HIGH PERFORMANCE METAL CHELATE INTERACTION CHROMATOGRAPHY

高效金属螯合物相互作用色谱

• 批准号: 3770469
• 负责人: A DEL GROSSO
• 金额: --
• 依托单位国家: 美国
• 资助国家: 美国
• 起止时间: 至
• 项目状态: 未结题
• 来源: https://reporter.nih.gov/project-details/3770469
• 关键词: analytical method; antiinfective agents; atomic absorption spectrometry; benzenesulfonamide; chelating agents; chemical synthesis; high performance liquid chromatography; metal complex; method development; sulfonamides

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 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 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.

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 醋酸盐缓冲水溶液中的三甲氧基硅丙基单体和 在200摄氏度和0.55托尔的衍生化。可复制表面 在100埃，550埃上获得了3.0微摩尔/m平方的覆盖率 M-平方/克二氧化硅。分析柱上负载了铜(II)、镍(II)和 锌(II)的前沿洗脱过程；穿透体积符合良好 用原子吸收分光光度法测定金属摄取量。 采用缓冲水-有机流动相分离 磺胺类抗菌剂，包括磺胺-二氮，磺胺-噻唑， 磺胺嘧啶和磺胺吡啶。经验保留率表达式为 发展了与色层保留相关的：a)静电 酸性磺胺官能团与阳离子固定剂的相互作用 相，b)涉及杂环的二次金属-配体络合物 溶质的芳香族取代基和c)增溶 流动相中相对疏水的溶质。被拘留的人 与有机改性剂和缓冲剂的浓度成反比 一般与洗脱液的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。