超高效液相色谱-高分辨质谱法测定蜂蜜中12种有机磷酸酯类阻燃剂
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作者单位:

1.北京工商大学 食品与健康学院,北京 100048;2.国家食品安全风险评估中心,北京 100021

作者简介:

张弛 男 在读研究生 研究方向为食品科学与工程 E-mail: chi3131@126.com

通讯作者:

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

中图分类号:

R155

基金项目:

国家重点研发计划(2023YFF1105301)


Determination of 12 organophosphate esters in honey by ultra-high-performance liquid chromatography-high-resolution mass spectrometry
Author:
Affiliation:

1.School of Food and Health, Beijing Technology and Business University, Beijing 100048, China;2.China National Center for Food Safety Risk Assessment, Beijing 100021, China

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    摘要:

    目的 建立一种超高效液相色谱-高分辨质谱检测蜂蜜中12种有机磷酸酯(OPEs)类阻燃剂的方法。方法 采用糖诱导乙腈-水液液萃取体系提取、富集和净化分析目标物,以甲醇-甲酸水进行梯度洗脱,采用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结合同位素内标法进行定量。结果 在0.2~20 μg/L范围内,12种OPEs呈良好线性关系(R2>0.99),方法检出限为0.05~0.3 μg/kg,定量限为0.1~0.9 μg/kg,3个不同加标水平的回收率为86.2%~119.5%,相对标准偏差为1.24%~8.16%。在16份蜂蜜样品的检测分析中,磷酸三苯酯的检出率达100%,浓度范围为1.7~11.8 μg/kg,磷酸三乙酯的检出率为50%,浓度范围为未检出~1.5 μg/kg。结论 该方法操作便捷,重现性好,灵敏度高,为蜂蜜中OPEs的痕量检测提供了技术支撑。

    Abstract:

    Objective To develop a method for the determination of 12 organophosphate esters (OPEs) fire retardants in honey by ultra-high-performance liquid chromatography-high-resolution mass spectrometry.Methods The samples were enriched, extracted and cleaned-up by a sugar-induced acetonitrile-water liquid-liquid extraction system, eluted with a gradient of methanol-formic acid-water, and then separated on a HSS T3 chromatographic column (2.1 mm×100 mm, 1.8 μm). The analytes were determined by high-resolution mass spectrometry in the targeted single-ion monitoring mode, with the quantification by isotope internal standard method.Results The linearity of the 12 OPEs, with R2>0.99, was observed from 0.2 to 20 μg/L, while the range of the LODs and the LOQs were 0.05-0.3 μg/kg and 0.1-0.9 μg/kg, respectively. Recoveries of the 12 OPEs at three different spiked levels ranged from 86.2% to 119.5%, with RSDs ranging from 1.24% to 8.16%. Analysis of 16 honey samples revealed 100% detection of TPhP at concentrations ranging from 1.7 to 11.8 μg/kg and 50% detection of TEP at levels from LOD to 1.5 μg/kg.Conclusion The method is convenient, reproducible, sensitive and suitable for the trace determination of OPEs in honey.

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张弛,申慧婧,陈达炜,吴永宁.超高效液相色谱-高分辨质谱法测定蜂蜜中12种有机磷酸酯类阻燃剂[J].中国食品卫生杂志,2024,36(12):1342-1348.

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  • 收稿日期:2024-03-28
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  • 在线发布日期: 2025-03-19
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