色谱

色谱 ›› 2014, Vol. 32 ›› Issue (12): 1295-1300.DOI: 10.3724/SP.J.1123.2014.09015

• 研究论文 • 上一篇    下一篇

基于七元瓜环多维配位聚合物的新型固相微萃取纤维的制备及对环境水样中多环芳烃的检测应用

颜丽芬1, 吕研1, 邵琳1, 周清娣2, 董南1   

  1. 1. 贵州大学化学与化工学院, 贵州 贵阳 550025;
    2. 悉尼大学化学院, 澳大利亚新南威尔士州 2006
  • 收稿日期:2014-09-10 修回日期:2014-10-13 出版日期:2014-12-08 发布日期:2014-11-28
  • 通讯作者: 董南,E-mail:scindong@163.com
  • 基金资助:

    国家自然科学基金项目(81160398);教育部春晖计划项目(Z2012062).

Preparation of new solid-phase microextraction fiber based on cucurbit[7]uril coordination polymers and its application in determination of polycyclic aromatic hydrocarbons from environmental water samples

YAN Lifen1, LÜ Yan1, SHAO Lin1, ZHOU Qingdi2, DONG Nan1   

  1. 1. College of Chemistry and Chemical Engineering, Guizhou University, Guiyang 550025, China;
    2. School of Chemistry, the University of Sydney, New South Wales 2006, Australia
  • Received:2014-09-10 Revised:2014-10-13 Online:2014-12-08 Published:2014-11-28

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219

被引次数

2

摘要：

以四氯化镉酸根离子[CdCl4]2-诱导形成的Eu3+-七元瓜环(Q[7]/Eu)多维配位聚合物为涂层材料,采用高温环氧树脂固定涂层制备了一种新型固相微萃取纤维。利用电镜和热重分析对纤维的表面形态和热稳定性进行了考察。实验结果表明该聚合物涂层表面疏松、多孔,热稳定性好。在优化的实验条件下(萃取温度75 ℃, NaCl质量浓度为200 g/L,萃取时间40 min, 250 ℃下解吸2 min)结合GC/FID的方法测定了水样中萘、苊、芴、菲、蒽、荧蒽、芘7种多环芳烃(PAHs)化合物。7种PAHs的线性范围为1~1000 μg/L,检出限在0.29~2.09 μg/L之间,相对标准偏差(RSD, n=5)不大于8.6%。将建立的方法用于实际样品花溪河水中PAHs加标回收率的测定,回收率在97.2%~109.0%之间,结果令人满意。在各自的最优萃取条件下,该涂层对7种PAHs的萃取效果与商品PDMS的萃取效果相当,证明该Q[7]/Eu多维配位聚合物在固相微萃取方面具有应用潜力。

关键词: 多环芳烃, 固相微萃取纤维, 瓜环多维配位聚合物, 环境水, 气相色谱

Abstract:

A novel solid-phase microextraction fiber was prepared via simple adhesion process. Fused-silica fiber was used as supporting substrate and the cucurbit[7]uril/Eu coordination polymers induced by [CdCl4]2- anion was affixed onto the surface of fused-silica fiber with high-temperature epoxy resin as a sorbent coating. The SPME coating was characterized by scanning electron microscopy and thermal analysis. Coupled to gas chromatography, the fiber was used to extract polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 75 ℃; mass concentration of NaCl, 200 g/L; extraction time, 40 min; desorption time, 2 min; desorption temperature, 250 ℃) compared with commercial fibers for the same analytes. For the seven PAHs (naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene and pyrene), good linearity was obtained ranging from 1 μg/L to 1000 μg/L. Limits of detection were 0.29-2.09 μg/L with the RSDs no more than 8.6%. The established SPME-GC method was applied to determine the spiked PAHs in real river water samples and satisfactory results were obtained with recoveries between 97.2% and 109.0%. Under the optimal conditions, the extraction effect of home-made coating was similar to the commercial PDMS (polydimethylsiloxane) coating, which further confirmed its potential in the solid-phase microextraction.

Key words: cucurbit[7]uril coordination polymers, environmental water, gas chromatography (GC), polycyclic aromatic hydrocarbons, solid-phase microextraction (SPME)

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