色谱

色谱 ›› 2019, Vol. 37 ›› Issue (12): 1275-1281.DOI: 10.3724/SP.J.1123.2019.05033

• 研究论文 • 上一篇    下一篇

(3,5-二甲基苯基氨基甲酸酯)衍生的纤维素手性固定相

谌学先, 张鹏, 何义娟, 徐文, 袁黎明   

  1. 云南师范大学, 能源与环境科学学院, 化学化工学院, 昆明 650500
  • 收稿日期:2019-05-21 出版日期:2019-12-08 发布日期:2020-12-11
  • 通讯作者: 袁黎明.E-mail:yuan_limingpd@126.com.
  • 基金资助:
    国家自然科学基金项目（91856123，21165022）.

Chiral stationary phases of cellulose derived using 3,5-dimethyl phenylcarbamate

CHEN Xuexian, ZHANG Peng, HE Yijuan, XU Wen, YUAN Liming   

  1. School of Energy and Environment Science, School of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650500, China
  • Received:2019-05-21 Online:2019-12-08 Published:2020-12-11
  • Supported by:
    National Natural Science Foundation of China (Nos. 91856123, 21165022).

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摘要： 纤维素三（3，5-二甲基苯基氨基甲酸酯）是液相色谱中使用最广泛的手性柱。该文详细地研究了不同程度衍生的纤维素（3，5-二甲基苯基氨基甲酸酯）以及不同硅胶（粗制硅胶、氨丙基粗制硅胶、精制硅胶、氨丙基精制硅胶、大孔硅胶、氨丙基大孔硅胶）作为支撑体对该柱手性分离能力的影响。自制了13根手性色谱柱，分别考察了其对16种外消旋体的拆分，分离结果显示：三取代纤维素柱 > 二取代纤维素柱 > 纤维素柱；精制硅胶和大孔硅胶优于粗制硅胶，大孔硅胶的柱压更低；硅胶的氨丙基化对手性选择性有一定的影响；这些手性柱之间具有一定的互补性，尤其是纤维素柱。该文有助于人们更深刻地理解和更好地把握高效液相色谱手性柱的制备。

关键词: 高效液相色谱, 纤维素, 硅胶, 纤维素(3,5-二甲基苯基氨基甲酸酯), 手性固定相

Abstract: Chiral columns based on cellulose tri(3,5-dimethyl phenylcarbamate) (CTDMPC) have been extensively used for enantioseparation by high-performance liquid chromatography (HPLC). The effects of cellulose derived using different amounts of 3,5-dimethyl phenylcarbamate and silica gels prepared by different methods on the chiral separation characteristics have been investigated. Thirteen chiral chromatographic columns were prepared, and their separation capability for sixteen racemate samples was evaluated. The efficiency of enantioselective resolution followed the order trisubstituted cellulose column > disubstituted cellulose column > cellulose column. Refine silica gel and macroporous silica gel showed better performance than did coarse silica gel. The use of macroporous silica gel resulted in low column pressure. Whether the silica gels were derived by aminopropyl could affect the enantioseparations. The thirteen chiral chromatographic columns were complementary for the separation of racemates, especially the cellulose column. This is a comparative study on the preparation of chiral stationary phases for HPLC, and the findings would enable us to design and fabricate chromatographic columns.

Key words: high performance liquid chromatography (HPLC), cellulose, silica gel, cellulose tri(3,5-dimethyl phenylcarbamate) (CTDMPC), chiral stationary phase

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