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Process for preparing chlorogenic acid from honeysuckle

A technology of chlorogenic acid and honeysuckle, which is applied in the separation/purification of carboxylate, organic chemistry and other directions, can solve the problems of inability to carry out large-scale industrial production, inability to declare national first-class new drugs, etc., and achieve the effect of increasing the extraction cost.

Inactive Publication Date: 2005-05-18
济南永曜医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the instability of chlorogenic acid, it is often accompanied by the decomposition of chlorogenic acid during the extraction and separation process, and it is difficult to make the content reach more than 90%. For example, the extraction method recorded in Chinese patent 01144170.4 can only extract 84% of purity , The extraction method recorded in Chinese patent 02133448.X can only extract 80% of the purity
Although some laboratory preparation methods can obtain higher purity, they cannot be used for large-scale industrial production
Therefore, although the curative effect of chlorogenic acid is definite, it has been unable to declare the national first-class new drug due to the technical reasons of extraction and separation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 500g of honeysuckle is packed into the extractor, water with 5 times the weight of honeysuckle is added, and heating is extracted three times, each time being 3.5 hours. Medicinal solution is filtered and decompressed to recover solvent, and medicinal ethanol is added for precipitation, so that the final alcohol content reaches 75%, let stand overnight, filter or centrifuge, discard the precipitate, concentrate the filtrate to no ethanol, add water to make every milliliter contain 2g of crude drug. 0.5g, let it stand overnight, filter or centrifuge to discard the precipitate, and put the filtrate on a macroporous resin column. Elute with water and 10% ethanol, check by thin layer chromatography, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, and collect the components containing chlorogenic acid The acid eluate was concentrated to 2 g crude drug per m...

Embodiment 2

[0023] Put 250g of honeysuckle into the extractor, add ethanol with 5 times the weight of the crude drug, heat and reflux to extract three times for 3 hours, filter, recover the solvent from the filtrate, add water to make the crude drug content per ml 0.5g, let stand overnight, filter or centrifuge Remove precipitation, put the filtrate on a macroporous resin column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, concentrate To contain 2g crude drug per milliliter, extract with ethyl acetate. The solvent was recovered to obtain a concentrate, which was dried to obtain 4 g of fine chlorogenic acid with a content greater than 95%.

Embodiment 3

[0025] Put 1250g honeysuckle into the extractor, add 5 times the amount of 30% ethanol, heat and extract three times for 2.5 hours, filter, recover the solvent from the filtrate, add medicinal ethanol to make the alcohol content 50%, let it stand overnight, filter or centrifuge and discard Remove precipitation, put the filtrate on a macroporous resin column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, put it on a polyamide column, elute with water and 10% ethanol, collect the components containing chlorogenic acid, concentrate to the extract form, dried under reduced pressure, applied to a silica gel chromatographic column, eluted with ethyl acetate-ethanol, recovered the eluent, and obtained chlorogenic acid crystals with a content greater than 98%.

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PUM

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Abstract

The present invention relates to process of extracting chlorogenic acid from honeysuckle and belongs to the field of medicinal chemical technology. The process includes the steps of: reflux extraction of honeysuckle with water or ethanol, filtering to collect filtrate, recovering solvent, ethanol deposition to eliminating impurity, letting stand overnight, filtering, decompression recovering solvent, adding water and letting stand overnight, filtering, eluting the filtrate in macroporous resin column, concentrating eluent, collecting chlorogenic acid component, eluting on polyamide column with eluent, collecting chlorogenic acid component, concentration, rectification to obtain chlorogenic acid product with content over 95 %. The present invention is suitable for industrial application.

Description

technical field [0001] The invention relates to a process for extracting and separating chlorogenic acid from honeysuckle. Background technique [0002] Honeysuckle is a commonly used traditional Chinese medicine with a long history of medicinal use. Traditional medicine believes that honeysuckle has the functions of clearing away heat and detoxifying, cooling and dispelling wind-heat, and it is mostly used clinically to treat febrile diseases, fever, wind-heat cold, sore throat, pneumonia, erysipelas and other diseases. "Pharmacopoeia of the People's Republic of China" 2000 Edition stipulates that chlorogenic acid is an index component in honeysuckle, and its content shall not be less than 1.5%. However, the content of chlorogenic acid in honeysuckle is extremely unstable, and is easily affected by various internal and external factors. Medical research and practice have proved that chlorogenic acid is the most important active ingredient in honeysuckle. Chlorogenic acid...

Claims

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Application Information

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IPC IPC(8): C07C67/48C07C69/732
Inventor 庞松涛薛惠新
Owner 济南永曜医药科技有限公司
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