Determination of nine novel brominated flame retardants in milk by atmospheric pressure gas chromatography­triple quadrupole mass spectrometry
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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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R155

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    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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YANG Runhui, NIU Yumin, XING Yang, SHAO Bing. Determination of nine novel brominated flame retardants in milk by atmospheric pressure gas chromatography­triple quadrupole mass spectrometry[J].中国食品卫生杂志,2022,34(2):247-253.

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  • Received:October 08,2021
  • Revised:
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  • Online: May 18,2022
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