色谱

色谱 ›› 2012, Vol. 30 ›› Issue (11): 1178-1182.DOI: 10.3724/SP.J.1123.2012.07003

• 研究论文 • 上一篇    下一篇

气相色谱-负化学源-三重四极杆质谱法测定化妆品中的硝基麝香类化合物

王征*   

  1. 福建省产品质量检验研究院, 国家加工食品质量监督检验中心, 福建 福州 350002
  • 收稿日期:2012-07-02 修回日期:2012-08-16 出版日期:2012-11-28 发布日期:2012-11-21
  • 通讯作者: 王征,博士研究生,主要从事食品安全分析. Tel: (0591)83762000, E-mail: syymwan@sina.com.

Determination of synthetic nitro-musks in cosmetics by gas chromatography coupled with negative chemical ionization-triple quadrupole mass spectrometry

WANG Zheng*   

  1. Fujian Inspection and Research Institute for Product Quality, National Quality Supervision and Testing Center for Processed Food, Fuzhou 350002, China
  • Received:2012-07-02 Revised:2012-08-16 Online:2012-11-28 Published:2012-11-21

PDF

452

被引次数

11

摘要： 建立了一种用于不同化妆品中5种硝基麝香含量的气相色谱-负化学离子源三重四极杆质谱联用(GC-MS/MS)检测方法。采用丙酮/正己烷混合溶液超声提取化妆品中的硝基麝香,将提取液浓缩,以CNWBOND Si固相萃取柱净化。再由GC-MS/MS检测,氘代二甲苯麝香内标法定量。该方法对化妆品中5种硝基麝香的加标回收率为85.81%～103.77%,相对标准偏差(RSD)不大于5.32%,灵敏度高,定量限为50.0～500 ng/kg;选择性好,能有效消除复杂基体干扰。可作为常见化妆品中硝基麝香类化合物含量检测的确证方法。

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关键词: 负化学离子源三重四极杆质谱, 化妆品, 气相色谱, 硝基麝香

Abstract: A confirmatory method is presented for the determination of five nitro-musks (musk ambrette, musk xylene, musk moskene, musk tibeten and musk ketone) in different cosmetics by gas chromatography coupled with negative chemical ionization (NCI)-triple quadrupole mass spectrometry (GC-MS/MS). The samples were extracted under ultrasonication using a mixture of acetone and hexane. The extract was concentrated and then cleaned up by CNWBOND Si solid phase extraction cartridge. Five different instrument parameters such as the temperature programmed, ion source temperature, reagent gas pressure, collision energy, monitoring ion pairs were optimized for higher sensitivity. Then the analytes were qualitatively and quantitatively analyzed under the multiple reaction monitoring (MRM) mode after the chromatographic separation on an HP-5MS capillary column (30 m×0.25 mm, 0.25 μm), and employing d15-musk xylene as internal standard. The mixed standards were spiked in the blank cosmetics samples (each nitro-musk was about 500 ng/kg), and the recoveries were in the range of 85.81%~103.77% with the relative standard deviations (RSDs) not more than 5.32%. The limits of quantification of the method were about 50.0~500 ng/kg. The method is accurate, rapid, sensitive and can be used in the inspection of the five nitro-musks in cosmetics.

Key words: cosmetics, negative chemical ionization-triple quadrupole mass spectrometry, nitro-musks, gas chromatography (GC)