Preparation and application of beta-cyclodextrin metal organic framework material HPLC column

A technology of cyclodextrin and organic ligand is applied in the field of preparation and application of chiral high performance liquid chromatography column materials to achieve the effect of expanding the scope of application

Active Publication Date: 2021-07-16
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation and application of beta-cyclodextrin metal organic framework material HPLC column
  • Preparation and application of beta-cyclodextrin metal organic framework material HPLC column
  • Preparation and application of beta-cyclodextrin metal organic framework material HPLC column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1: Preparation of β-CD-MOFs materials β-CD-MOFs-P50 and β-CD-MOFs-P20

[0064] One-pot synthesis of β-CD-MOFs-P50:

[0065] β-CD (0.67g), m-carboxybenzenesulfonyl chloride (0.52g) and potassium chloride (0.31g) were stirred and dissolved in 26mL methanol aqueous solution (concentration can be 20-90v / v%, no influence on product morphology) In this example, 120 mg of CTAB was added into methanol solution with a concentration of 60v / v%, sealed, and allowed to stand at room temperature for 24 hours to obtain colorless crystals, which were filtered and dried for later use. At this time, the particles of the obtained β-CD-MOFs material are relatively uniform, with a particle size of about 50 μm, named β-CD-MOFs-P50, and its specific appearance is as follows figure 1 shown.

[0066] Synthesis of β-CD-MOFs-P20 by vapor diffusion method:

[0067] β-CD (0.1000g), m-carboxybenzenesulfonyl chloride (0.0778g) and potassium chloride (0.0460g) were stirred and dissolved in ...

Embodiment 2

[0075] Example 2 Preparation of β-CD-MOFs chiral HPLC column

[0076] Using the two β-CD-MOFs materials synthesized in Example 1 as chiral separation materials, they were prepared as chiral HPLC column fillers, and then prepared high-performance liquid chromatography HPLC columns. Transmission electron microscopy and scanning electron microscopy were used to confirm the properties of the fillers. Pros and cons.

[0077] 1. Preparation method of HPLC column packing

[0078] The preparation method is as follows: first acidify commercially available silica beads with a particle size of 5 μm (i.e. fully porous spherical silica gel), dry them for later use; β-CD-MOFs (β-CD-MOFs-P50 or β-CD-MOFs-P20) in N 2 In the atmosphere, add the treated fully porous spherical silica gel (the mass ratio of β-CD-MOFs to fully porous spherical silica gel in this example is 1:2), stir and react at 115°C for 24h, filter, wash and dry after the reaction is complete ,spare.

[0079] 2. Characteriz...

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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 two beta-CD-MOFs high performance liquid chromatography chiral column materials, and an HPLC chiral column prepared from the beta-CD-MOFs materials can be used for splitting enantiomers of chiral substances. The preparation comprises the following steps: 1, constructing a chiral environment by using the beta-CD-MOFs material, bonding the chiral environment with high performance liquid chromatography silicon beads to form a stationary phase filler, and further preparing the chiral column which is applied to high performance liquid chromatography; 2, finding the optimal formula and conditions through proper characterization means, and optimizing the method and the conditions; 3, the preparation method of the oxaprop-p-ethyl and chlorpheniramine maleate single enantiomer can be established by using the prepared beta-CD-MOFs chiral column. and 4, the prepared beta-CD-MOFs chiral column can be used for separating the chiral compound, and a method for separating and qualitatively and quantitatively analyzing enantiomers of nine chiral substances, namely oxaprop-p-ethyl, quizalofop-p-ethyl, fluralan, bifenthrin, ranolazine, ornidazole, doxazosin, chlorpheniramine maleate and dropropizine is established.

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 two kinds of β-cyclodextrin (β-CD) metal-organic framework (metal-organic framework (MOFs)) material HPLC hand The preparation and application of chiral column materials, that is, the method of preparing β-CD-MOFs materials into HPLC chiral columns, and the separation research and application of chiral pesticides and chiral drug enantiomers. Background technique [0002] The growing demand for materials science has led to the continuous discovery of various new materials, and metal-organic frameworks (Metal-Organic Frameworks, MOFs) materials have achieved unprecedented development due to their flexible plasticity and excellent functionality. The excellent functionality of MOFs is mainly reflected in the large specific surface area, high porosity and structural diversity. Plasticity is m...

Claims

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Application Information

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IPC IPC(8): B01J20/29B01J20/30B01D15/38C07C69/743C07B57/00C07C67/56C07D213/38C07D241/04C07D241/44C07D261/04C07D263/58C07D295/15C07D405/12
CPCB01J20/29B01D15/3833C07B57/00C07D263/58C07D213/38C07D295/15C07D241/04C07C67/56C07D241/44C07D405/12C07D261/04C07B2200/07C07C2601/02C07C69/743
Inventor 沈静茹陆金富覃信铭李春涯
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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