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-单体，来自乙酸盐缓冲水溶液，和 在200 ℃和0.55 ℃下衍生化。 可再生曲面 在100埃，550埃，100埃 m2/g二氧化硅。 分析柱装载有Cu（II）、Ni（II）、Cu（II）和Ni（II）。 和Zn（II）的前沿洗脱过程;突破体积对应 用原子吸收测定金属吸收的孔 分光光度法 缓冲的水-有机移动的相用于 分离包括磺胺-二嗪在内的磺酰胺抗菌剂， 磺胺-噻唑、磺胺-美拉嗪和磺胺-吡啶。 实证 建立了相关色谱保留值表达式， 保留：a）酸性磺酰胺的静电相互作用 与阳离子固定相一起起作用，B）第二金属配体 涉及杂环芳族取代基的络合物 和c）相对疏水性溶质溶解在 移动的阶段。 保留率与 有机改性剂和缓冲液的浓度，并且通常 pH 7.3磷酸盐的洗脱液 缓冲液和50%甲醇是有效地减少静电 相互作用，同时允许基于金属配体的保留 交互. 这项工作是一个博士的主题。论文，题为 磺胺类药物的静电和金属作用色谱 在1991年6月被辩护并接受。 一份手稿， 这项研究正在进行中。

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 degrees C and 0.55 torr. Reproducible surface coverages of 3.0 micromoles/m-squared were obtained on 100-angstrom, 550 m-squared/g silica. Analytical columns were loaded with Cu(II), Ni(II) and Zn(II) by frontal elution process; breakthrough volumes corresponded well with metal uptake determined by atomic absorption spectrophotometry. Buffered aqueous-organic mobile phases were used for separations of sulfonamide antimicrobials that included sulfa-diazine, sulfa-thiazole, 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 in June, 1991. A manuscript based on this study is in progress.