顶空固相微萃取/气相色谱-质谱法测定液态化妆品中8种增塑剂  

Determination of 8 Phthalate Esters in Liquid Cosmetics Using Solid-phase Microextraction/Gas Chromatography-Mass Spectrometry

作　　者：张璇[1] 陈大舟[2] 汤桦[2] 冯洁[1] 庄惠明[3] 李蕾[1] 

机构地区：[1]北京化工大学理学院化学系,北京100029 [2]中国计量科学研究院化学计量与分析科学研究所,北京100013 [3]云南省计量测试技术研究院,云南昆明650228

出　　处：《分析测试学报》2012年第3期317-321,共5页Journal of Instrumental Analysis

基　　金：质检总局环境激素测量基标准研究(AHY0708)

摘　　要：建立了顶空固相微萃取(HS-SPME)/气相色谱-质谱(GC-MS)同时测定液态化妆品中8种邻苯二甲酸酯类增塑剂(PAEs)的分析方法,并对萃取涂层、萃取温度、搅拌速率、盐浓度等参数进行了优化。最终采用65μm聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)固相微萃取纤维头,调节待萃取液盐浓度为360 g.L-1,在搅拌速率600 r/min及萃取温度90℃条件下萃取60 min,在250℃进样口解吸4 min后供GC-MS分析。结果表明,该方法对除邻苯二甲酸二苯酯(DPhP)外的7种目标化合物的线性范围为10～2 000μg.kg-1,检出限为0.7～13.6μg.kg-1,回收率为83%～97%,相对标准偏差(RSD)为2.5%～10.0%;由于DPhP在萃取涂层上的保留较弱,其回收率为70%,检出限为75μg.kg-1,RSD为13.9%。该方法能很好地富集基体中的目标化合物,满足液态化妆品中多种PAEs的分析要求。A method based on solid-phase microextraction （SPME） technique followed by gas chroma- tography with mass spectrometry detector（ GC -MS） was developed for the determination of 8 phthalic acid esters （PAEs） in liquid cosmetics. The parameters affecting the partitions of analytes such as fi- ber coating, extraction temperature, stirring speed and salt concentration were optimized. The final SPME method employed a 65 μm polydimethylsiloxane （PDMS）/divinylbenzene （DVB） coating fiber and the saturated sodium chloride solution at 90 ℃ under stir for 60 min, then the fiber was intro- duced into the GC injector port and the extract was desorbed at 250 ℃ for 4 min. The detection limits for the other 7 PAEs except for DPhP ranged from 0.7 μg · kg-1 to 13.6 μg · kg^-1 , and the recover- ies for spiked samples were between 83% and 97% with RSDs （n = 5） of 2.5% - 10. 0% . For its weak adsorption to fiber coating, the detection limit for DPhP was 75 μg · kg^-1, and the recovery was 70% with RSD（n =5） of 13.9%. The method was applied in the determination of 8 PAEs in liquid samples with satisfactory results.

关 键 词：固相微萃取 气相色谱-质谱法 液态化妆品 邻苯二甲酸酯 增塑剂 

分 类 号：O657.63[理学—分析化学] TQ414[理学—化学]