色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 477-484.DOI: 10.3724/SP.J.1123.2013.12004

• 研究论文 • 上一篇    下一篇

超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱快速筛查化妆品中的24种激素

李兆永1,2, 王凤美2, 牛增元2, 罗忻2, 张罡2, 陈军辉1   

  1. 1. 国家海洋局第一海洋研究所海洋生态研究中心, 山东 青岛 266061;
    2. 山东出入境检验检疫局检验检疫技术中心, 山东 青岛 266002
  • 收稿日期:2013-12-09 修回日期:2014-01-13 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 牛增元
  • 基金资助:

    国家质检总局科研项目（2011IK224，2011IK037）.

Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry

LI Zhaoyong1,2, WANG Fengmei2, NIU Zengyuan2, LUO Xin2, ZHANG Gang2, CHEN Junhui1   

  1. 1. Research Center for Marine Ecology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;
    2. Technical Center for Inspection and Quarantine of Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China
  • Received:2013-12-09 Revised:2014-01-13 Online:2014-05-08 Published:2014-04-26

PDF

372

被引次数

15

摘要：

建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用（UPLC-LTQ/Orbitrap MS）快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取，用Waters ACQUITY UPLC BEH C18色谱柱（50 mm×2.1 mm，1.7 μm）分离，以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到激素化合物的准分子离子的精确质量数，实现对化妆品中激素的快速筛查；再以保留时间和数据依赖扫描（data dependent scan）模式获得的子离子质谱图进行定性确证。24种激素化合物的质量准确度误差小于3×10-6（3 ppm）；线性良好，相关系数大于0.99；检出限≤10 μg/kg（S/N=3），能满足实际化妆品样品的分析要求。应用该方法对不同剂型的50余种化妆品样品进行筛查分析，结果良好。该方法是化妆品中激素快速筛查、定性识别的有效方法。

关键词: 超高效液相色谱, 化妆品, 激素, 线性离子阱/静电场轨道阱组合质谱

Abstract:

A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) using a gradient elution of acetonitrile/water containing 0.1%(v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3×10-6(3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N=3) of the 24 compounds were ≤10 μg/kg, which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.

Key words: cosmetics, hormones, linear ion trap/orbitrap mass spectrometry (LTQ/Orbitrap MS), ultra high performance liquid chromatography (UPLC)

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