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Synthesis for weak hydrophobic framework amide resin and application of the same in purifying gingko total lactone

A technology of total ginkgo lactone and amide resin, which is applied in the direction of medical raw materials derived from ginkgo biloba, can solve the problems of poor strength and resin rupture, and achieve the effects of environmental friendliness, low production cost and simple process

Inactive Publication Date: 2008-01-09
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this gel-type resin is in a highly swollen state in water, has poor strength, and will shrink in alcohol, which will cause resin rupture during actual column operation.

Method used

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  • Synthesis for weak hydrophobic framework amide resin and application of the same in purifying gingko total lactone
  • Synthesis for weak hydrophobic framework amide resin and application of the same in purifying gingko total lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of the amide adsorption resin of weak hydrophobic skeleton provided by the present invention is realized through the following steps:

[0027] At room temperature, dissolve polyvinyl alcohol in water to prepare 450g of an aqueous solution with a mass percentage of 0.5%, and heat it to 40°C in a water bath in a 1000ml three-necked flask; a mixture of 60.5g of methyl acrylate and 14.5g of divinylbenzene Reaction monomer, with 70g of heptane as porogen, 0.75g of azobisisobutyronitrile as initiator, mixed evenly, then added to a three-necked bottle, started stirring, adjusted the size of oil droplets between 0.3-1.0mm, and Suspension polymerization, slowly raise the temperature to 70°C for 4 hours at a heating rate of 1°C / min, then continue to raise the temperature to 85°C for 6 hours, stop the reaction, and obtain a white resin after filtration and washing.

[0028] Add 100g of the above-mentioned white resin to a 500ml three-necked bottle, fully swe...

Embodiment 2

[0032] At room temperature, dissolve polyvinyl alcohol in water to prepare 450g of an aqueous solution with a mass percentage of 1.0%, and heat it to 35°C in a water bath in a 1000ml three-necked flask; the total reaction unit is a mixture of 64g of methyl acrylate and 11g of divinylbenzene body, with 75g heptane as the porogen and 1.0g azobisisobutyronitrile as the initiator, mix evenly and add it into the three-necked bottle, start stirring, adjust the size of the oil droplets between 0.3-1.0mm, and carry out suspension polymerization , at a heating rate of 1°C / min, slowly raise the temperature to 65°C for 4 hours, then continue to raise the temperature to 85°C for 6 hours, stop the reaction, and obtain a white resin after filtration and washing.

[0033] Add 100g of the above-mentioned white resin into a 500ml three-necked bottle, fully swell with 400ml of N,N-dimethylformamide, add 150g of triethylenetetramine, stir evenly, heat up to 125°C and react for 10 hours, after the...

Embodiment 3

[0036] At room temperature, dissolve polyvinyl alcohol in water to prepare 4.5kg of an aqueous solution with a mass percentage of 1.5%, and heat it to 45°C in a water bath in a 10-liter three-necked bottle; use a mixture of 0.60kg methyl acrylate and 0.15kg divinylbenzene For the reaction monomer, use 0.68kg heptane as the porogen and 0.015kg azobisisobutyronitrile as the initiator, mix well and add it into the three-necked bottle, start stirring, and adjust the size of the oil droplets between 0.3-1.0mm , after suspension polymerization, slowly raise the temperature to 60°C for 4 hours at a heating rate of 1°C / min, then continue to raise the temperature to 85°C for 6 hours, stop the reaction, and obtain a white resin after filtration and washing.

[0037]Add 1 kg of the above-mentioned white resin to a 5-liter three-necked bottle, fully swell with 4 liters of N,N-dimethylformamide, add 1 kg of polyethylene polyamine, stir evenly, and raise the temperature to 130°C for 10 hours...

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Abstract

Synthesis of amide adsorptive resin with weak hydrophobic skeleton is carried out by co-polymerizing methyl acrylate with vinyl benzene to obtain ester-based resin, aminolyzing for ester base, acidylating to obtain amide adsorptive resin with weak hydrophobic skeleton, adsorbing flavone compound from Ginkgo extract onto resin by the resin and hydrogen bond synergistic function, flowing ginkgo-lactone, re-crystallizing and eluting to obtain final product. The purity is above 90%, it's simple and non-toxic, it has friendly environment and can be used to supply experimental samples for development of ginkgo lactone.

Description

【Technical field】 [0001] The invention belongs to the technical field of extraction and separation of effective components of traditional Chinese medicine, in particular to a preparation method of a hydrogen bond adsorption resin with a weak hydrophobic skeleton, and establishes an adsorption-elution one-step resin extraction process to prepare ginkgo with a purity higher than 90%. total lactones. 【Background technique】 [0002] Ginkgolide is one of the active ingredients in Ginkgo biloba extract. It is a unique ingredient in Ginkgo biloba with special molecular structure and significant pharmacological activity. It is an effective PAF (platelet aggregation inducer) natural antagonist. It can improve SOD activity, eliminate free radicals, and delay aging. In recent years, a lot of fruitful work has been carried out on the extraction and purification of ginkgolides at home and abroad. Existing extraction methods include organic solvent extraction and column chromatography. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/14C08F8/32A61K36/16
Inventor 王春红施荣富任萍
Owner NANKAI UNIV
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