色谱

色谱 ›› 2012, Vol. 30 ›› Issue (02): 135-140.DOI: 10.3724/SP.J.1123.2011.10018

• 研究论文 • 上一篇    下一篇

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

王冠男1, 汤桦2, 陈大舟2, 冯洁1, 李蕾1*   

  1. 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
  • 收稿日期:2011-10-18 修回日期:2011-12-02 出版日期:2012-02-28 发布日期:2012-03-22
  • 通讯作者: 李蕾,教授,主要研究方向为无机材料和环境痕量分析化学. Tel: (010)64434903,
  • 基金资助:

    科技部创新方法项目(2008IM021800).

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

WANG Guannan1, TANG Hua2, CHEN Dazhou2, FENG Jie1, LI Lei1*   

  1. 1. College of Science, Beijing University of Chemical Technology, Beijing 100029, China; 2. National Institute of Metrology of P. R. China, Beijing 100013, China
  • Received:2011-10-18 Revised:2011-12-02 Online:2012-02-28 Published:2012-03-22

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503

被引次数

23

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65 μm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0.05～1.00 μg/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, 1.00 μg/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。

关键词: 顶空固相微萃取, 合成麝香, 气相色谱-质谱联用, 香水

Abstract: 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.

Key words: gas chromatography-mass spectrometry (GC-MS), perfume, synthetic musks, headspace solid-phase microextraction (HS-SPME)