.5%,相对标准偏差为0.2%~9.2%(n=6)。结论 该方法简便、准确、灵敏度高,适用于食用猪油中2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸、五氯酚3种物质的高通量检测。

    Abstract:

    Objective A ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) was developed for the simultaneous determination of 2,4,5-trichlorophenol, 2,4,5-trichlorophenoxyacetic acid and pentachlorophenol in edible lard. Methods The edible lard samples were extracted by 80% acetonitrile, then puried with solid phase extraction(SPE)and exane, and loaded on a Atlantis T3 column (2.1 mm×150 mm,3 μm). Acetonitrile-5.0 mmol/L ammonium acetate solution was used as the mobile phase for gradient elution.The compounds were detected by UPLC-MS/MS with negative electrospray ion source (ESI-) under multiple reaction monitoring mode. The matrix-matched external standard method was used for quantitation. Results 2,4,5-trichlorophenol, 2,4,5-trichlorophenoxyacetic acid and pentachlorophenol had an excellent linear relationship in the range of 2.0-100.0 μg/L with correlation coefficient (r) above 0.999. The limits of detection were 0.09,1.59 and 0.90 μg/kg, and the quantification limits were 0.29,5.28 and 3.00 μg/kg. The recoveries of the three compounds ranged from 71.9%-109.5% with relative standard deviation of 0.2%-9.2% (n=6). Conclusion The method was simple,sensitive and accurate, and was suitable for high-throughput detection for 2,4,5-trichlorophenol, 2,4,5-trichlorophenoxyacetic acid and pentachlorophenol in edible lard.

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莫迎,蒋湘,刘展华,张倩勉,蒋定之,范兴.超高效液相色谱-串联质谱法测定食用猪油中氯酚类物质[J].中国食品卫生杂志,2019,31(2):136-140.

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  • 收稿日期:2019-02-15
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  • 在线发布日期: 2019-05-17
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