婴幼儿配方奶粉中六溴环十二烷的超高效液相色谱-串联质谱法测定
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作者单位:

江苏省疾病预防控制中心,江苏 南京 210009

作者简介:

沈菲 女 主管技师 研究方向为理化检验 E-mail:njutcmsf@126.com

通讯作者:

吉文亮 男 主任技师 研究方向为理化检验 E-mail:641827872@qq.com

中图分类号:

R155

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Determination of hexabromocyclododecanes in infant formula by ultra high performance liquid chromatography-tandem mass spectrometry
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Jiangsu Provincial Center for Disease Control and Prevention, Jiangsu Nanjing 210009, China

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    摘要:

    目的 建立超高效液相色谱-串联质谱法测定婴幼儿配方奶粉中六溴环十二烷的方法。方法 样品经水溶解,乙腈溶液提取,用增强型脂质去除净化填料(EMR-Lipid)结合QuEChERS分散吸附剂净化除杂,以水和甲醇/乙腈(50∶50,V/V)为流动相进行梯度洗脱,经ACQUITY UPLC BEH C18(2.1×100 mm,1.7 μm)色谱柱分离,负离子模式下以多反应监测方式检测,同位素稀释法定量。结果 在0.5~50 μg/L范围内,3种六溴环十二烷的相关系数(r)均在0.999以上,检出限为0.01~0.04 μg/kg,定量限为0.03~0.13 μg/kg,回收率为92.1%~100.2%,相对标准偏差为1.2%~3.8%。结论 该方法简便、灵敏、准确,适用于婴幼儿配方奶粉中六溴环十二烷的检测。

    Abstract:

    Objective To establish a method for the determination of hexabromocyclododecanes in infant formula using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods The samples were dissolved in water,extracted with acetonitrile, and purified with enhanced matix removal lipid (EMR-Lipid) combined with QuEChERS dispersed adsorbent. The analytes were separated on an ACQUITY UPLC BEH C18 column (2.1×100 mm, 1.7 μm) with water and methanol/acetonitrile (50∶50, V/V) as mobile phases. The target compounds were analyzed by multiple reaction monitoring mode(MRM) and quantified by isotope dilution internal standard method in negative scanning mode.Results The correlation coefficients (r) of three hexabromocyclododecanes were above 0.999 in the range of 0.5-50 μg/L. The detection limits and quantitative limits were in the range of 0.01-0.04 μg/kg and 0.03-0.13 μg/kg, respectively. The recoveries ranged from 92.1% to 100.2%, and the relative standard deviation were 1.2%-3.8%.Conclusion The method is simple, accurate and sensitive, and can be used to detect hexabromocyclododecanes in infant formula.

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沈菲,王溪,朱峰,张立辉,谷静,吉文亮.婴幼儿配方奶粉中六溴环十二烷的超高效液相色谱-串联质谱法测定[J].中国食品卫生杂志,2025,37(5):432-437.

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  • 收稿日期:2024-06-28
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  • 在线发布日期: 2025-08-20
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