色谱

色谱 ›› 2014, Vol. 32 ›› Issue (10): 1152-1156.DOI: 10.3724/SP.J.1123.2014.08011

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱-质谱法测定皮革制品中短链氯化石蜡

张伟亚1, 万昕2, 李丽霞1, 王成云1, 金淑培2, 邢钧2   

  1. 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;
    2. 生物医学分析化学教育部重点实验室, 武汉大学化学与分子科学学院, 湖北 武汉 430072
  • 收稿日期:2014-08-13 出版日期:2014-10-08 发布日期:2014-09-29
  • 通讯作者: 邢钧，E-mail：gc-ms@263.net
  • 基金资助:

    国家质检总局科技计划项目（2011IK105）.

Determination of short chain chlorinated paraffins in leather products by solid phase extraction coupled with gas chromatography-mass spectrometry

ZHANG Weiya1, WAN Xin2, LI Lixia1, WANG Chengyun1, JIN Shupei2, XING Jun2   

  1. 1. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China;
    2. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2014-08-13 Online:2014-10-08 Published:2014-09-29

PDF

334

被引次数

9

摘要：

短链氯化石蜡（SCCPs）是我国皮革加脂过程中常用的添加剂，但近年已被欧盟等列为禁止使用的持久性有机污染物。由于SCCPs结构复杂，且皮革基质干扰严重，目前尚没有完善的皮革制品中SCCPs的标准检测方法。本文采用硅胶为固相萃取柱萃取，以正己烷-二氯甲烷（2:1，v/v）为洗脱剂，使SCCPs与皮革基质中的干扰组分完全分离，建立了用于测定皮革制品中SCCPs的固相萃取-气相色谱-质谱方法。该方法的回收率为90.47%~99.00%，检出限为0.069~0.110 mg/kg，相对标准偏差（RSD）为4.20%~6.69%。该方法适用于皮革中SCCPs的定性、定量分析。

关键词: 短链氯化石蜡（SCCPs）, 固相萃取, 皮革制品, 气相色谱-质谱法（GC-MS）

Abstract:

The short chain chlorinated paraffins (SCCPs) are the additives frequently used in the leather production in China, but they have been put into the list of forbidden chemicals issued by European Union recently. In fact, there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thoroughly separated from the analyte of the SCCPs on a home-made solid phase extraction (SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chloride (2:1, v/v). With this method, the recoveries for the SCCPs spiked in the real leather samples varied from 90.47% to 99.00% with the relative standard deviations (RSDs) less than 6.7%, and the limits of detection (LODs) were between 0.069 and 0.110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.

Key words: gas chromatography-mass spectrometry (GC-MS), leather products, short chain chlorinated paraffins (SCCPs), solid phase extraction (SPE)

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