Silica gel chromatographic stationary phase bonded with CMBZ, its preparation method and application

By modifying the silica gel surface with a 5-chlorobenzimidazole-2-thiol structure, a multi-ligand heterocyclic silica gel chromatographic stationary phase was prepared, which solved the problem of insufficient selectivity for the separation of multiple types of compounds in the prior art, and achieved efficient separation and good peak shape control of flavonoids.

CN122399772APending Publication Date: 2026-07-17DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
Filing Date
2025-01-16
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing chromatographic stationary phases are insufficient to meet the separation requirements of various types of compounds in the extraction process of traditional Chinese medicine, especially flavonoids, which suffer from dead adsorption and poor selectivity. Reversed-phase chromatography has long separation time, and supercritical fluid chromatography has limited selectivity.

Method used

A silica gel chromatographic stationary phase with bonded multi-ligand heterocyclic structures was prepared. By modifying the silica gel surface with a 5-chlorobenzimidazole-2-thiol structure, various interactions such as polar interactions, hydrophobic interactions, π-π interactions, and hydrogen bonding interactions were provided to improve selectivity.

Benefits of technology

It achieves efficient separation of various types of compounds, especially flavonoids, with normal peak shapes and excellent selectivity. The separation process is simple, the conditions are mild, and it has good reproducibility and stability.

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Abstract

本发明提供一种键合CMBZ的硅胶色谱固定相及其制备方法和应用,属于色谱分离技术领域,硅胶色谱固定相的制备方法包括:溶解于甲苯中的3‑(2,3‑环氧丙氧)丙基三甲氧基硅烷与硅胶在30℃下反应,纯化后得到环氧中间体硅胶;环氧中间体硅胶加入溶解于DMF的5‑氯苯并咪唑‑2‑硫醇CMBZ中,纯化后获得键合CMBZ的硅胶色谱固定相。该硅胶色谱固定相用于对黄酮类化合物、苷类化合物、醛类化合物、酸类化合物、生物碱类化合物进行分离。本发明提供一种新型的改性硅胶,其配体基团为5‑氯苯并咪唑‑2‑硫醇,制备得到一种高效分离多种类型化合物的新型色谱固定相,在分离过程中可提供多种相互作用,选择性更加优异。
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