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Method for purifying phloretin from malus spectabilis leaves

A technology of phloretin and Begonia leaves, applied in the field of phloretin purification, can solve the problems of large amount of solvent, long period of macroporous resin chromatography, restricting industrialization, etc., to avoid cost, save time and cost, process simple effect

Active Publication Date: 2017-05-10
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the shortcomings of macroporous resin chromatography, such as long cycle time and large amount of solvent, the possibility of industrialization is greatly limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 5kg of dried leaves of Hubei crabapple (with phlorizin content 10.3%), put them into an extraction tank, add 50L and 40L of 30% ethanol to extract twice, 2h each time, after filtering the extract, concentrate under reduced pressure to a density of 1.15, add 4 times the volume of absolute ethanol, filter overnight after alcohol precipitation, concentrate the filtrate until there is no alcohol smell, add 1 / 2 volume of butyl acetate to extract twice, concentrate the extract and dry to obtain the extract. After adding 8 times the amount of the extract to reflux and dissolve it, it is filtered. The filtrate is cooled and crystallized under stirring, filtered, and dried to obtain 460.5 g of light yellow crystals with a content of 93.2%.

[0029] The light yellow crystals were added to 10 times the amount of 1.5mol / L hydrochloric acid, reacted at 85-95°C for 4h, cooled to room temperature to adjust the pH to 5-6, filtered and concentrated to obtain crude phloretin. The crude...

Embodiment 2

[0031] Take 5kg of dried leaves of Hubei crabapple (with phlorizin content 10.3%), put them into the extraction tank, add 60L and 50L of 50% ethanol to extract twice, 2h each time, after the extract is filtered, the filtrate is concentrated to density under reduced pressure It is 1.18, add 4 times volume of absolute ethanol, filter overnight after alcohol precipitation, concentrate until no alcohol smell, add 1 / 2 volume of ethyl acetate to extract twice, concentrate the extract and dry to obtain the extract. After adding 8 times the amount of water to the extract to reflux and dissolve, it is filtered. The filtrate is cooled and crystallized under stirring, filtered, and dried to obtain 463.0g of light yellow crystals with a content of 92.5%.

[0032] The light yellow crystals were added to 10 times the amount of 1.5mol / L hydrochloric acid, reacted at 85-95°C for 4h, cooled to room temperature to adjust the pH to 5-6, filtered and concentrated to obtain crude phloretin. The crude...

Embodiment 3

[0034] Take 10kg of Hubei crabapple dry leaves (with phlorizin content 10.3%), put them into an extraction tank, add 120L and 80L of 70% ethanol to reflux extraction twice, 2h each time, after filtering the extract, concentrate under reduced pressure to a density 1.12, add 4 times the volume of absolute ethanol, filter overnight after alcohol precipitation, concentrate the filtrate until there is no alcohol smell, add 1 / 2 volume of dichloromethane for extraction twice, concentrate the extract and dry to obtain the extract. Add 8 times the amount of the extract and reflux to dissolve and filter. The filtrate is cooled and crystallized under stirring conditions, filtered, and dried to obtain 918.3 g of light yellow crystals with a content of 91.6%.

[0035] Add light yellow crystals to 10 times the amount of 0.5mol / L hydrochloric acid, react at 85-95°C for 4h, cool to room temperature to adjust pH to 5-6, filter and concentrate to obtain crude phloretin. The crude product was reflu...

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PUM

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Abstract

The invention relates to a method for purifying phloretin from malus spectabilis leaves. According to the technical scheme, the method mainly comprises the steps of extraction, alcohol precipitation, extraction, crystallization, acid hydrolysis, extraction, purification and the like, accordingly the phloretin content of 98% or above is obtained, and the yield is 70% or above. The method is simple in process, low in cost and suitable for industrialized production.

Description

Technical field [0001] The invention relates to a method for purifying phloretin, specifically a method for purifying phloretin from leaves of crabapple. Background technique [0002] The chemical name of phloretin: 3-(4-hydroxyphenyl)-1-(2, 4, 6-trihydroxyphenyl)-1-propanone, which is a flavonoid. Phloretin has a strong moisturizing effect, as well as good antioxidant, anti-cancer, and whitening effects. With the increasing demand for high-purity phloretin, it has a broad market prospect. [0003] For the extraction of phloretin, phloretin is generally extracted first, and then subjected to enzymatic or acid hydrolysis to obtain phloretin. For example, the patent application number: 201010510889.x. This invention uses apple and crabapple leaves as raw materials. After the extract is purified by macroporous resin, the phloretin with a purity of more than 96% is prepared by biological enzymatic hydrolysis. However, enzymatic hydrolysis restricts its application due to high cost a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C49/83
CPCC07C45/78C07C49/83
Inventor 张则平梁红宝姚景春赵金伟
Owner LUNAN PHARMA GROUP CORPORATION
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