色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 34-39.DOI: 10.3724/SP.J.1123.2013.08005

• 研究论文 • 上一篇    下一篇

高效液相色谱-质谱法测定电子电气产品塑料部件中偶氮染料释放的致癌芳香胺

牛增元1, 罗忻1, 叶曦雯1, 王卉卉2, 李晶莹2   

  1. 1. 山东出入境检验检疫局检验检疫技术中心, 山东 青岛 266002;
    2. 青岛科技大学环境与安全工程学院, 山东 青岛 266042
  • 收稿日期:2013-08-01 修回日期:2013-09-20 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 牛增元
  • 基金资助:

    质检公益性行业科研专项(10-66)；国家质检总局科研项目计划(2011IK037)；国家认监委标准制修订项目(2011B265k).

Determination of carcinogenic aromatic amines derived from azo colorants in plastic components of electrical and electronic products by high performance liquid chromatography-mass spectrometry

NIU Zengyuan1, LUO Xin1, YE Xiwen1, WANG Huihui2, LI Jingying2   

  1. 1. Technical Center for Inspection and Quarantine of Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;
    2. College of Environment and Safety Engineering, Qingdao University of Science and Technology, Qingdao 266042, China
  • Received:2013-08-01 Revised:2013-09-20 Online:2014-01-08 Published:2013-12-26

PDF

365

被引次数

27

摘要：

采用高效液相色谱-质谱(HPLC-MS)法对电子电气产品塑料部件中偶氮染料还原裂解产生的21种芳香族伯胺进行同时测定。塑料用有机溶剂溶解或溶胀，释放其中存在的偶氮染料，在连二亚硫酸钠的强还原性环境中，偶氮染料被还原为芳香胺。用甲基叔丁基醚提取芳香胺，提取液浓缩后用甲醇-水(1：1，v/v)定容，HPLC-MS检测。采用ZORBAX Eclipse XDB C18色谱柱分离，乙腈和0.1%(v/v)甲酸溶液为流动相，流速0.6 mL/min，选择离子监测(SIM)采集数据，色谱峰保留时间和特征离子定性。21种芳香胺的线性关系良好，r >0.998，方法检出限为0.5 mg/kg。除个别物质外，在空白塑料基质中的加标回收率为60.1%~129.5%，相对标准偏差小于14.0%。本研究表明电子电气塑料部件中的禁用偶氮染料还原产生的芳香胺能够被定性定量测定，本方法的准确度高，精密度好。

关键词: 电子电气产品, 芳香胺, 高效液相色谱-质谱法, 偶氮染料, 塑料

Abstract:

A study for the simultaneous determination of 21 primary aromatic amines derived from the reduction of the azo colorants in plastic components of electrical and electronic products was conducted. Organic solvents were used to dissolve or swell the plastics to release the azo dyes existing in the plastic components. The azo colorants were reduced to aromatic amines under strong reducing condition of dithionite. Aromatic amines were extracted with methyl tert-butyl ether. Methanol-water (1:1, v/v) was used to concentrate the extract to constant-volume for HPLC-MS analysis. The analytes were separated on a ZORBAX Eclipse XDB C18 column using the gradient elution with acetonitrile and 0.1% (v/v) formic acid aqueous solution at a flow rate of 0.6 mL/min. The analyte confirmation was performed using retention time and characteristic ions in selected ion monitoring (SIM) mode. The correlation coefficients (r) of all the standard curves were more than 0.998, and the limits of quantification of the analytes were 0.5 mg/kg. The recoveries were 60.1%-129.5% for the 21 aromatic amines with the RSDs not more than 14.0% except for a few compounds. The results showed that the banned azo colorants in the plastic products can be analyzed qualitatively and quantitatively through reductive conversion into aromatic amines. In addition, this method has high accuracy and good precision.

Key words: aromatic amines, azo colorants, electrical and electronic products, high performance liquid chromatography-mass spectrometry (HPLC-MS), plastic

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