HIGH PERFORMANCE METAL CHELATE INTERACTION CHROMATOGRAPHY

一种可络合的二乙烯三胺功能固定相 开发了过渡金属离子，并对其在高效液相色谱中的使用进行了评估 分居。合成包括蒸发三甲氧基硅基丙基- 醋酸盐缓冲水溶液中的单体及其200℃衍生化 摄氏0.55度。可复制的表面覆盖率为3.0微克 在100埃，550米/克二氧化硅上得到摩尔/m平方。 用正面洗脱的方法在分析柱上负载了铜(II)、镍(II) 过程；突破体积与金属摄取量很好地对应 用原子吸收分光光度法测定。缓冲水溶液- 有机流动相用于磺胺的分离 抗菌药物，包括磺胺嘧啶、磺胺噻唑、磺胺美嗪 和磺胺吡啶。建立了一个经验保留率表达式。 与色层保留有关的：a)静电相互作用 带有阳离子固定相的酸性磺胺功能，b) 含杂环芳香化合物的二次金属-配体络合物 溶质的取代基和c)相对分子的增溶 流动相中的疏水溶质。保留率则相反 与有机改性剂和缓冲剂的浓度成正比 通常与洗脱液的pH值成正比。一种pH为7.3的洗脱液 磷酸盐缓冲液和50%甲醇可有效地减少静电 相互作用，同时允许基于金属-配体相互作用的保留。 这项工作是一篇博士论文的主题，题为《静电和 对磺胺类药物的金属相互作用色谱进行了辩护和分析 1991年4月30日接受待定的编辑修订。

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.