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Synthesis of New Classes of Ionic Liquids and Polymeric Ionic Liquids and their Applications in Microextraction Techniques.

机译：新型离子液体和高分子离子液体的合成及其在微萃取技术中的应用。

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摘要

Ionic liquids (ILs) are nonmolecular solvents that consist of organic cations and organic/inorganic anions. The chemical and physical properties of ILs can be tuned conveniently by changing the combination of cations and anions or tailoring the structure of cations. Recently, ILs has emerged as a novel media for various microextraction techniques. Three different applications involving ILs and polymeric ionic liquids (PILs) in the extraction and quantification of different analytes will be discussed.;In the first application, the extraction of boric acid/borate from water was achieved using glucaminium-based ILs. The synthesis of glucaminium-based ILs will be discussed. 11B NMR was used as a tool to confirm the complexation between glucaminium ILs and boric acid/borate. The effect of glucaminium IL concentration and pH on complex formation was studied. The application of in situ dispersive liquid-liquid microextraction for boric acid/borate extraction from water was successfully demonstrated. A comprehensive binding study of the glucaminium IL-borate complex was also performed using 11B NMR. Regeneration of the glucaminium-based IL will be discussed.;The compound 2-aminopyrimidine-5-ylboronic acid (2-APYBA) may be present as an impurity in 2-aminopyrimidine-5-pinacolboronate ester (2-APPBE), a popular reagent used within the pharmaceutical industry in the Suzuki-Miyuara coupling reaction. The poor solubility of 2-APYBA in water and organic solvents poses a challenge for the separation and determination of 2-APYBA within the 2-APPBE reagent. This challenge was successfully addressed using two newly designed glucaminium-based ILs and separating the formed complex using reversed phase high performance liquid chromatography. The complexation between the two new glucaminium-based ILs and 2-APYBA was confirmed using 11B NMR. The effect of temperature and IL concentration on the complex was also studied. The method was successfully employed for the quantification of 2-APYBA in a real 2-APPBE sample used within the pharmaceutical industry.;Lastly, the use of PILs as sorbent coatings in solid-phase microextraction (SPME) for the analysis of polychlorinated biphenyls (PCBs) present in water and bovine milk will be discussed. The effect of different parameters such as extraction temperature, extraction time and salt concentration on the extraction of PCBs was studied. The analytical performance of the PIL-based SPME fibers was compared to the commercial polydimethylsiloxane (PDMS) fiber. A side-by-side comparison of detection limits was carried out using gas chromatography employing two detectors, namely, electron capture and mass spectrometry. The applicability of the PIL-based SPME method was evaluated in the analysis of two real sample matrixes, namely, ocean water and bovine milk.
机译：离子液体（ILs）是由有机阳离子和有机/无机阴离子组成的非分子溶剂。通过改变阳离子和阴离子的组合或调整阳离子的结构，可以方便地调节IL的化学和物理性质。最近，白介素已成为各种微萃取技术的新型培养基。将讨论在不同分析物的提取和定量中涉及IL和聚合离子液体（PIL）的三种不同应用。在第一个应用中，使用基于葡糖胺的IL从水中提取硼酸/硼酸盐。将讨论基于葡糖铵的IL的合成。 11B NMR被用作确认葡糖胺ILs与硼酸/硼酸盐之间络合的工具。研究了葡萄糖胺IL浓度和pH对复合物形成的影响。成功地证明了原位分散液-液微萃取技术从水中提取硼酸/硼酸盐的应用。还使用11B NMR对葡糖胺IL-硼酸盐复合物进行了全面的结合研究。将讨论基于葡糖铵的IL的再生。化合物2-氨基嘧啶-5-基硼酸（2-APYBA）可能以杂质形式存在于2-氨基嘧啶-5-频哪醇硼酸酯（2-APPBE）中Suzuki-Miyuara偶联反应中制药工业中使用的试剂。 2-APYBA在水和有机溶剂中的不良溶解度对2-APPBE试剂中2-APYBA的分离和测定提出了挑战。使用两个新设计的基于葡萄糖ami的ILs并使用反相高效液相色谱分离形成的复合物，成功解决了这一难题。使用11B NMR证实了两种新的基于葡糖胺的IL与2-APYBA的络合。还研究了温度和IL浓度对复合物的影响。该方法已成功用于制药行业中使用的实际2-APPBE样品中的2-APYBA定量分析;最后，在固相微萃取（SPME）中将PIL用作吸附剂涂层用于分析多氯联苯（将讨论水和牛乳中存在的多氯联苯。研究了提取温度，提取时间和盐浓度等不同参数对多氯联苯提取的影响。将基于PIL的SPME纤维与商用聚二甲基硅氧烷（PDMS）纤维的分析性能进行了比较。使用两个检测器的气相色谱法，即电子捕获和质谱法，对检测限进行了并排比较。基于PIL的SPME方法在分析两种真实样品基质（即海水和牛乳）中的适用性得到了评估。

著录项

  • 作者

    Joshi, Manishkumar Dilipkumar.;

  • 作者单位

    The University of Toledo.;

  • 授予单位 The University of Toledo.;
  • 学科 Analytical chemistry.;Organic chemistry.
  • 学位 Ph.D.
  • 年度 2013
  • 页码 187 p.
  • 总页数 187
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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