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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 establish a method for the determination of fourteen organic solvents in cosmetics by automated headspace-gas chromatography-mass spectrometry (HS-GC / MS). Methods Based on a series of headspace conditions such as headspace equilibrium temperature, headspace equilibrium time and sample volume, the conditions of chromatographic mass spectrometry and pretreatment of samples were optimized, and the analytical methods of organic solvents in various cosmetics were established. Fourteen kinds of organic solvents in cosmetics were extracted by 90 ℃ headspace for 30 min, then separated by HP-INNOWAX capillary column and analyzed by gas chromatography / mass spectrometry. The retention time was qualitative and the external standard method was used for quantification. Results The linear range of acrylonitrile and acetonitrile was 0.5 mg / L ~ 50 mg / L. The linear range of the other 12 organic solvents was 0.05 mg / L ~ 5 mg / L. The detection limits of 14 organic solvents ranged from 1 mg / kg to 3 mg / kg. The recoveries ranged from 73.6% to 98.5%. The relative standard deviations (RSDs) ranged from 1.7% to 6.7%. Conclusion The method is simple, accurate, sensitive, good stability, less impurities, suitable for the simultaneous determination of 14 organic solvents in cosmetics.