色谱

色谱

• 研究论文 • 上一篇    下一篇

聚醚砜酮涂层纤维顶空固相微萃取-气相色谱法分析水中痕量的酚类化合物

姚桂燕,观文娜,许峰,王华,关亚风   

  1. Department of Instrumentation ＆ Analytical Chemistry, Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China
  • 收稿日期:2008-10-27 修回日期:2008-10-27 出版日期:2008-10-27 发布日期:1983-09-25
  • 通讯作者: 关亚风
  • 基金资助:
    国家自然科学基金项目(Nos. 20575068, 20635010).

Analysis of phenolic compounds in aqueous samples by gas chromatography coupled with headspace solid-phase microextraction using poly(phthalazine ether sulfone ketone) coated fiber

YAO Guiyan, GUAN Wenna, XU Feng, WANG Hua, GUAN Yafeng   

  1. Department of Instrumentation ＆ Analytical Chemistry, Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China
  • Received:2008-10-27 Revised:2008-10-27 Online:2008-10-27 Published:1983-09-25
  • Contact: GUAN Yafeng

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摘要： 应用自制的聚醚砜酮(PPESK,30 μm)涂层纤维，采用顶空固相微萃取-气相色谱法测定水中痕量的酚类化合物。优化了固相微萃取温度、萃取时间、pH值和离子强度。方法的检出限为0.003～0.041 μg/L,相对标准偏差低于16%(n=5)。将PPESK涂层纤维与商品化的聚丙烯酸酯涂层纤维对比,结果表明PPESK萃取酚类化合物有较高的萃取富集倍数。用所制备的PPESK萃取头分析自来水、海水等实际水样,20 μg/L添加水平下的回收率分别为100.5%～111.8%和94.8%～117.3%。

关键词: 顶空固相微萃取, 酚类化合物, 聚醚砜酮涂层纤维, 气相色谱, 水

Abstract: The direct trace analysis of phenolic compounds in aqueous samples was performed by headspace solid-phase microextraction/gas chromatography (HS-SPME/GC). A laboratory made poly(phthalazine ether sulfone ketone) (PPESK, 30 μm) coated fiber was used to extract the phenols from aqueous samples. The parameters affecting the extraction efficiency, such as extraction temperature and time, pH value, and salt concentration, were optimized. The low pH value and high salt concentration can increase the extraction efficiency of phenols. The limits of detection (LODs) were from 0.003 to 0.041 μg/L, which were within the range of EPA Method 604. The relative standard deviations (RSDs) were less than 16%. Compared with commercial polyacrylate (PA) fiber (85 μm), the PPESK fiber shows high affinity toward phenolic compounds, and therefore, high absolute recoveries. The phenols were detected with the recoveries of 100.5%-111.8% for a tap water sample and 94.8%-117.3% for a seawater sample at the spiked level of 20 μg/L.

Key words: aqueous samples , gas chromatography （GC）, headspace solid-phase microextraction （HS-SPME）, phenolic compounds, poly(phthalazine ether sulfone ketone) coated fiber