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Preparation and application of bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin hplc column material

A technology of deoxycitric acid and chiral stationary phase, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, chemical instruments and methods, etc., and can solve the problems of difficult and mutual exclusion of chromatographic columns

Active Publication Date: 2020-04-21
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, dry packing will still cause the packing to adhere to the inner wall, and will repel each other due to strong electrostatic interaction, making it difficult to fill the chromatographic column evenly and tightly.

Method used

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  • Preparation and application of bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin hplc column material
  • Preparation and application of bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin hplc column material
  • Preparation and application of bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin hplc column material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: Bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin (β-CD-D 2 ) preparation

[0054] According to the literature (Ding Zhigang, Ren Weiheng, Xi Lingling, etc., the synthesis of β-cyclodextrin derivatives and their inhibitory effect on urease. Catalytic Chemistry, 1996, 6(17): 567-569.) prepared β-CD-D 2 Finally, it was determined to be the desired target compound by means of ultraviolet, infrared spectroscopy, fluorescence and XRD.

[0055] Specific method: first place maleic anhydride and β-CD (molar ratio 15:1) in a constant temperature water bath at 80°C to react for 8 hours, stop the reaction, and post-process the powdery product that is β-CD-maleic anhydride (abbreviated as β -CD-A 2 ), placed in a desiccator for later use. β-CD-A 2 Put it in an Erlenmeyer flask with chloroacetic acid (molar ratio 1:4), react in a constant temperature water bath at 80°C for 8 hours, take it out and cool it to room temperature, and post-process the white powder pr...

Embodiment 2

[0067] Example 2β-CD-D 2 Preparation of Chiral HPLC Columns

[0068] Using the chiral separation material synthesized in Example 1—two [-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin (β-CD-D 2 ) as an HPLC chiral selector to prepare a chiral HPLC column filler, and then prepare a high performance liquid chromatography HPLC column, and use a transmission electron microscope and a scanning electron microscope to confirm the quality of the filler preparation.

[0069] 1. Preparation method of HPLC column packing

[0070] The preparation method is as follows: first acidify the commercial silica beads (fully porous spherical silica matrix) with a particle size of 5 μm, and dry them for later use; β-CD-D 2 In the crosslinking agent γ-(2,3-glycidoxy)propyltrimethoxysilane (β-CD-D 2 In the presence of cross-linking agent molar ratio 5:1), N 2In the atmosphere, add the treated fully porous spherical silica gel (the present embodiment β-CD-D 2 The mass ratio to fully porous sp...

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Abstract

The invention relates to the technical field of preparation and application of chiral high-performance liquid chromatography column materials, and discloses preparation and application of beta-CD-D2 high-performance liquid chromatography chiral column material. A high-performance liquid chromatography chiral column is prepared from beta-CD-D2 and is used for splitting chiral medicine enantiomers. The preparation and the application of the beta-CD-D2 high-performance liquid chromatography chiral column material comprise the following steps: 1, constructing a chiral environment by using beta-CD-D2, bonding the chiral environment with high-performance liquid chromatography silica beads into a fixed phase filler, then preparing the fixed phase filler into a chiral column, and applying the chiral column into high-performance liquid chromatography; 2, finding out an optional formula and an optional condition by using a proper characterization means, and optimizing the method and the condition; 3, establishing a preparation method of a salmeterol single enantiomer by using the prepared beta-CD-D2 chiral column, and splitting a chiral compound by using a cyclodextrins derivative for the first time; and 4, splitting drugs by using the prepared beta-CD-D2 chiral column, and establishing a method for splitting and qualitatively and quantitatively analyzing seven chiral drugs including salmeterol, terbutaline, procaterol, cetirizine, lamivudine, cefuroxime and ceftriaxone.

Description

technical field [0001] The invention relates to the technical field of preparation and application of chiral high-performance liquid chromatography (HPLC) column materials, in particular to a bis[-6-oxo-(3-deoxycitrate monoester-4)]-β-cyclodextrin (β-CD-D 2 ) Preparation and application of HPLC chiral column materials, namely β-CD-D 2 The preparation method of high-performance liquid chromatography (HPLC) chiral column and the separation research and application of enantiomers of chiral drugs. Background technique [0002] The resolution of optical isomers in chiral drugs by high performance liquid chromatography is mainly determined by the interaction force between the sample and the stationary phase. Synthesis and derivation of new, durable and efficient chiral stationary phases is an important step in liquid chromatography. One of the key tasks of gender split. In the resolution process, the chiral environment is created by introducing these stationary phases, and the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/29B01J20/30C07B57/00C07C213/10C07C217/10C07C215/60C07D215/26C07D295/088C07D411/04C07D501/34C07D501/36C07D501/12
CPCB01J20/286B01J20/29C07B57/00C07B2200/07C07C213/10C07D215/26C07D295/088C07D411/04C07D501/12C07D501/34C07D501/36C07C217/10C07C215/60
Inventor 沈静茹吴天骄柯雅莉付诗瑜
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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