Determination of seven organophosphate esters in milk by ultra-high-performance liquid chromatography-high-resolution mass spectrometry
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1.NHC Key Laboratory of Food Safety Risk Assessment, Chinese Academy of Medical Sciences Research Unit No.2019RU014, China National Center for Food Safety Risk Assessment, Beijing 100021, China;2.Inner Mongolia Yili Industrial Group Co., Ltd., Inner Mongolia Hohhot 010110, China

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R155

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    Abstract:

    Objective An analytical method was established to determine seven organophosphate esters (OPEs) flame retardant residues in milk by ultra-high-performance liquid chromatography-high-resolution mass spectrometry.Methods Samples were extracted, cleaned up, and enriched using an acetonitrile-water cold-induced liquid-liquid extraction (CI-LLE) technique. The chromatographic separation of OPEs was performed on an HSS T3 column (2.1 mm × 100 mm, 1.8 μm) by gradient elution using methanol-water as mobile phases. The analytes were detected by high-resolution mass spectrometry using targeted single-ion monitoring mode, and the internal standard method was used for quantitative analysis.Results The determination of seven OPEs showed a good linear relationship ranging from 0.2 to 20 μg/L (R2 >0.99). The limits of detection and quantitation were in the ranges of 0.01-0.21 μg/L and 0.04-1.72 μg/L, respectively. At three different spiked levels, the recoveries for pesticides in blank samples ranged from 88.4% to 118%, with relative standard deviation of 1.15-7.15%.Conclusion This method is simple, reproducible, and sensitive and can be applied to determine trace OPEs in milk.

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WANG Xuan, GUO Zhanhui, ZHANG Chi, FANG Congrong, LI Shaohua, ZHAO Yunfeng, CHEN Dawei. Determination of seven organophosphate esters in milk by ultra-high-performance liquid chromatography-high-resolution mass spectrometry[J].中国食品卫生杂志,2023,35(5):692-698.

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  • Received:March 02,2023
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  • Online: August 14,2023
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