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 与原子吸收分光光度法测定的金属吸收良好。 缓冲的水-有机移动的相用于分离 磺胺类抗菌剂，包括磺胺嘧啶，磺胺噻唑， 磺胺美拉嗪和磺胺吡啶。 经验保留表达式为 开发了相关的色谱保留：a）静电 酸性磺酰胺官能团与阳离子 固定相，B）涉及以下的二级金属-配体络合： 溶质的杂环芳族取代基和c）增溶 在移动的相中相对疏水的溶质的浓度。 保留金 与有机改性剂的浓度成反比， 洗脱液的pH通常与洗脱液的pH成正比。 pH7.3的磷酸盐缓冲液和50%甲醇有效地减少了 静电相互作用，同时允许基于金属配体的保留 交互. 这项工作是一位博士的主题论文，题为 “磺胺类药物的静电和金属相互作用色谱法”， 于1991年6月通过并获得通过。 一份基于此的手稿 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 moles/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.