固相萃取-气相色谱-质谱法同时测定化妆品中多环芳烃和邻苯二甲酸酯类物质

doi:10.13218/j.cnki.csdc.2018.06.011

摘要/Abstract

摘要： 建立了固相萃取(SPE)-GC-MS法同时测定化妆品中的16种多环芳烃(PAHs)和17种邻苯二甲酸酯类(PAEs)的分析方法。样品经乙腈超声萃取后,经PSA/Slica玻璃柱净化,以Agilent Select PAH色谱柱分离,气相色谱-质谱法选择离子(SIM)监测测定。16种PAHs和17种PAEs在0.5~200 μg/L范围内线性良好,相关系数均大于0.99;PAHs方法检出限为0.6~1.0 μg/kg,方法定量限为1.9~3.3 μg/kg,阴性样品3个添加水平的平均回收率为86.4%~112.2%;PAEs方法检出限为0.4~2.3 μg/kg,方法定量限为1.5~7.6 μg/kg,阴性样品3个添加水平的平均回收率为82.2%~114.1%;相对标准偏差均小于10% (n=6)。

关键词: 化妆品, 多环芳烃, 邻苯二甲酸酯类, 固相萃取, 气相色谱-质谱法

Abstract: A sensitive method for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) and 17 phthalic acid esters (PAEs) in cosmetics by gas chromatography-mass spectrometry (GC-MS) coupled with solid-phase extraction (SPE) was established.Samples were ultrasonically extracted with acetonitrile,purified using PSA/Slica Glass SPE column,separated using Agilent Select PAH chromatographic column and detected by GC-MS with selected ion monitoring (SIM).Results indicate that the linear relationship of 16 PAHs and 17 PAEs in the range of 0.5-200 μg/L is good,with correlation coefficient greater than 0.99.The limits of detection and quantification of the method for PAHs are in the range of 0.6-1.0 and 1.9-3.3 μg/kg,respectively,the average recoveries of negative samples at three spiked levels are between 86.4% and 112.2%.The limits of detection and quantification of the method for PAEs are in the range of 0.4-2.3 and 1.5-7.6 μg/kg,respectively,the average recoveries of negative samples at three spiked levels are between 82.2% and 114.1%,and the relative standard deviation (RSD,n=6) is less than 10%.

Key words: cosmetics, polycyclic aromatic hydrocarbons, phthalic acid esters, solid-phase extraction, gas chromatography-mass spectrometry

中图分类号:

TQ658

张瑞瑞, 汪晨霞, 李秀英, 杜伟锋, 郭新东. 固相萃取-气相色谱-质谱法同时测定化妆品中多环芳烃和邻苯二甲酸酯类物质[J]. 日用化学工业, 2018, 48(6): 356-362.

ZHANG Rui-rui, WANG Chen-xia, LI Xiu-ying, DU Wei-feng, GUO Xin-dong. Simultaneous determination of polycyclic aromatic hydrocarbons and phthalic acid esters in cosmetics by GC-MS with solid-phase extraction[J]. China Surfactant Detergent & Cosmetics, 2018, 48(6): 356-362.

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