Preparation method of high-purity carnosol

A carnosol, high-purity technology is applied in the field of preparation of natural active compounds, which can solve the problems of limited sources, difficulties, and difficulty in obtaining target substances, and achieves the effects of simple operation process and controllable cost.

Inactive Publication Date: 2013-09-25
高政 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the Chinese patent CN102115442A, by extracting rosemary with a solvent and performing phosphoric acid-silica gel column chromatography under nitrogen protection, carnosol with a content of 92% is obtained. Although this method can obtain sage with a higher purity carnosol, but the conditions used are too harsh, the silica gel needs to be phosphorylated to make phosphoric acid-silica gel, and the chromatography process needs nitrogen protection, so it is difficult to prepare a large amount of carnosol, and it is also difficult to popularize and practically apply this special method
However, high-purity carnosic acid is required a...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 2000g of dried rosemary branches and leaves, add petroleum ether 14L, reflux extraction 3 times, each time for 3 hours, combine the extracts 3 times, concentrate and recover petroleum ether to obtain extract; dissolve the extract with 40% ethanol, filter Remove the insoluble matter, get 1000ml of mother liquor as the adsorption solution, and use 500ml of D101 macroporous adsorption resin for adsorption. After the adsorption is completed, use 1000ml of purified water to elute, and then use 1500ml of 90% ethanol solution for elution. The eluent is divided into 6 sections. Combine the 4 parts in the middle; concentrate the combined eluate to 100ml under reduced pressure, add 200ml of water, stir and precipitate the precipitate, and let it stand for 3 hours; centrifuge to obtain a precipitate containing carnosol; dissolve the precipitate with 200ml of ethyl acetate, and add 200ml of it to it Petroleum ether, stirred, and precipitated; filtered to obtain carnosol crude p...

Embodiment 2

[0019] Take 2000g of dried rosemary branches and leaves, add 10L of dichloromethane, reflux extraction 3 times, each time for 3 hours, combine the extracts 3 times, concentrate and recover dichloromethane to obtain extract; dissolve the extract with 60% ethanol , filtered to remove insoluble matter, 1000ml of mother liquor was obtained as the adsorption solution, and was adsorbed with 500ml AB-8 macroporous adsorption resin. 6 sections, 4 parts in the middle were combined; the combined eluate was concentrated under reduced pressure to 150ml, added 200ml of water, stirred to precipitate a precipitate, and left for 5 hours; centrifuged to obtain a precipitate containing carnosol; the precipitate was dissolved in 150ml of dichloromethane, Add 200ml of petroleum ether, stir, and precipitate; filter to obtain carnosol crude product, which is crystallized with 700ml of methanol to obtain carnosol crystals; filter and dry to obtain 14.7 g of crystals, and detect carnosol content by HP...

Embodiment 3

[0021] Weigh 500g of rosemary extract (the content of carnosol as determined by HPLC is 5.7%), dissolve it with 2500ml of 60% ethanol, filter out the insoluble matter, use the mother liquor as the adsorption liquid, and use 800ml of HZ818 macroporous adsorption resin for adsorption. After completion, elute with 2000ml of purified water, and then with 2000ml of 90% ethanol solution. The eluent is divided into 6 sections, and the middle 4 parts are combined; the combined eluent is concentrated to 300ml under reduced pressure, and 350ml of water is added, and stirred to precipitate Precipitate, stand for 3 hours; centrifuge to get a precipitate containing carnosol; dissolve the precipitate with 300ml of ethyl acetate, add 200ml of petroleum ether to it, stir, and precipitate out; filter to get the crude product of carnosol, which is crystallized with 1000ml of methanol , to obtain carnosol crystals; filtered and dried to obtain 23.9 g of crystals, and the content of carnosol was 9...

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Abstract

The invention relates to a preparation method of a natural active compound. The preparation method provided by the invention comprises the following steps: 1, extracting a dry carnosol-containing raw material per kilogram by the use of 3-10 liters of a lipophilic organic solvent for 2-5 times, merging extracts, and condensing to obtain a carnosol-containing extract or solid; 2, dissolving by the use of a 10-90% hydrophilic organic solvent, filtering and precipitating, and carrying out macroreticular resin refining processing on a filtrate to obtain a carnosol-containing precipitate; 3, dissolving the precipitate by the use of a mixed lipophilic organic solvent, standing, precipitating a precipitate; and filtering the precipitate to obtain a carnosol crude product; and 4, crystallizing by the use of a hydrophilic organic solvent so as to obtain high-purity carnosol crystals with the HPLC detection content being more than 95%. The preparation method provided by the invention has advantages of simple operation process and controllable cost, and is suitable for large-scale preparation and production of high-purity carnosol.

Description

technical field [0001] The invention relates to a preparation method of a natural active compound. Background technique [0002] rosemary( Rosmarinus officinalis Carnosol and other phenolic diterpenoids contained in plants such as L. are recognized as natural antioxidants in recent years and are widely used in the fields of food industry, daily chemical industry, medicine and health care; and studies have shown that carnosol Turmeric phenol can have anti-tumor effect by inhibiting NF-kB channel, so it is a natural active compound favored by new drug researchers in recent years. [0003] Regarding the preparation of carnosol, in the Chinese patent CN101040901A, a rosemary extract containing 5-12% carnosol is obtained by solvent extraction, cold precipitation, and activated carbon decolorization of rosemary; China In the patent CN101402864A, through the process of extracting the essential oil of rosemary with water vapor first, then extracting the residue with organic solve...

Claims

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Application Information

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IPC IPC(8): C07D493/08
Inventor 刘海龙高政
Owner 高政
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