水浸润法取样-气相色谱-质谱法测定纹身贴中24种游离初级芳香胺的含量

Determination of 24 Free Primary Aromatic Amines in Tattoo by Gas Chromatography-Mass Spectrometry with Sampling by Water Infiltration

用水润湿并剥离纹身贴样品的水转印纸后,用玻璃棒取下覆膜上的油墨,置于80℃烘箱中加热至恒重。分取1.0 g,加入乙酸乙酯10 mL,于35℃超声提取60 min。提取液进入气相色谱-质谱仪,不分流进样,在DB-35MS毛细管色谱柱上程序升温分离其中24种游离初级芳香胺,以配有电子轰击离子源的质谱仪检测。结果显示,各游离初级芳香胺的质量浓度均在2.5~30 mg·L^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.8~2.6 mg·kg^(-1)。按标准加入法进行回收试验,回收率为94.8%~99.8%,测定值的相对标准偏差(n=7)为0.60%~2.6%。方法用于7款纹身贴样品的分析,均检出了2,4-二甲基苯胺,检出量为1.32~3.94 mg·kg^(-1)。

After wetting with water and peeling the water-transfer sticker of the tattoo sample, the ink on the film was removed with a glass rod, and heated to constant weight in an oven at 80 ℃. An aliquot(1.0 g) of the sample was taken, and 10 mL of ethyl acetate was added. The mixture was extracted by ultrasound at 35 ℃ for 60 min, and the extract was introduced into gas chromatography-mass spectrometer. Twenty-four free primary aromatic amines were separated by programmed temperature on the DB-35MS capillary column, and detected by the mass spectrometer equipped with electron impact ion source. It was shown that the mass concentrations of each free primary aromatic amine were linearly related with the peak areas in the same range of 2.5-30 mg·L^(-1), with detection limits(3S/N) in the range of 0.8-2.6 mg·kg^(-1). Test for recovery was made by standard addition method, giving results of recovery in the range of 94.8%-99.8%, and RSDs(n=7) of the determined values ranged from 0.60% to 2.6%. The proposed method was applied to the analysis of the 7 actual tattoo samples, and 2,4-dimethylaniline was detected in all samples, with detection amounts in the range of 1.32-3.94 mg·kg^(-1).