冷冻去脂-液液分配净化/气相色谱-质谱法测定化妆品中16种多环芳烃

Determination of polycyclic aromatic hydrocarbons(PAHs) in cosmetic samples by freezing lipid filtration-liquid-liquid distribution cleanup and gas chromatography-mass spectrometry

建立了保湿护肤系列化妆品中16种多环芳烃的气相色谱-质谱测定法。对于水剂样品,采用环己烷提取、浓缩等简单前处理;对于膏霜剂样品,采用乙腈+丙酮(8+2,V/V)涡旋提取样品中的待测物,提取液经冷冻去脂、液液萃取净化(氨水-环己烷、水-环己烷),气相色谱-质谱法测定。16种多环芳烃在1～50μg/L均与对应峰面积呈良好线性关系。添加量在1～50μg/kg时,平均回收率(n=6)为78.1%～103.7%,相对标准偏差为2.4%～7.1%,方法检测限为1～10μg/kg。该法可用于化妆品中16种多环芳烃的测定。

A method for the determination of 16 polycyclic aromatic hydrocarbons（PAHs） in moisturizing and skin care cosmetic samples was established.Different pre-treatment methods were applied to different types of samples：for aqueous samples,which were extracted with cyclohexane,and concentrated to 1.0 mL by N2.For cream samples,which were extracted with acetonitrile＋acetone（8＋2,V/V）,and most of lipids in the extract were eliminated by freezing lipid filtration,then the extract was further purified with liquid-liquid distribution（ammonia-cyclohexane,water-cyclohexane）,followed by determination with GC-MS.Calibration curves of 16 PAHs were linear from 1 to 50 μg/L,with correlation coefficients of more than 0.99.Recoveries of the PAHs were in the range of 78.1%-103.7% with relative standard deviations of 2.4%-7.1% in a spiked concentration range of 1-50 μg/kg（n=6）,the method detection limits ranged from 1 to 10 μg/kg（S/N=3）.