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Monolithic column, preparation method and application thereof

A technology of monolithic columns and ligands, applied in the field of preparation of monolithic separation media, can solve the problems of easy chain transfer, difficult to precisely control the pore size, poor mechanical properties, etc., to improve the non-uniformity of the column structure and the reproducibility of the preparation method. Good, improve the effect of volume shrinkage

Inactive Publication Date: 2009-09-23
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the reaction mechanism of ordinary free radical polymerization itself, such as fast reaction speed, uncontrollable molecular weight, and easy chain transfer, etc., the prepared column structure is mostly a particle-stacked structure. There are many disadvantages in this structure of column: Such as uneven structure, difficult to precisely control the pore size, poor mechanical properties, etc.
However, these two methods still have some limitations, such as the narrow range of material selection in the step-by-step polycondensation method; the high temperature (>100°C) required for the regulation of polymerization by nitroxide radicals, and inconvenient operation, etc.

Method used

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  • Monolithic column, preparation method and application thereof

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preparation example Construction

[0021] In the method for preparing a monolithic column provided by the present invention, the polymer monolithic separation medium used is formed by the polymerization of divinyl polymerized monomers ethylene glycol methacrylate and divinylbenzene, and the polymerization system also includes methanol and n-hexane A composite porogen composed of two organic substances, a composite porogen composed of toluene and dodecanol, an initiator, a catalyst and a catalyst ligand.

[0022] The concrete steps of this method are as follows:

[0023] 1) Synthesis of monolithic column:

[0024] Inject the reaction solution after mixing the above substances into the mold, such as 50×4.6mm i.d., 100×4.6mm i.d. stainless steel chromatographic column tube, react at room temperature for a sufficient time, and then connect it to the high-pressure infusion pump and rinse with organic solvent Porogens and other soluble substances in the column;

[0025] 2) Modification of the integral column:

[0...

Embodiment 1

[0030] Reagents and solvents:

[0031] The polymerization monomer is ethylene glycol methacrylate (EDMA); the porogen is methanol and n-hexane; the initiator is bromopropionate (BPE); the catalyst is CuBr and CuBr 2 ; The polyamine is pentamethyldiethylenetriamine (PDMETA), the bipyridine is 2,2-bipyridine (BPY), the antioxidant is ascorbic acid (vitamin C, Vc), and the modified functional monomer is methacrylic acid n-butyl ester.

[0032] Column preparation process:

[0033] The first step, column synthesis

[0034] EDMA 0.50mL (2.64mM), 0.50mL methanol, 0.50mL n-hexane, 0.050mL (0.39mM) BPE, 0.056g (0.39mM) CuBr, 0.080mL (0.39mM) PDMETA mixed together, ultrasonically mixed and injected into stainless steel In the chromatographic column tube, after reacting at room temperature for 24 hours, install the chromatographic column head at both ends of the column tube, and then connect it to a high-pressure infusion pump. 1, v / v) Washing with mixed solvent, and then carry out A...

Embodiment 2

[0042] Reagents and solvents:

[0043] The polymerization monomer is ethylene glycol methacrylate (EDMA); the porogen is methanol and n-hexane; the initiator is bromopropionate (BPE); the catalyst is CuBr and CuBr 2 The polyamine is pentamethyldiethylenetriamine (PDMETA), the bipyridine is 2,2-bipyridine (BPY), the antioxidant is ascorbic acid (vitamin C, Vc), and the modified functional monomer is ethyl methacrylate ester.

[0044] Column preparation process:

[0045] The first step, column synthesis

[0046] This step is exactly the same as the first step in Example 1.

[0047] The second step, cylinder modification

[0048] The proportion of grafting reaction solution is 68mg (0.39mM) CuBr 2 , 87mg (0.39mM) PMDETA, methanol and n-hexane (1:1, v / v) 50.0mL, ethyl methacrylate 3.12g (27.3mM), Vc 0.27g (1.56mM), after ultrasonic mixing, use The syringe pump was injected into the chromatographic column at a flow rate of 3.0 mL / h and reacted at room temperature for 14 h. A...

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Abstract

The invention discloses a monolithic column, a preparation method and a application thereof. The preparation method comprises the following steps: 1) polymeric monomer, pore-foaming agent, initiator and cuprous bromide are mixed together and then added with catalyst ligand after being deoxidized; the mixture is put into a chromatographic column tube to react in a sealing way; after the reaction, the chromatographic column tube is connected with a high pressure transfer pump, and the soluble substances such as the pore-foaming agent and the like are rinsed and removed by organic solvent, so that a monolithic column with a three-dimensional continuous skeleton structure is obtained; 2) the mixture of the organic solution, catalyst, catalyst ligand and antioxidant of the functional monomer is injected into the monolithic column, and bromine group remained on the surface of the column body initiates the surface grafting polymerization reaction of vinyl monomer. The method leads polymerization reaction to be carried out at the room temperature, so as to greatly solves the problems of inhomogeneous column body structure, volume contraction and the like caused by high polymerization temperature. Compared with the traditional monolithic column, the obtained monolithic column has obviously different structure, thus being applicable to separating biological macromolecules such as steroid hormone drugs, protein or the like.

Description

technical field [0001] The invention relates to a method for preparing an integral separation medium, in particular to an integral column and its preparation method and application. Background technique [0002] With the development of proteomics, the requirements for fast, efficient and high-throughput separation science are getting higher and higher. As far as the application of high performance liquid chromatography in separation science research is concerned, people have made corresponding improvements in hardware (high pressure infusion pump, chromatographic column, detector) and software (data acquisition system and processing software). The core part of chromatographic separation is the chromatographic column. The traditional packed column cannot achieve a balance between column efficiency and flux, that is, the column back pressure also increases when the column efficiency is improved, which cannot meet the requirements of fast, efficient, and high throughput. Separ...

Claims

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Application Information

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IPC IPC(8): B01J20/281C07J5/00C07J1/00C07J7/00C07K1/16
Inventor 齐莉张荣月辛培勇魏晓奕姚春荷乔娟
Owner INST OF CHEM CHINESE ACAD OF SCI
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