摘要
目的建立化妆品中十四种有机溶剂残留的自动顶空-气相色谱-质谱联用(HS-GC/MS)的测定方法。方法通过对顶空平衡温度、顶空平衡时间以及样品体积等一系列顶空条件、色谱质谱条件和样品前处理条件的优化,确立了各种化妆品中有机溶剂残留的分析方法。化妆品中十四种有机溶剂经90℃顶空温度提取30 min后,经HP-INNOWAX毛细管柱分离,采用气相色谱/质谱仪进行分析,以保留时间定性,外标法定量。结果丙烯腈和乙腈的线性范围为0.5 mg/L^50 mg/L,其余12种有机溶剂的线性范围为0.05 mg/L^5 mg/L。14种有机溶剂的检出限为1 mg/kg^3 mg/kg,回收率为73.6%~98.5%,相对标准偏差(RSD)为1.7%~6.7%。结论本方法操作简便,准确,灵敏度高,稳定性好,杂质干扰少,适用于化妆品中14种有机溶剂残留的同时测定。
Objective To develop a method for simultaneous determination of 14 organic solvent residues in cosmetics by auto- mated headspace gas chromatography - mass spectrometry. Methods The experimental conditions of headspace （ such as tem- perature, time and sample volume） , GC and sample treatment were optimized to establish a method for analysis of organic sol- vent residues in cosmetics. Cosmetic samples were extracted by headspace at 90 ℃ for 30 min, then separated by HP - INNO- WAX capillary column, and determined by GC - MS. The retention time of the peaks was used for qualitative analysis, while external standard method was used for quantitative analysis. Results The method had good linearity over the range of 0.05 mg/L -50 mg/L for 12 orgainc solvent residues, while that of acrylonitrile and acetonitrile was between 0.5 mg/L 50 mg/L. The detection limits of the 14 organic solvents ranged from 1 mg/kg to 3 mg/kg with recoveries of 73.6 % - 98.5 % and relative standard deviation （RSD） of 1.7% -6.7% （n = 6）. Conclusion The method is simple, rapid, sensitive and sta- ble, it is suitable for simultaneous monitoring of 14 organic solvent residues in cosmetics.
出处
《中国卫生检验杂志》
北大核心
2014年第6期773-775,778,共4页
Chinese Journal of Health Laboratory Technology
基金
国家质量监督检验总局科技计划项目(2011QK045)
关键词
有机溶剂残留
化妆品
顶空
气相色谱-质谱法
Organic solvent residues
Cosmetics
Headspace
Gas chromatography - mass spectrometry
