色谱

色谱 ›› 2013, Vol. 31 ›› Issue (5): 481-484.DOI: 10.3724/SP.J.1123.2013.01012

• 技术与应用 • 上一篇    下一篇

同位素稀释-顶空气相色谱-质谱联用法测定化妆品中的二口恶烷残留量

李晶瑞1, 马强1*, 李文涛1, 王超1, 白桦1, 马会娟1, 蔡天培1, 焦阳2, 张晓丽2   

  1. 1. 中国检验检疫科学研究院, 北京 100123;
    2. 国家质量监督检验检疫总局国际检验检疫标准与技术法规研究中心, 北京 100028
  • 收稿日期:2013-01-06 修回日期:2013-01-25 出版日期:2013-05-28 发布日期:2013-05-16
  • 通讯作者: 马强,Tel:(010)85773279,E-mail:maqiang1129@yahoo.com.cn.
  • 基金资助:

    质检公益性行业科研专项项目(2012104013-4,2012104013-9);国家质检总局科技计划项目(2011IK196);国家标准化管理委员会计划项目(20101084-T-607);国家科技支撑计划项目(2013BAK04B03).

Determination of dioxane residue in cosmetics by isotope dilution-headspace gas chromatography-mass spectrometry

LI Jingrui1, MA Qiang1*, LI Wentao1, WANG Chao1, BAI Hua1, MA Huijuan1, CAI Tianpei1, JIAO Yang2, ZHANG Xiaoli2   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    2. Research Center for International Inspection and Quarantine Standard and Technical Regulation, General Administration of Quality Supervision, Inspection and Quarantine, Beijing 100028, China
  • Received:2013-01-06 Revised:2013-01-25 Online:2013-05-28 Published:2013-05-16

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摘要：

建立了化妆品中二(口恶)烷的同位素稀释-顶空气相色谱-质谱联用测定方法。称取2 g化妆品样品于顶空样品瓶中,加入1 g氯化钠及20 mg/L氘代二(口恶)烷内标溶液1 mL,再加入9 mL水。密封后摇匀,置于顶空进样器中,在70 ℃平衡40 min。气液平衡后的上部气体经HP-5MS石英毛细管气相色谱柱(30 m×0.25 mm×0.25 μm)分离后,采用选择离子扫描模式进行质谱定性及定量分析。二(口恶)烷的方法定量限为2.5 mg/kg;在2.5～50 mg/kg的3个添加水平范围内的平均回收率为90.5%～104.0%,相对标准偏差为1.26%～3.98%。本方法准确、简便、快速,能够满足化妆品样品中二(口恶)烷残留量的检测要求。

关键词: 顶空气相色谱-质谱联用, 二(口恶)烷, 化妆品, 同位素稀释

Abstract:

A comprehensive analytical method based on isotope dilution-headspace gas chromatography-mass spectrometry was developed for the determination of dioxane residue in the cosmetics. Cosmetic sample (2 g) was placed in a headspace vial. Then, 1 g sodium chloride, 1 mL d8-dioxane solution (20 mg/L) and 9 mL water were added. The vial was sealed and heated at 70 ℃ for 40 min. The qualitative and quantitative analyses were carried out for the analyte in selected ion monitoring (SIM) mode after the chromatographic separation on an HP-5MS column (30 m×0.25 mm×0.25 μm). The limit of quantification (LOQ) for dioxane was 2.5 mg/kg. The mean recoveries were 90.5%-104.0% at the spiked levels of 2.5-50 mg/kg with the relative standard deviations in the range of 1.26%-3.98%. The method is accurate, simple, rapid, and applicable for the inspection of dioxane residue in cosmetics.

Key words: cosmetics, dioxane, headspace gas chromatography-mass spectrometry (HS-GC-MS), isotope dilution

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