超高效液相色谱-高分辨质谱法测定牛奶中7种有机磷酸酯类阻燃剂
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作者单位:

1.国家食品安全风险评估中心,国家卫生健康委员会食品安全风险评估重点实验室,中国医学科学院创新单元2019RU014号,北京 100021;2.内蒙古伊利实业股份有限公司,内蒙古 呼和浩特 010110

作者简介:

王轩 男 助理研究员 研究方向为食品安全 E-mail:wangxuan@cfas.net.cn

通讯作者:

陈达炜 男 研究员 研究方向为食品安全 E-mail:chendw@cfas.net.cn

中图分类号:

R155

基金项目:

国家自然科学基金(21607035)


Determination of seven organophosphate esters in milk by ultra-high-performance liquid chromatography-high-resolution mass spectrometry
Author:
Affiliation:

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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    摘要:

    目的 建立牛奶中7种有机磷酸酯类(OPEs)阻燃剂的超高效液相色谱-高分辨质谱分析方法。方法 基于乙腈-冷冻诱导液液萃取技术提取、净化和富集样品,以甲醇-水作为流动相,梯度洗脱程序,HSS T3色谱柱(2.1 mm×100 mm,1.8 μm)分离,高分辨质谱靶向单一离子监测模式测定,内标法定量。结果 7种OPEs在0.2~20 μg/L范围内呈良好的线性关系(R2>0.99),方法检出限为0.01~0.21 μg/L,定量限为0.04~1.72 μg/L,3个不同加标水平的回收率为88.4%~118%,相对标准偏差为1.15%~7.15%。结论 该方法操作简便,重复性好,灵敏度高,可应用于牛奶中OPEs的痕量检测。

    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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王轩,郭战辉,张弛,方从容,李少华,赵云峰,陈达炜.超高效液相色谱-高分辨质谱法测定牛奶中7种有机磷酸酯类阻燃剂[J].中国食品卫生杂志,2023,35(5):692-698.

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  • 收稿日期:2023-03-02
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  • 在线发布日期: 2023-08-14
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