CN104045671A - Method for extracting and purifying phlorizin in apple root-bark - Google Patents

Method for extracting and purifying phlorizin in apple root-bark Download PDF

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Publication number
CN104045671A
CN104045671A CN201310108251.7A CN201310108251A CN104045671A CN 104045671 A CN104045671 A CN 104045671A CN 201310108251 A CN201310108251 A CN 201310108251A CN 104045671 A CN104045671 A CN 104045671A
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China
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phlorizin
extracting
root bark
apple fruit
purifying
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CN201310108251.7A
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Chinese (zh)
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盘斌
窦家琨
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Yongzhou Yi Dong Biotechnology LLC
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Yongzhou Yi Dong Biotechnology LLC
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Priority to CN201310108251.7A priority Critical patent/CN104045671A/en
Publication of CN104045671A publication Critical patent/CN104045671A/en
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Abstract

The invention discloses a method for extracting and purifying phlorizin in apple root-bark. The method comprises the following steps: 1, extraction: crushing an apple root-bark raw material, extracting the crushed raw material with low degree alcohol 1-3 times, and collecting to obtain an extract liquid; 2, concentration: carrying out reduced pressure concentration on the extract liquid until no alcohol in the extract liquid, cooling, and filtering to remove precipitates to obtain a filtrate; 3, resin adsorption: carrying out macro-porous resin adsorption on the filtrate, cleaning with distilled water, eluting with 50% alcohol, collecting the obtained 50% alcohol eluate, carrying out reduced pressure concentration, cooling for precipitating crystals at 0-40DEG C, and centrifuging and dehydrating the obtained crystals; and 4, recrystallization: dissolving the crystals by adding distilled water and heating, adding active carbon, dehydrating, centrifuging, carrying out reduced pressure concentration on the obtained filtrate, recrystallizing, and drying to obtain a phlorizin product with the content of above 98%.

