取化妆品样品(1.000 g),用二甲基亚砜(DMSO)超声溶解,加DMSO定容至50 mL,分取5.00 mL进行顶空采样,采用平衡温度及时间分别为85 ℃和30 min。采用HP-5MS石英毛细管柱作为分离柱,在50 ℃~220 ℃之间进行程序升温色谱分离。质谱测定中采用EI离子源和SIM检测模式。所测14种挥发性有机化合物的质量浓度均在0.001~1.0 mg·L-1范围内与其峰面积呈线性关系,其检出限(3S/N)在0.019~0.068 μg·g-1之间。以实样为基体,在1.0,20.0 mg·kg-1两种浓度水平上加入混合标准溶液进行回收试验,测得回收率在82.1%~112%之间,测定值的相对标准偏差(n=6)均小于5.0%。

The cosmetic sample (1.000 g) was dissolved ultrasonically in dimethylsulfoxide (DMSO) and made up to 50 mL with the same solvent. An aliquot of 5.00 mL of the sample solution was introduced into the head-space flask and equilibrated at 85 ℃ for 30 min. The volatile organic compounds (VOC) were separated by passing through the HP-5MS quartz capillary column under the mode of programed temperature elevation from 50 ℃ to 220 ℃. Ionization source of EI and SIM mode of detection were adopted in MS determinations. Linear relationships between values of peak areas and mass concentrations of the 14 VOC′s were found in the same range of 0.001-1.0 mg·L-1, and values of DL′s (3S/N) for the 14 VOC′s found were range from 0.019 to 0.068 μg·g-1. Test for recovery was made by standard addition method at the concentration levels of 1.0, 20.0 mg·kg-1 using 2 substantial cosmetic samples as matrixes, giving results of recovery in the range from 82.1% to 112%, with values of RSD′s (n=6) all less than 5.0%.