大气压气相色谱串联质谱法测定牛奶中的9种新型溴代阻燃剂
作者:
作者单位:

1.中国农业大学动物医学院,北京 100193;2.北京市疾病预防控制中心, 食品中毒诊断与溯源技术北京市重点实验室,北京 100013

作者简介:

杨润晖 女 博士生 研究方向为动物源性食品安全 E-mail:18911582397@163.com

通讯作者:

邵兵 男 研究员 研究方向为食品污染物分析 E­mail:shaobingch@sina.com

中图分类号:

R155

基金项目:

国家重点研发计划(2019YFC1605102);国家自然科学基金青年项目(21607010)


Determination of nine novel brominated flame retardants in milk by atmospheric pressure gas chromatography­triple quadrupole mass spectrometry
Author:
Affiliation:

1.College of Veterinary Medicine, China Agricultural University, Beijing 100193, China;2.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China

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    摘要:

    目的 建立了一种基于大气压气相色谱串联质谱(APGC-MS/MS)同时测定牛奶中9种新型溴代阻燃剂(NBFRs)的方法,并对提取溶剂和净化方法进行了优化。方法 冻干牛奶样品经正己烷/二氯甲烷(1∶1, V/V)提取后,采用GPC净化,浓硫酸进一步除脂后,采用多反应监测模式进行分析。结果 目标化合物在一定浓度范围内线性关系良好,R2均 > 0.99,检测限(LOD)和定量限(LOQ)分别为0.000 2~0.098 4 μg/L(fw)和0.000 5~0.295 2 μg/L(fw)。采用空白牛奶进行加标回收实验,加标回收率为73.94%~116.98%,精密度不大于19.30%。该方法已成功地应用于22份牛奶样品。其中,五溴甲苯、五溴乙苯、2-乙基己基-四溴苯甲酸、1,2-双(2,4,6-三溴苯氧基)乙烷和十溴二苯乙烷是主要的污染物,检出率分别为86.36%、100.00%、54.55%、50.00%和54.55%,浓度分别为0.001~0.20 μg/L(fw)、<LOQ~0.06 μg/L(fw)、<LOQ~0.11 μg/L(fw)和<LOQ~0.85 μg/L(fw)。结论 本方法灵敏度高,精密度和准确度好,可用于牛奶中9种NBFRs的同时测定。

    Abstract:

    Objective A method was developed for the simultaneous determination of nine novel brominated fire retardants (NBFRs) in milk by atmospheric pressure gas chromatography-tandem mass spectrometry (APGC-MS/MS), and the extraction solvent and clean-up method were optimized.Methods The freeze-dried milk samples were extracted by hexane/dichloromethane (1∶1, V/V), cleaned up by GPC and further degreased by sulfuric acid, and then analyzed by Multi-selected reaction monitoring(MRM) mode.Results The result showed that there were good linear relationships for the target compounds in a certain concentration range, with their correlation coefficients (R2) no less than 0.99. The limits of detection and the limits of quantification (LOQs) were 0.000 2-0.098 4 μg/L (fw) and 0.000 5-0.295 2 μg/L (fw), respectively. The spiked recoveries were 73.94%-116.98% with RSD not more than 19.30% using blank milk. The method has been successfully applied to 22 milk samples. Among them, PBT, PBEB, EH-TBB, BTBPE and DBDPE were the major contaminants with the detection rates of 86.36%, 100.00%, 54.55%, 50.00% and 54.55%, respectively. The concentrations were 0.001-0.20 μg/L (fw), < LOQ-0.06 μg/L (fw), < LOQ-0.11 μg/L (fw) and < LOQ-0.85 μg/L (fw), respectively.Conclusion The method was sensitive, precise and accurate, and can be used for the simultaneous determination of 9 NBFRs in milk.

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杨润晖,牛宇敏,邢杨,邵兵.大气压气相色谱串联质谱法测定牛奶中的9种新型溴代阻燃剂[J].中国食品卫生杂志,2022,34(2):247-253.

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  • 收稿日期:2021-10-08
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  • 在线发布日期: 2022-05-18
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