色谱 ›› 2019, Vol. 37 ›› Issue (2): 143-148.DOI: 10.3724/SP.J.1123.2018.09020

• 研究论文 • 上一篇    下一篇

一种新型极性脲丙基-C30固定相的制备和性能评价

卫敏, 金小青, 赵岳星   

  1. 浙江师范大学化学与生命科学学院, 浙江 金华 321004
  • 收稿日期:2018-09-13 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 赵岳星,E-mail:eugenezhao@zjnu.cn

Preparation and performance evaluation of a novel polar urea-propyl-C30 stationary phase

WEI Min, JIN Xiaoqing, ZHAO Yuexing   

  1. Academy of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004, China
  • Received:2018-09-13 Online:2019-02-09 Published:2014-12-31

摘要:

以3-脲丙基三甲氧基硅烷为偶联剂,制备了一种新型极性脲丙基-C30(TPU-C30)反相色谱固定相。采用扫描电子显微镜、元素分析、红外光谱和热分析等对该固定相进行表征。结果表明,TPU-C30固定相已成功制备,连续制备3次固定相,其元素含量的相对偏差均小于5%,说明该合成工艺重复性良好。以不同极性、位置异构、碱性化合物为溶质探针,以传统的C18色谱柱与C30色谱柱为参比,对制备的固定相的色谱性能进行了研究。研究结果表明,TPU-C30固定相具有不同于传统C18柱、C30柱的选择性和更优的择形性,明显改善了碱性物质的峰形,其具有广阔的应用空间。

关键词: 高效液相色谱, 极性脲丙基-C30固定相, 极性嵌入, 择形性, 制备

Abstract:

A novel polar urea-propyl-C30 (TPU-C30) reversed stationary phase was prepared by using 3-ureidopropyltrimethoxysilane as a coupling agent. The characteristics of TPU-C30 were analyzed by scanning electron microscopy, elemental analysis, infrared spectroscopy and thermal analysis. The results showed that the TPU-C30 stationary phase was successfully prepared. Furthermore, the relative deviations of the element contents of TPU-C30 were within 5% (n=3), which indicated that the proposed synthesis had good repeatability. The chromatographic performances in the stationary phase were evaluated by using different polar compounds, positional isomers and basic compounds as solute probes. Compared to the conventional C18 and C30 columns, the TPU-C30 stationary phase had different selectivity and better shape selection. The TPU-C30 stationary phase can be applied in various fields.

Key words: high performance liquid chromatography (HPLC), polar embedding, polar urea-propyl-C30 (TPU-C30) stationary phase, preparation, shape selection

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