高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (9): 1684.

• 研究论文 • 上一篇    下一篇

新型酯型反相高效液相色谱填料的制备、表征及性能评价

黄晓佳, 刘学良, 王俊德, 丛润滋   

  1. 中国科学院大连化学物理研究所, 大连 116012
  • 收稿日期:2001-05-22 出版日期:2002-09-24 发布日期:2002-09-24
  • 通讯作者: 王俊德(1942年出生),男,研究员,博士生导师,主要从事色谱和医学分离材料研究.E-mail:wjd@dicp.ac.cn E-mail:wjd@dicp.ac.cn
  • 基金资助:

    中国分析测试协会科学仪器发展基金(1999年)资助

Synthesis, Characterization and Evaluation of a Novel Ester-bonded for Reversed-phase HPLC

HUANG Xiao-Jia, LIU Xue-Liang, WANG Jun-De, CONG Run-Zi   

  1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116012, China
  • Received:2001-05-22 Online:2002-09-24 Published:2002-09-24

PDF (PC)

被引次数

28

摘要： 将一种新型硅烷偶联剂β-(3,4-环氧环己基)乙基三甲氧基硅烷(β-ECTS)与辛酸反应,然后再键合到硅胶上,得到了酯型键合固定相.用元素分析、13C固体核磁共振谱、红外光谱进行了表征.以甲醇和水为二元流动相,用包括碱性、酸性和中性有机化合物在内的混合物评价了该固定相的疏水性、选择性和亲硅醇基效应,并考察了该填料适用的pH范围及水解稳定性.结果表明,该固定相具有较好的色谱性能,且在pH=2.5～7.5之间稳定性良好,可有效地用于碱性化合物的分析分离.

关键词: 硅烷偶联剂, 酯型键合固定相, 反相液相色谱, 键合相

Abstract: Anovel ester bonded packing for reversed phase HPLC(RP HPLC) was synthesized by reacting octanoic acid with β (3,4 epoxycyclohexyl) ethyltrimethoxy silane and then the intermediate product was coupled onto porous silica. Characterization of the prepared packing was carried out with elemental analysis, solid state 13 C NMR, and Fourier transform infrared spectrometry. Hydrophobicity, selectivity and silanophilic activity of the packing were evaluated by using organic components including acidic, basic and neutral analytes as probe molecules and methanol water as binary mobile phase. The usage ranges of pHand stability of the packing were also evaluated. The results show that the novel stationary phase has excellent chromatographic properties and resist to hydrolysis between pH=2.5-7.5, it can be used for the separation of basic solutes efficiently.

Key words: Silane coupling agent, High performance liquid chromatography, Reversed phase packing, Ester bonded stationary phase

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