顶空固相微萃取-气相色谱-质谱联用测定香水中5种合成麝香  

Determination of five synthetic musks in perfume by headspace solid-phase microextraction and gas chromatography-mass spectrometry

作　　者：王冠男[1] 汤桦[2] 陈大舟[2] 冯洁[1] 李蕾[1] 

机构地区：[1]北京化工大学理学院,北京100029 [2]中国计量科学研究院,北京100013

出　　处：《色谱》2012年第2期135-140,共6页Chinese Journal of Chromatography

基　　金：科技部创新方法项目(2008IM021800)

摘　　要：建立了香水中5种合成麝香的顶空固相微萃取-气相色谱-质谱联用分析方法。实验选用65μm的聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)萃取纤维,在磁力搅拌600 r/min条件下,考察了萃取温度、平衡时间、萃取时间、解吸时间、进样口温度和盐效应6个方面对实验结果的影响。优化后的条件为:10 mL顶空瓶中加入适量用水稀释过的样品,于60℃平衡3 min后,顶空萃取20 min,随即插入气相色谱进样口,于250℃解吸3 min进行定性、定量分析。5种合成麝香在0.05～1.00μg/g范围内线性关系良好,检出限(LOD)为0.6～2.1 ng/g。空白样品在3个浓度加标水平下(0.05,0.50,1.00μg/g)的回收率为82.0%～103.3%,相对标准偏差(RSD)为1.8%～9.4%。本方法简便、准确、快速、灵敏,适用于香水中合成麝香的分析检验工作。A method for headspace solid-phase microextraction（HS-SPME）,followed by gas chromatography-mass spectrometry（GC-MS） analysis was established for the determination of five commonly used synthetic musks in perfume.Two polycyclic musks（celestolide and tonalide） and three nitro musks（musk ambrette,musk xylene and musk ketone） were used as analytes in the optimization of the analytical method.Six parameters,such as the extraction temperature,equilibrium time,extraction time,desorption time,injector temperature and solution of salting out,were optimized by exposing the 65 μm polydimethylsiloxane-divinylbenzene（PDMS-DVB） fiber to the headspace of magnetically stirred（600 r/min） sample.According to the results of the optimization experiments,the following conclusion can be drawn： The water-diluted sample in a 10 mL headspace-vial was efficiently extracted for 20 min after the system was equilibrated for 3 min at 60 ℃.After extraction,the fiber was immediately inserted into the GC injector and desorbed at 250 ℃ for 3 min.The spiked recoveries were in the range of 82.0%-103.3% and the relative standard deviations（RSDs） were between 1.8% and 9.4%.Meanwhile,the limits of detection（LODs） ranged from 0.6 ng/g to 2.1 ng/g.This method is characterized by rapidity,high sensitivity,good linearity and repeatability for all the target compounds.It is applicable to the analysis of synthetic musks in perfumes.

关 键 词：顶空固相微萃取 气相色谱-质谱联用 合成麝香 香水 

分 类 号：O658[理学—分析化学]