应用液相色谱-串联质谱法测定化妆品中联苯胺、4,4′二氨基二苯醚、邻氨基甲苯醚、3,3′二甲基联苯胺、2,4,5三甲基苯胺、4,4′二氨基二苯硫醚、5硝基邻甲苯胺、3,3′二氯联苯胺、4氨基偶氮苯等9种禁用芳香胺的含量。样品经1%(φ)三氯乙酸溶液和乙腈提取,分取部分上清液经固相萃取小柱净化。所得净化液以C18色谱柱(50 mm×4.6 mm,1.8 μm)为分离柱,以不同体积比的0.05%(φ)甲酸溶液和含0.05%(φ)甲酸的乙腈的混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。3,3′二氯联苯胺的线性范围为0.5~50 mg·kg-1,检出限(3S/N)为0.15 mg·kg-1。其余8种芳香胺的线性范围均为0.2~50 mg·kg-1,检出限(3S/N)均为0.05 mg·kg-1。加标回收率在78.3%~103%之间,测定值的相对标准偏差(n=6)均小于6.0%。

LCMS/MS was applied to the determination of 9 banned aromatic amines, i.e. benzidine, 4,4′oxydianiline, oanisidine, 3,3′dimethylbenzidine, 2,4,5trimethylaniline, 4,4′thiodianiline, 5nitrootoluidine, 3,3′dichlorobenzidine and 4aminoazobenzene in cosmetics. The sample was extracted with 1% (φ) trichloroacetic acid solution and acetonitrile. An aliquot of the supernatant was purified on solid phase extraction column, the eluate was separated by using C18 column (50 mm×4.6 mm, 1.8 μm) as stationary phase, and mixtures of 0.05% (φ) formic acid solution and acetonitrile (containg φ 0.05% formic acid) with different ratios was used as mobile phase in gradient elution. ESI+ and MRM were adopted in MS/MS determination. Linearity range of 3,3′dichlorobenzidine was found between 0.5-50 mg·kg-1 with detection limits (3S/N) of 0.15 mg·kg-1. Linearity ranges of the other 8 aromatic amines were found same between 0.2-50 mg·kg-1 with same detection limit (3S/N) of 0.05 mg·kg-1.Values of recovery found by standard addition method were in the range of 78.3%-103%, and values of RSD′s (n=6) less than 6.0%.