HIGH PERFORMANCE METAL CHELATE INTERACTION CHROMATOGRAPHY

一种二亚乙基三胺功能固定相， 过渡金属离子，开发和评价用于HPLC 分居 合成涉及蒸发三甲氧基甲硅烷基丙基- 从乙酸盐缓冲水溶液中分离单体，并在200 ℃下衍生化 摄氏0.55度。 3.0微克的可再现表面覆盖率 在100埃、550平方米/克二氧化硅上获得摩尔/平方米。 分析柱通过前沿洗脱负载Cu（II）、Ni（II 过程;穿透体积与金属吸收量对应良好 通过原子吸收分光光度法测定。 缓冲水溶液- 采用有机流动相分离磺胺类药物 包括磺胺嘧啶、磺胺噻唑、磺胺美拉嗪在内的抗菌剂 和磺胺吡啶。 开发了一个经验保留表达式， 相关的色谱保留：a）静电相互作用的 酸性磺酰胺官能团与阳离子固定相，B） 涉及杂环芳族的二级金属-配体络合物 溶质的取代基，和c）相对的 在移动的相中的疏水溶质。 保留率与 与有机改性剂和缓冲液的浓度成比例， 通常与洗脱液pH成正比。pH 7.3的洗脱液 磷酸盐缓冲液和50%甲醇是有效地减少静电 同时允许基于金属-配体相互作用的保留。 这项工作是博士论文的主题，题为“静电和 磺胺类药物的金属相互作用色谱法”， 1991年4月30日接受编辑修订。

A diethylenetriamine functional stationary phase, capable of complexing transition metal ions, was developed and evaluated for use in HPLC separations. Synthesis involved evaporation of the trimethoxysilylpropyl- monomer from acetate buffered aqueous solution and derivatization at 200 degree C 0.55 torr. Reproducible surface coverages of 3.0 microgram moles/m-squared were obtained on 100-angstrom, 550 m-squared/g silica. Analytical columns were loaded with Cu(II), Ni(II) by frontal elution process; breakthrough volumes corresponded well with metal uptake determined by atomic absorption spectrophotometry. Buffered aqueous- organic mobil phases were used for separations of sulfonamide antimicrobials that included sulfa-diazine, sulfathiazole, sulfa-merazine and sulfa-pyridine. An empirical retention expression was developed that related chromatographic retention to: a)electrostatic interaction of the acidic sulfonamide function with the cationic stationary phase, b) secondary metal-ligand complexations involving the heterocyclic aromatic substituents of the solutes and c) solubilization of the relatively hydrophobic solutes in the mobile phase. Retentions were inversely proportional to concentrations of organic modifier and buffer and were generally directly proportional to eluent pH. An eluent of pH 7.3 phosphate buffer and 50% methanol was effective in minimizing electrostatic interactions while allowing retention based on metal-ligand interactions. This work was the topic of a Ph.D dissertation, entitled "Electrostatic and Metal Interaction Chromatography of Sulfonamides" that was defended and accepted pending editorial revisions on April 30, 1991.