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首页> 外文学位 >Characterization and application of pseudostationary phases in micellar electrokinetic chromatography (MEKC).
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Characterization and application of pseudostationary phases in micellar electrokinetic chromatography (MEKC).

机译：胶束电动色谱（MEKC）中伪平稳相的表征和应用。

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摘要

Various micellar, mixed micellar and polymeric pseudostationary phases were evaluated using linear solvation energy relationships (LSER) and applied for the separation of various groups of pharmaceutically and environmentally relevant compounds in micellar electrokinetic chromatography (MEKC) and mixed micellar electrokinetic chromatography (MMEKC).; First, individual as well as mixtures of bile salt surfactants and/or sodium dodecyl sulfate (SDS) were employed to separate a group of seventeen structurally similar corticosteroids. Addition of SDS to the mixtures of bile salt micelles resulted in significant extension of the elution window and subsequently improvement in resolution. The separation of a complex mixture of seventeen corticosteroids was further improved by employing various bile salt and/or alkylsulphonate mixtures for use in MMEKC. Retention behavior of corticosteroids in SDS and bile salt micelles was examined using linear solvation energy relationships (LSER). The effects of alkylsulphonate carbon chain length and concentration on capacity factor, selectivity, efficiency, and the size of the elution window were investigated. LSER models were also used to investigate additional MEKC surfactant systems including mixed bile salt systems (e.g. sodium deoxycholate (SDC) and sodium cholate (SC)) and mixed SDS/bile salt systems (e.g. SDS/SC and SDS/SDC). It was found that the migration behavior of a group of 60 uncharged aromatic compounds is influenced primarily by their size and hydrogen bond acceptor strength in all systems investigated. Mixed bile salt systems also provided results differing from the two individual systems. In addition, LSER analysis was applied for the study of a mixed fluorocarbon (lithium perfluorooctane sulphonate (LiPFOS))/hydrocarbon (lithium dodecyl sulfate (LiDS)) surfactant system. Elution patterns of various solutes in mixed micellar systems were compared and rationalized through results of LSER analysis.; Second, an ionic tri-block co-polymer, poly(methyl methacrylate/ethyl acrylate/methacrylic acid) (Elvacite 2669) was used as a pseudostationary phase in MEKC. Highly hydrophobic compounds such as polycyclic aromatic hydrocarbons (PAH's) and fullerenes were separated using Elvacite 2669 as an MEKC pseudostationary phase along with high percentages of organic modifier. The effect of addition of methanol to Elvacite 2669 MEKC systems was studied using LSER models. It was found that retention in these polymeric/methanolic pseudostationary phases is primarily influenced by the size of the molecule and their hydrogen bond accepting basicity. LSER results obtained in Elvacite 2669/methanolic MEKC systems were compared to results obtained in C-18 reversed phase liquid chromatography (RPLC) systems using methanol/water mobile phases.
机译：使用线性溶剂化能量关系（LSER）评估了各种胶束，混合胶束和聚合物假平稳相，并用于胶束电动色谱（MEKC）和混合胶束电动色谱（MMEKC）中的各种药物和环境相关化合物的分离。首先，采用胆汁盐表面活性剂和/或十二烷基硫酸钠（SDS）的混合物以及它们的混合物来分离一组17种结构相似的皮质类固醇。将SDS添加到胆盐胶束混合物中可显着延长洗脱窗口并随后提高分离度。通过将各种胆盐和/或烷基磺酸盐混合物用于MMEKC，进一步改善了17种皮质类固醇的复杂混合物的分离。使用线性溶剂化能量关系（LSER）检查了皮质类固醇在SDS和胆汁盐胶束中的保留行为。研究了烷基磺酸碳链长度和浓度对容量因子，选择性，效率和洗脱窗口尺寸的影响。 LSER模型还用于研究其他MEKC表面活性剂系统，包括混合胆汁盐系统（例如脱氧胆酸钠（SDC）和胆酸钠（SC））和混合SDS /胆汁盐系统（例如SDS / SC和SDS / SDC）。发现在所有研究的系统中，一组60种不带电荷的芳族化合物的迁移行为主要受其尺寸和氢键受体强度的影响。混合胆汁盐系统还提供了不同于两个单独系统的结果。此外，LSER分析用于研究碳氟化合物（全氟辛烷磺酸锂（LiPFOS））/碳氢化合物（十二烷基硫酸锂（LiDS））混合表面活性剂系统。通过LSER分析的结果比较并合理化了混合胶束系统中各种溶质的洗脱模式。其次，将离子型三嵌段共聚物聚（甲基丙烯酸甲酯/丙烯酸乙酯/甲基丙烯酸）（Elvacite 2669）用作MEKC中的准平稳相。使用Elvacite 2669作为MEKC准平稳相和高百分比的有机改性剂，可以分离出高度疏水的化合物，例如多环芳烃（PAH's）和富勒烯。使用LSER模型研究了向Elvacite 2669 MEKC系统中添加甲醇的效果。发现在这些聚合物/甲醇假平稳相中的保留主要受分子大小及其氢键接受碱性的影响。将Elvacite 2669 /甲醇MEKC系统中获得的LSER结果与使用甲醇/水流动相的C-18反相液相色谱（RPLC）系统中获得的结果进行了比较。

著录项

  • 作者

    Bumgarner, Jefferson Gail.;

  • 作者单位

    North Carolina State University.;

  • 授予单位 North Carolina State University.;
  • 学科 Chemistry Analytical.
  • 学位 Ph.D.
  • 年度 1996
  • 页码 164 p.
  • 总页数 164
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
  • 关键词

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