色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 890-896.DOI: 10.3724/SP.J.1123.2014.04008

• 技术与应用 • 上一篇    下一篇

气相色谱/质谱测定皮革及其制品中乙二醇醚类有机溶剂的残留量

王成云, 张伟亚, 李丽霞, 沈雅蕾, 林君峰, 谢堂堂, 褚乃清   

  1. 深圳出入境检验检疫局工业品检测技术中心, 广东 深圳 518067
  • 收稿日期:2014-04-03 修回日期:2014-07-03 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 王成云，E-mail：wangchengyun2009@126.com
  • 基金资助:

    国家质检总局科研项目（2011IK105）；国家认监委科研制标项目（2013B239k）.

Determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry

WANG Chengyun, ZHANG Weiya, LI Lixia, SHEN Yalei, LIN Junfeng, XIE Tangtang, CHU Naiqing   

  1. Testing and Technology Center for Industrial Products, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China
  • Received:2014-04-03 Revised:2014-07-03 Online:2014-08-08 Published:2014-08-01

PDF

371

被引次数

55

摘要：

建立了同时测定皮革及其制品中12种乙二醇醚类有机溶剂残留量的气相色谱/质谱-选择离子监测方法。以乙酸乙酯为萃取溶剂，在45℃下超声萃取皮革及其制品中的乙二醇醚类有机溶剂，萃取液经固相萃取柱净化后进行气相色谱/质谱-选择离子监测法测定，外标法定量。在信噪比（S/N）=3的条件下，乙二醇单乙醚（EGEE）的检出限为0.10 mg/kg，其余11种乙二醇醚类有机溶剂的检出限均小于0.05 mg/kg。在3个加标水平下，该方法的平均加标回收率为81.2%~95.5%，相对标准偏差（RSD）为1.4%~6.6%（n=9）。该方法简便快捷，灵敏度高，检出限远远低于欧盟法规《化学品的注册、评估、授权和限制》（REACH）的限量要求，适用于皮革及其制品中乙二醇醚类有机溶剂残留量的测定，为制定相关检测标准提供了参考。

关键词: 超声萃取, 皮革, 气相色谱/质谱, 选择离子监测, 乙二醇醚类化合物

Abstract:

An effective method was established for the simultaneous determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry. Glycol ethers in leather and leather products were ultrasonically extracted at 45℃, using ethyl acetate as the extraction solvent. The extracts were purified by solid phase extraction (SPE) columns, and then analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode. The content of each analyte was calibrated by external standard method. The limit of detection of ethylene glycol ethyl ether (EGEE) was 0.10 mg/kg under the condition of signal to noise (S/N) of 3 and the limits of the other 11 glycol ethers were all less than 0.05 mg/kg. The spiked recoveries varied from 81.2% to 95.5% at three different spiked levels with the relative standard deviations (RSDs) ranged from 1.4% to 6.6%. The proposed method is simple, rapid and accurate, with the limits of detection much less than the requirements of the Regulation Concerning Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) of European Union. It is applicable to the determination of residual glycol ethers in leather and leather products, and provides a reference for the relevant testing standards.

Key words: gas chromatography/mass spectrometry (GC/MS), glycol ethers, leather, selected ion monitoring (SIM), ultrasonic extraction

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