色谱 ›› 2011, Vol. 29 ›› Issue (12): 1179-1182.DOI: 10.3724/SP.J.1123.2011.01179

• 研究论文 • 上一篇    下一篇

顶空气相色谱-质谱联用法测定胶粘剂中的残余单体

刘丹1, 陈晓青1*, 吴名剑2, 李绍晔2, 戴云辉2   

  1. 1. 中南大学化学化工学院, 湖南 长沙 410083; 2. 湖南中烟工业有限责任公司技术中心, 湖南 长沙 410014
  • 收稿日期:2011-07-15 修回日期:2011-08-19 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 陈晓青,教授,主要研究方向为药物活性成分分离分析新技术. Tel: (0731)88830833

Determination of residual acrylate monomers in adhesives by headspace gas chromatography-mass spectrometry

LIU Dan1, CHEN Xiaoqing1*, WU Mingjian2, LI Shaoye2, DAI Yunhui2   

  1. 1. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China; 2. Technical Center of China Tobacco Hunan Industrial Co., Ltd., Changsha 410014, China
  • Received:2011-07-15 Revised:2011-08-19 Online:2011-12-28 Published:2012-01-15

摘要: 建立了一种测定胶黏剂中6种丙烯酸酯和甲基丙烯酸酯类残余单体的分析方法。样品经100 ℃、30 min顶空加热后,通过DB-WAX色谱柱(30 m×0.25 mm×0.25 μm)分离和质谱选择离子模式检测,内标法定量。结果表明,6种残余单体能达到良好的分离,检出限(信噪比为3)为0.069~0.096 mg/kg,定量限(信噪比为10)为0.23~0.32 mg/kg,平均回收率为96.0%~104.6%,相对标准偏差(RSD)小于7.2%。该方法操作简便、准确、重复性好、灵敏度高,可用于胶黏剂中丙烯酸酯和甲基丙烯酸酯类残余单体的快速测定。

关键词: 丙烯酸酯类残余单体, 顶空气相色谱-质谱联用法, 胶黏剂

Abstract: A method was developed for the determination of methyl acrylate, ethyl acrylate, butyl acrylate, methyl methacrylate, ethyl methacrylate and butyl methacrylate in adhesives by headspace gas chromatography-mass spectrometry (HS-GC-MS). The samples were treated at 100 ℃ for 30 min, then separated on a DB-WAX column (30 m×0.25 mm×0.25 μm) and determined by MS under selected ion monitoring mode and quantified by internal standard method. The established method showed good separation with the limits of detection (LODs, S/N=3) of 0.069~0.096 mg/kg and the limits of quantification (LOQs, S/N=10) of 0.23~0.32 mg/kg. The recoveries for acrylate monomers were in the range from 96.0% to 104.6% with the relative standard deviations less than 7.2%. The method is simple, accurate, rapid and highly sensitive. It can be applied to analyze the residual acrylates and methyl acrylates in adhesives.

Key words: residual acrylate monomers, adhesives, headspace gas chromatography-mass spectrometry (HS-GC-MS)