Preparation method of chiral ligand exchange chromatographic stationary phase

A technology of exchange chromatography and chiral ligands, which is applied in the field of preparation of chiral ligand exchange chromatography stationary phases, can solve the problems of long analysis time, complicated operation, long time required, etc., and achieves wide application range and short analysis time. , the effect of a large amount of bonding

Inactive Publication Date: 2004-10-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Chinese patent application (application number 99117305.8) discloses a chiral ligand exchange chromatography stationary phase and a preparation method thereof, specifically using L-phenylalanine as a raw material to prepare a new type of chiral selector 2-(2 -Hydroxy-3-alkoxy) propyl group-(S)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid, which is then coated on the bonded stationary phase of reversed-phase chromatography; It can realize the direct separation of amino acid samples; its disadvantages are: the separation takes a long time, and the tailing of the effluent components is serious; compared with the bonded stationary phase, the coated stationary phase is easy to lose, limit its useful life
Synthesis of two kinds of L-proline silica gel bonded chiral ligand exchange stationary phases with different bonding amounts (Zhu Xinyi, Han Xiaoqian et al. "Chromatography", 2002, 20(3): 223-226), using ligand exchange Chromatography separates a series of amino acids, and the result...

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  • Preparation method of chiral ligand exchange chromatographic stationary phase
  • Preparation method of chiral ligand exchange chromatographic stationary phase
  • Preparation method of chiral ligand exchange chromatographic stationary phase

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Embodiment 1

[0029] Preparation of chiral ligand exchange chromatography stationary phase with L-isoleucine as chiral selector:

[0030] Kromasil spherical silica gel: Sweden Eka Nobel company, particle size 5μm, specific surface 340m 2 / g, pore size 10nm; L-isoleucine: purchased from Sigma (USA)

[0031] Take 4.0g of acid-treated silicon spheres, dry them in vacuum at 150°C for 4-6 hours, cool them down, place them in a 250mL round-bottomed three-necked flask, add 2mL of 3-glycidylpropyltrimethoxysilane and 40ml of toluene, and put them in Stir and reflux at 110°C for 6-7 hours, cool, filter, wash several times with toluene, methanol, and acetone in sequence, and dry in vacuum at 50°C for 2 hours to obtain 3-glycidylpropyl silica gel;

[0032] Take 3.93g L-isoleucine, add a considerable amount of sodium carbonate (for example: 0.03mol isoleucine is treated with 0.015mol sodium carbonate) and an appropriate amount of water, stir to dissolve, evaporate to nearly dryness, add 40ml methanol,...

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Abstract

A process for using L-isoleucine as the chiral selective agent to prepare the stationary phase for chiral ligand displacement chromatography is disclosed. Its advantages are simple operation (directly splitting the chiral substance in simple experimental condition), high analysis speed, and wide application range.

Description

technical field [0001] The invention relates to the separation of amino acid enantiomers, in particular to a preparation method of a chiral ligand exchange chromatographic stationary phase. Background technique [0002] The separation of amino acid enantiomers can be done by gas chromatography and liquid chromatography, but usually requires pre-column sample derivatization. The derivatization process is not only time-consuming and troublesome, but also may cause racemization of the analyte, thereby affecting the analysis effect . Chiral Ligand Exchange Chromatography (CLEC), developed by Davankov et al. in the early 1970s, is an effective method for separating chiral compounds, especially amino acids and hydroxyacid enantiomers, with high selectivity, No pre-column derivatization is required. [0003] The coating and preparation of bonded phases using photoactive amino acids or pipecolic acid as chiral selectors are the mainstream in the development of chiral ligand exchan...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/10
Inventor 丁国生黄晓佳刘莺王俊德
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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