同位素稀释-顶空气相色谱-质谱联用法测定化妆品中的二噁烷残留量  

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

作　　者：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] 

机构地区：[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

出　　处：《色谱》2013年第5期481-484,共4页Chinese Journal of Chromatography

基　　金：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)

摘　　要：建立了化妆品中二噁烷的同位素稀释－顶空气相色谱－质谱联用测定方法．称取2g化妆品样品于顶空样品瓶中，加人1g氯化钠及20mg／L氘代二噁烷内标溶液ImL，冉加入9mL水。密封后摇匀．置于顶夺进样器中．化70℃平衡40min．气液平衡后的上部气体经HP-5MS石英毛细管气相色谱柱（30m×0．25mm×0．25μm）分离后，采用选择离子扫描模式进行质谱定性及定量分析．二噁烷的方法定量限为2。5mg／kg；和2．5～50mg／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噁烷残留量的检测要求。A comprehensive analytical method based on isotope dilution-headspace gas chroma- tography-mass spectrometry was developed for the determination of dioxane residue in the cos- metics. Cosmetic sample （2 g） was placed in a headspace vial. Then, l g sodium chloride, ! mL d8-dioxane solution （20 mg/L） and 9 mL water were added. The vial was sealed and heated at 70 ℃（3 for 40 rain. 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 col- umn （30 m x0.25 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, sim- ple, rapid, and applicable for the inspection of dioxane residue in cosmetics.

关 键 词：同位素稀释 顶空气相色谱-质谱联用 二噁烷 化妆品 

分 类 号：O658[理学—分析化学]