HIGH PERFORMANCE METAL CHELATE INTERACTION CHROMATOGRAPHY

一种二亚甲基三胺功能固定相， 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 0.55 ℃。3.0微米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。 分析柱通过前向色谱柱加载Cu（II）、Ni（II）和Zn（II）。 洗脱过程;穿透体积与金属吸收良好对应 通过原子吸收分光光度法测定。缓冲有机水溶液 移动的相用于分离磺酰胺类抗菌剂， 包括磺胺嘧啶、磺胺噻唑、磺胺美拉嗪和磺胺吡啶。 开发了一个经验保留表达式， 色谱保留：a）酸性的静电相互作用 磺酰胺官能团与阳离子固定相，B）仲 含杂环芳族取代基的金属-配体络合物 和c）溶解相对疏水的溶质 在移动的阶段。保留率与 浓度的有机改性剂和缓冲液，并通常直接 pH 7.3的磷酸盐缓冲液和50%的缓冲液的洗脱液。 甲醇有效地使静电相互作用最小化， 允许基于金属-配体相互作用的保留。

A diemethylenetriamine 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 micro- 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 sulfadiazine, 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.