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High molecular type reverse chromatography fixing phase and its preparing method

A reversed-phase chromatography, polymer technology, applied in the field of reversed-phase chromatography stationary phase and its preparation, can solve the problems of limited chemical stability, complicated preparation process conditions, affecting life, etc., and achieves fast adsorption-desorption process and chemical stability. Excellent performance and stable pore structure

Inactive Publication Date: 2007-06-27
刘开禄
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Then it also has several defects: (1) The chemical stability is limited, it can only be used in the range of PH2-9, and it cannot be regenerated with a solution with strong acid or strong alkali. Once it is contaminated by the sample, it is difficult to regenerate, thus affecting its (2) Its preparation requires expensive silicon etherification reagents, resulting in complex preparation process conditions and high production costs, so the price is relatively expensive; (3) In the preparation-grade chemically bonded silica sphere stationary phase, it often contains residual silanol groups, Easy to produce irreversible adsorption, affecting product yield
Therefore, the above deficiencies limit the widespread use of chemically bonded silica sphere immobilization in large-scale preparative chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A In the container, add 280g of divinylbenzene and 290g of ethylvinylbenzene into 120g of methylstyrene, stir evenly to form polymerized monomers;

[0030] B. Add 300g n-heptanol and 3.5g dibenzoyl peroxide to the polymerized monomer prepared in step A and mix uniformly to form an oil phase;

[0031] C. In a reactor equipped with a high-speed stirrer, add 15 g of gelatin and 150 g of sodium chloride into 3000 g of water, heat and stir to fully mix to form a water phase;

[0032] D. Add the oil phase to the water phase. Under high-speed stirring, the oil phase is fully dispersed into the water phase to form micro-droplets with a particle size of less than 0.3mm. Heat at 60-65°C for 8 hours, and then slowly increase the temperature to 100 Carry out free radical copolymerization reaction at ℃ to generate solid copolymer microbeads. After the reaction is completed, filter out the microbeads, steam the porogen with water steam, wash away the residual solvent and other impuri...

Embodiment 2

[0035] A In the container, add 280g of divinylbenzene and 290g of ethylvinylbenzene into 120g of styrene, stir evenly to form polymerized monomers;

[0036] B. Add 300g of 2-ethylhexanol and 7g of azobisisobutyronitrile to the polymerized monomer prepared in step A and mix uniformly to form an oil phase;

[0037] C. In a reactor equipped with a high-speed stirrer, add 15g of polyvinyl alcohol and 200g of calcium chloride into 3000g of water, stir and heat to fully mix to form a water phase;

[0038]D. Add the oil phase to the water phase, under high-speed stirring, the oil phase is fully dispersed into the water phase to form micro-droplets with a particle size of less than 0.3mm, heat at 60-65°C for 8 hours, and slowly heat up to 100°C Carry out free radical copolymerization reaction to generate solid copolymer microbeads. After the reaction is completed, filter out the microbeads, steam the porogen with water steam, and wash away the residual solvent and other impurities wit...

Embodiment 3

[0041] The composition of the device and the water phase is the same as in Example 1 of the present invention, and the oil phase consists of: 300g ethylene glycol dimethacrylate, 200g diallyl itaconate, 95g methyl methacrylate, 400g toluene, 6g Azobisisobutyronitrile, the operating steps and conditions are the same as in Example 1 of the present invention to obtain porous polymer beads; grading by sieving to obtain particle sizes of 0.3-0.2mm, 0.2-0.13mm, and 0.13-0.074mm respectively , 0.074-0.04mm, 0.04-0.03mm, 0.03-0.01mm particle size of five groups of porous microbeads, its chemical structure is cross-linked polymethyl methacrylate copolymer, the pore structure is a specific surface area of ​​100-120m 2 / g, with a pore size of 40-50%, and a pore size distribution of 50-800A°, these microbeads can be used as stationary phases for reversed-phase chromatography.

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Abstract

The invention is especially related to fixed phase of reversed phase chromatography (FPRPC) in macromolecule type of a series of different chemical constitution, and preparation method. Possessing macromolecule micro beads in regular spherical porous type, the disclosed FPRPC in macromolecule type possesses basic property of FPRPC. Using the disclosed FPRPC to carry out verification of chromatographic separation indicates that when macromolecule micro beads in porous type acts as FPRPC, pore structure is steady; under condition of compression elution, micro beads does not break up; adsorption-desorption procedure is quick; comparing with chemical bond silicon ball fixed phase in same granularity, FPRPC possesses closed column performance and closed separation. The disclosed FPRPC is applicable to separating and purifying medical bulk drug, and natural drug as well as applicable to enriching and preparing trace quantity substance in biologic and samples.

Description

technical field [0001] The invention relates to a class of reversed-phase chromatographic stationary phases and a preparation method thereof, in particular to a series of polymer reversed-phase chromatographic stationary phases with different chemical structures and a preparation method thereof. Background technique [0002] Reversed-phase chromatography is a chromatographic mode based on the hydrophobic effect between the solute, polar mobile phase, and non-polar stationary phase surface. This is the most widely used separation mode in HPLC. In pharmaceuticals, the vast majority of product analysis is done by this method, and it is widely used in the fields of agriculture, medicine, bioengineering, food and environmental science. Many organic compounds related to human life can be separated and prepared by reversed-phase chromatography. Reversed-phase chromatography stationary phase is the heart of reversed-phase chromatography, most of which are porous chemically bonded ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89B01J20/281
Inventor 刘开禄袁斯鸣刘进刘哗
Owner 刘开禄
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