同位素稀释技术结合顶空气相色谱-质谱法检测5种气溶胶类化妆品中二噁烷  

Determination of 1,4-dioxane in aerosol cosmetic by new isotope dilution-headspace gas chromatography-mass spectrometry

作　　者：荣维广[1] 朱铭洪[1] 吉文亮[1] 刘华良[1] 霍宗利[1] 宋宁慧[2] Rong Weiguang;Zhu Minghong;Ji Wenliang;Liu Hualiang;Huo Zongli;Song Ninghui(Jiangsu Provincial Center for Disease Control and Prevention,Nanjing 210009,China;Nanjing Institute of Environment Science,Department of Environmental Protection,Nanjing 210042,China)

机构地区：[1]江苏省疾病预防控制中心,南京210009 [2]环境保护部南京环境科学研究所,南京210042

出　　处：《卫生研究》2020年第2期280-284,共5页Journal of Hygiene Research

基　　金：江苏省“科教兴卫工程”医学重点学科(实验室)(No.ZDXKA2016008)。

摘　　要：目的建立同位素稀释技术结合顶空气相色谱-质谱法检测5种气溶胶类化妆品中二噁烷的检测方法。方法用1,3-二甲基-2-咪唑啉酮溶解样品,加入二噁烷-d8内标,转移至顶空进样瓶中,压盖密封后超声15 min,置于自动顶空进样器中顶空进样,经HP-5MS石英毛细管色谱柱(30 m×25 mm,0.25μm)分离后,采用选择离子监测模式,内标法定量。结果在1.0~100 mg/kg的线性范围内,方法线性良好,线性相关系数大于0.999。方法检出限为0.3 mg/kg,在0.3、1.0、5.0和30 mg/kg的4个浓度添加水平的平均回收率为91.4%~104.2%,日内和日间相对标准偏差分别小于6.3%和6.4%(n=6)。结论方法准确、简便、快速,能够满足气溶胶类化妆品中二噁烷残留的检测要求。OBJECTIVE To develop a simple, fast and sensitive analytical method based on isotope dilution-headspace gas chromatography-mass spectrometry for the determination of 1,4-dioxane residue in the aerosol cosmetics. METHODS Sample was successive weighed and dissolved in 1,3-dimehyl-2-imidazolidinone(DMI)solvent and isotope internal standard was added. Then transfered to a 20 mL headspace vial. The headspace vial was sealed and extracted 15 min by ultrasonic-assisted extraction. After separated by HP-5 MS fused silica capillary column(30 m×25 mm,0.25 μm), the compound was analyzed by gas chromatography-mass spectrometry in selected ion monitoring mode(GC-MS-SIM) and quantified by internal standard method. RESULTSThere were good linear correlations with R^2 no less than 0.999 in the range of 1.0-100 mg/kg. The limit of detection(LOD) of this method was 0.3 mg/kg. At 0.3,1.0,5.0 and 30 mg/kg four added concentration,recovery for five kinds of aerosol cosmetic were all between 91.4% and 104.2%. The relative standard deviations(RSDs) were 1.5%-6.3% and 1.7%-6.4%(n=6), respectively. CONCLUSION The developed method has proved convenient, time-saving, accurate and sensitive and suited for determination 1,4-dioxane in aerosol cosmetic.

关 键 词：二噁烷 气溶胶类化妆品 顶空气相色谱-质谱法 

分 类 号：TQ658.3[化学工程—精细化工] R168[医药卫生—公共卫生与预防医学]