高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (7): 1254.

• 研究简报 • 上一篇    下一篇

杯[8]芳烃键合硅胶固定相的制备、表征及色谱性能

刘敏, 达世禄, 冯钰锜, 李来生   

  1. 武汉大学化学与分子科学学院, 武汉 430072
  • 收稿日期:2003-05-12 出版日期:2004-07-24 发布日期:2004-07-24
  • 通讯作者: 达世禄(1939年出生),男,教授,博士生导师,从事分离材料和微分离分析研究.E-mail:dashilu@public.wh.hb.cn E-mail:dashilu@public.wh.hb.cn
  • 基金资助:

    国家自然科学基金(批准号:20275029);教育部博士学科点基金(批准号:200048601)资助

Preparation, Characterization and Chromatographic Performance of p-t-Butyl-calix[8]arene Bonded Silica Stationary Phase

LIU Min, DA Shi-Lu, FENG Yu-Qi, LI Lai-Sheng   

  1. College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2003-05-12 Online:2004-07-24 Published:2004-07-24

摘要: 杯芳烃通过疏水Π-Π、氢键和静电等作用能与中性分子及离子形成包合物,在离子选择性电极、催化、分离和酶模拟等领域受到关注.已报道的杯芳烃键合固定相的制备方法[1~3]都是先合成含杯芳烃硅烷化试剂,然后通过硅胶硅烷化反应制备键合固定相.其制备路线反应过程长,各种有机中间体纯化操作复杂.前文[4]曾以氯丙基键合硅胶为中间体,通过固相连续反应制备了氮杂冠醚键合硅胶固定相.本文采用固相连续反应制备了一种新型的对-叔丁基杯[8]芳烃键合固定相,通过元素分析、红外光谱等手段获得键合相分子结构信息,以多环芳烃和二取代苯位置异构体为溶质,对固定相的色谱性能及保留机理进行了研究.

关键词: 固相连续反应, 对-叔丁基杯[8]芳烃键合硅胶固定相, 高效液相色谱

Abstract: p-t-Butyl-calixarene bonded silica stationary phase(CBS) for high performance liquid chromatography was prepared via condensation reaction on the surface of solid .The stationary phase was characterized by means of elemental analysis and FTIR. The chromatographic performance of CBS was studied by using disubstituted benzenes as the solutes and methanol-water or methanol-buffer as the mobile phases, and compared with that obtained on CPS and ODS. The results show that the chromrtographic process can proceed in various retention mechanism, such as π-π, hydrogen-bonding, charge-transfer and inclusion complexation, besides hydrophobic interaction.

Key words: Continuous reaction on the surface of solid, p-t-Butyl-calix[8]arene bonded silica stationary phase, HPLC

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