HIGH PERFORMANCE METAL CHELATE INTERACTION CHROMATOGRAPHY

一种可络合的二亚甲基三胺功能固定相 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 摄氏度和0.55托。可复制的表面覆盖率为3.0微米 在100埃、550米平方/克二氧化硅上得到摩尔/m平方。 分析柱正面负载铜(II)、镍(II)和锌(II) 洗脱过程；穿透体积与金属摄取很好地对应 用原子吸收分光光度法测定。缓冲水-有机 流动相用于磺胺类抗菌剂的分离 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，该公式与 色谱保留：a)酸性物质的静电相互作用 磺胺功能与阳离子固定相，b)二次 含杂环芳香取代基的金属-配体络合物 以及c)相对疏水的溶质的增溶作用 在移动阶段。保留率与 有机改性剂和缓冲剂的浓度一般直接 与洗脱液的pH值成正比。PH 7.3磷酸盐缓冲液50%的洗脱液 甲醇有效地减少了静电相互作用，而 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.