羧基膦酸改性氧化锆固定相的制备及其色谱性能

羧基膦酸改性氧化锆固定相的制备及其色谱性能 Preparation and Chromatographic Properties of the Dodecylamine N-Acetic Acid-N-Methylenephosphonic Acid Modified Zirconia Stationary Phase 姚礼峰 YAO Li-feng ~ 1 2 3 4 first-author 靳素荣 1 2 3 4 王志花 1 2 3 4 冯钰锜 1 2 3 4 达世禄 1 2 3 4 武汉大学化学与分子科学学院 武汉大学化学与分子科学学院 1,2),JIN Su-rong~2,WANG Zhi-hua~2,FENG Yu-qi~1,DA Shi-lu~1 1,2),JIN Su-rong~2,WANG Zhi-hua~2,FENG Yu-qi~1,DA Shi-lu~1 武汉理工大学理学院 武汉理工大学理学院 武汉大学化学与分子科学学院,湖北,武汉,430072 武汉大学化学与分子科学学院,湖北,武汉,430072 ,湖北,武汉,430070 ,湖北,武汉,430070 用十二胺-N-乙酸-N-亚甲基膦酸（DAPA）改性氧化锆制备了一种新的锆基质色谱固定相（DAPAZ）.研究发现,DAPA在氧化锆表面有两种结合方式:红外光谱中1 611 cm-1处的特征吸收表明羧基主要与胺基形成偶极离子,以羧酸根离子形式存在,大部分的DAPA分子通过膦酸基团与氧化锆结合;而与钼酸的显色反应则表明有少量DAPA以羧基与氧化锆结合.另外,对固定相的屏蔽效应、碱性条件（pH 9.5）下的稳定性等色谱性能的研究也证实这两种吸附方式同时存在,但以膦酸基结合为主. A new zirconia-based stationary phase（DAPAZ） was prepared by modified zirconia with dodecylamine-N-acetic acid-N-methylenephosphonic acid（DAPA）.The adsorption mode of DAPA on zirconia was studied in detail.The broad peak at 1 611 cm -1 in the FTIR spectra of DAPAZ indicated that the dissociated carboxylic group formed zwitterion with amine group of DAPA,and that most of the DAPA was adsorbed on zirconia with phosphonic group.However,the results of coloration reaction of DAPAZ with ammonium molybdate indicated that some DAPA were adsorbed on zirconia with carboxyl group.These adsorption modes were also supported by the chromatographic behaves and the stability test of the stationary phase at pH 9.5. 氧化锆 色谱固定相 十二胺-N-乙酸-N-亚甲基膦酸 zirconia stationary phase dodecylamine-N-acetic acid-N-methylenephosphonic acid O657.7 国家自然科学基金资助项目（20275029） 2005-06-01 2021-04-01 6