超高效液相色谱—串联质谱法同时测定动物源性食品中21种全氟类化合物残留
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(1. 重庆市食品药品检验检测研究院,重庆 401120;2. 国家市场监管重点实验室〔调味品监管技术〕,重庆 401120)

作者简介:

唐韵熙,女,重庆市食品药品检验检测研究院高级工程师,硕士。

通讯作者:

白亚敏(1977—),女,重庆市食品药品检验检测研究院高级工程师,硕士。E-mail:965241582@qq.com

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重庆市科学技术局计划项目(编号:cstc2021jxjl00022)


Simultaneous determination of 21 perfluorinated compounds in animal-derived food by UPLC-MS/MS
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(1. Chongqing Institute for Food and Drug Control, Chongqing 401120, China; 2. State Key Laboratory of Market Regulation 〔Condiment Supervision Technology〕, Chongqing 401120, China)

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    摘要:

    目的:建立超高效液相色谱—串联三重四极杆质谱(UPLC-MS/MS)同时测定动物源性食品中21种全氟类化合物残留的液质联用检测方法。方法:样品经1%甲酸—乙腈提取,C18N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,通过Waters Acquity UPLCBEH C18 色谱柱分离,采用甲醇—5 mmol/L乙酸铵水溶液梯度洗脱,多反应监测(MRM)模式监测,采用电喷雾负离子扫描。结果:21种全氟类化合物在0.2~10.0 ng/mL范围内线性关系良好,定量限(S/N=10)为0.25 μg/kg,在0.25,0.50,1.25 μg/kg 3个加标量下,平均回收率为71%~118%,批内精密度为3.5%~18.3% (n=6);批间精密度为2.2%~13.8%(n=3)。结论:该方法前处理简单快速,灵敏度高,可以满足动物源性食品中全氟类化合物快速、准确的检测要求。

    Abstract:

    Objective: To established a method for determination of 21 perfluorinated compounds in animal-derived food by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods: The sample was extracted with 1% formic acid-acetonitrile, cleaned up with a sorbent mixture of N-propylethylenediamine (PSA), octadecyl bonded silica gel (C18) and graphitized carbon black (GCB), then separated by acetonitrile-5mmol/L ammonium acetate aqueous solution and Acquity UPLC BEH C18, detected by liquid chromatography tandem mass spectrometry in negative mode using the multiple reaction monitoring (MRM) mode. Results: The calibration curves were linear in the range of 0.2~10 ng/mL for the 21 PFAS. The limits of quantification were 0.25 μg/kg. Average recoveries were in the range of 71%~118% with three spiked levels, namely 0.25, 0.50, 1.25 μg/kg. The relative standard deviations (RSDs%) of inter-batch and intra-batch were 3.5%~18.3% (n=6) and 2.2%~13.8% (n=3), respectively. Conclusion: The simple pretreatment and high sensitivity satisfied the fast and accurate detection requirement, meanwhile it is suitable for qualitative and quantitative analysis of perfluorinated compounds in animal-derived food.

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唐韵熙,白亚敏,刘露露,等.超高效液相色谱—串联质谱法同时测定动物源性食品中21种全氟类化合物残留[J].食品与机械,2023,39(7):29-39.
TANG Yun-xi, BAI Ya-min, LIU Lu-lu, et al. Simultaneous determination of 21 perfluorinated compounds in animal-derived food by UPLC-MS/MS[J]. Food & Machinery,2023,39(7):29-39.

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  • 收稿日期:2022-12-19
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  • 在线发布日期: 2023-10-20
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