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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (17): 1749-1757. 上一篇    下一篇

研究论文

新型溶胶-凝胶离子液体固相微萃取探头的研制

周欣1，尚佳1，刘名茗*,1，刘汉兰2，郝蓉1，冯雄汉1，刘凡1   

  1. (1华中农业大学资源与环境学院 武汉 430070)
    (2华中农业大学理学院 武汉 430070)
  • 投稿日期:2009-12-25 修回日期:2010-03-24 发布日期:2010-05-11
  • 通讯作者: 刘名茗 E-mail:liumm@mail.hzau.edu.cn
  • 基金资助:

    国家自然科学基金项目;教育部博士点专向基金新教师基金;华中农业大学科研启动基金;华中农业大学大学生科技创新基金

Preparation of Novel Ionic Liquids-Based Sol-Gel Coatings for Solid-Phase Microextraction

Zhou Xin1 Shang Jia1 Liu Mingming*,1 Liu Hanlan2 Hao Rong1 Feng Xionghan1 Liu Fan1   

  1. (1 College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070)
    (2 College of Science, Huazhong Agricultural University, Wuhan 430070)
  • Received:2009-12-25 Revised:2010-03-24 Published:2010-05-11
  • Contact: Liu MingMing E-mail:liumm@mail.hzau.edu.cn
  • Supported by:

    ;the Specialized Research Fund for the Doctoral Program of Higher Education of China;the Scientific Research Starting Foundation for the introduced talents of Huazhong Agricultural University;the Students Research Fund of Huazhong Agricultural University

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被引次数

11 | 1

以1-羟乙基-3-甲基咪唑四氟硼酸(HEMIM[BF4])和1-羟乙基-3-甲基咪唑双三氟甲磺酰亚胺(HEMIM- [N(SO2CF3)2])离子液体为涂层材料, 采用溶胶-凝胶方法制备了两种新型的离子液体-羟基硅油(OH-TSO)复合涂层固相微萃取探头, 并对溶胶-凝胶反应机理和涂层性能进行了考察. 由于阴离子结构不同, 两种离子液体-OH-TSO复合涂层的性能也存在一定差异. 首先, 从表面形貌来看, HEMIM[BF4]-OH-TSO涂层表面孔洞排列更整齐, 孔径更小, 且大小均一. 从热重分析结果来看, HEMIM[N(SO2CF3)2]-OH-TSO涂层具有更高的热稳定性, 最高使用温度可以达到360 ℃. 从萃取性能来看, HEMIM[BF4]-OH-TSO涂层对大多数酚类环境雌激素和芳胺的萃取效果明显高于HEMIM[N- (SO2CF3)2]-OH-TSO和未加离子液体的OH-TSO涂层. 除此之外, 它们还具有较强的抗溶剂冲洗能力, pH应用范围广, 重现性好. 以HEMIM[N(SO2CF3)2]-OH-TSO涂层为萃取头, 采用固相微萃取-气相色谱法测定了实际水体中的芳胺. 结果表明, 该方法检测限低(6.3～201.3 ng/L), 线性范围宽(3～4个数量级), 重现性好(RSD＜7%), 准确度高(回收率87.4%～111.5%).

关键词: 离子液体, 固相微萃取, 溶胶-凝胶, 酚类环境雌激素, 芳胺

Two hydroxylethyl-functionalized ionic liquids (ILs), 1-(2 -hydroxylethyl)-3-methylimidazolium tetrafluoroborate (HEMIM[BF4]) and 1-(2 -hydroxylethyl)-3-methylimidazolium bis-(trifluoromethanesulfonyl)imide (HEMIM[N(SO2CF3)2]) were first used as selective stationary phase to prepare ILs-hy- droxyl-terminated silicone oil (OH-TSO) hybrid organic-inorganic coatings for solid-phase microextraction (SPME) by sol-gel technology. The underlying mechanism of the sol-gel reaction was proposed and the successful binding of ILs to the sol-gel substrate was confirmed by FT-IR spectra. The performance of these two ILs-based coatings was somewhat different, depending on the type of anions in ILs structure. Firstly, in contrast to HEMIM[N(SO2CF3)2]-OH-TSO coating, the pores on the surface of HEMIM[BF4]-OH-TSO coating are arranged more orderly and uniformly with a smaller size. Secondly, the HEMIM- [N(SO2CF3)2]-based fibers had much higher thermal stability compared with the HEMIM[BF4]-based fibers. Thirdly, the extraction efficiency of HEMIM[BF4]-OH-TSO fiber towards phenolic environmental estrogens and aromatic amines was superior to that of HEMIM[N(SO2CF3)2]-OH-TSO fiber, and OH-TSO fiber without ILs. Moreover, these ILs-based SPME fibers had wonderful solvent resistance, wide useable pH range and good coating preparation reproducibility. Efficient analysis of aromatic amines with headspace SPME-GC was achieved using sol-gel-derived HEMIM[N(SO2CF3)2]-OH-TSO fiber. The method showed linear response over three to four orders of magnitude. The limits of detection were very low, ranged between 6.3 and 201.3 ng/L. The relative standard deviation values were below 7% and the recovery varied from 87.4% to 111.5%.

Key words: ionic liquids, solid-phase microextraction, sol-gel, phenolic environmental estrogens, aromatic amines