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日用化学工业:2018,Vol.>>Issue(6):356-362
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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
张瑞瑞,汪晨霞,李秀英,杜伟锋,郭新东
(广州检验检测认证集团有限公司,广东 广州 511447)
Simultaneous determination of polycyclic aromatic hydrocarbons and phthalate esters in cosmetics by GC-MS with solid-phase extraction
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中文摘要: 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)。
Abstract:A sensitive method for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) and 17 phthalate 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%, and the relative standard deviation (RSD, n=6) is less than 10%. 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%.
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