Description

A kind of method of extracting purifying phlorizin from apple fruit root bark
Technical field
The present invention relates to a kind of extraction process of natural phant effective ingredient, be specifically related to a kind of method of extracting phlorizin from apple fruit root bark.
Background technology
Phlorizin belongs to plant polyphenol compounds, has another name called phlorrhizen, and structural formula is as follows.Micro-yellow acicular crystals, can be dissolved in hot water, methyl alcohol, ethanol, acetone, ethyl acetate etc., is insoluble to ether, chloroform and benzene.Report, with skin glycosides, can activate cellular protein expression kinases, the unordered hyperplasia of cell is had to restraining effect, can be used for the assisting therapy of skin carcinoma and other tumours; Phlorizin has significant step-down, effect for reducing fat, and being described as is " natural depressor ", and energy check melanin cytoactive, has desalination effect etc. to various skin splashs.
At present, the current phlorizin technological process of production is: by raw material pulverizing, add alcohol heat reflux to extract, concentration and recovery ethanol is complete, filters, and filtrate is through macroporous resin adsorption, with ethanol gradient elution, by effluent liquid Fractional Collections, concentrated, with chloroform extraction, abandon chloroform layer, reconcentration to proportion is that 1~1.08,0~4 ℃ of crystallization is analysed, centrifugal, be dried to obtain finished product.This technical process is complicated, and cost is high, has adopted solvent chloroform, and production process danger is larger, and product has dissolvent residual.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of method of extracting purifying phlorizin from apple fruit root bark is provided, and the method technical process is simple, and production cost is low, pollutes littlely, is applicable to suitability for industrialized production.
For solving this technical problem: the technical solution used in the present invention is:
A method of extracting purifying phlorizin from apple fruit root bark, comprises the following steps:
(1) extract: by apple fruit root bark raw material pulverizing, by 15%~50% alcohol immersion of 4~6 times of amounts 2~3 hours for the apple fruit root bark after pulverizing, drop in extractor and boil, keep micro-and boil 2~3 hours, for the first time extracting solution; Again the residue dregs of a decoction are extracted 2~3 hours with 15%~50% alcohol heat reflux of 3~5 times of amounts, extracting solution for the second time, merging for the first time with secondary extracting solution;
(2) concentrated: extracting solution vacuum is reclaimed to ethanol complete, liquid is concentrated into 3~4 times of former extracting solution, and cooled and filtered obtains filtrate;
(3) resin absorption: filtered liquid is through macroporous resin adsorption, first with deionized water, effluent liquid is washed down, use again 40%~60% ethanol elution, collect alcohol eluen, it is complete that vacuum concentration reclaims ethanol, and liquid is concentrated into 0.5~1 times of amount of material quantity, standing cooling, 0 ℃~4 ℃ crystallizations, high speed centrifugation dehydration, obtains phlorizin coarse-grain;
(4) recrystallization: by the phlorizin coarse-grain obtaining, deionized water heating for dissolving by 5~8 times of amounts, the activated carbon decolorizing 30~60 minutes that adds again phlorizin coarse-grain weight 1%~8%, bleaching temperature is 60 ℃~80 ℃, filtered while hot, and filtrate adds alkaline reagents to be adjusted to weakly alkaline while hot, 0 ℃~4 ℃ placement crystallizations of filtrate, high speed centrifugation dehydration, vacuum-drying, obtains phlorizin finished product.
The ethanol adding in step (1) is 30%.
Macroporous resin described in step (3) is HPD100, HPD400 or D101.
Alkaline reagents described in step (4) is sodium hydroxide, potassium hydroxide, sodium bicarbonate or sodium carbonate.
Alkaline reagents described in step (4) is the mixing of any two kinds in sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate.
The ionized water adding described in step (4) is 7 times of amounts, and gac is 5% times of amount, and bleaching time is 40 minutes, and bleaching temperature is 75 ℃.
Weakly alkaline described in step (4) is that pH is between 7.5~8.5.
Advantage of the present invention is:
The one, in technological process, adsorption and desorption by resin is without gradient elution, thereby avoided the complicated technology of Fractional Collections.
The 2nd, in technological process, only used ethanol organic solvent, reduced the hazardous solvent in product residual, improved quality product.
The 3rd, phlorizin content >=97% of the method gained, the effective constituent rate of recovery is more than 80%.
Embodiment
Embodiment 1
(1) extract: by apple root raw material pulverizing, by 30% alcohol immersion of 6 times of material quantities 2 hours for apple fruit root bark, add in extractor and boil, keeping micro-boils 3 hours, obtain extracting solution, the dregs of a decoction extract 3 hours with 30% alcohol heat reflux of 5 times of material quantities again, obtain secondary raffinate, united extraction liquid;
(2) concentrated: extracting solution vacuum is reclaimed to ethanol complete, liquid is concentrated into 4 times of material quantity, and cooled and filtered obtains filtrate;
(3) resin absorption: filtered liquid is through D101 macroporous resin adsorption, crossing column flow rate is 2VB/h, first with deionized water, effluent liquid is washed down, then use 50% ethanol elution, collect alcohol eluen, it is complete that vacuum concentration reclaims ethanol, liquid is concentrated into 0.8 times of amount of material quantity, standing cooling, 0 ℃~4 ℃ crystallizations, high speed centrifugation dehydration, obtains coarse-grain;
(4) recrystallization: by the phlorizin coarse-grain obtaining, by 6 times of deionized water heating for dissolving, the activated carbon decolorizing 60 minutes that adds phlorizin coarse-grain weight 8%, bleaching temperature is 80 ℃, filtered while hot, and it is 8 that filtrate adds NaOH to adjust pH value while hot, 0 ℃~4 ℃ placement crystallizations of filtrate, high speed centrifugation dehydration, vacuum-drying, obtains phlorizin finished product; In phlorizin product, phlorizin content is 98.3%, and the effective constituent rate of recovery is 84.3%.
Embodiment 2
(1) extract: by apple root raw material pulverizing, by 50% alcohol immersion of 5 times of material quantities 3 hours for apple fruit root bark, add and boil, keep micro-and boil 2 hours, obtain extracting solution, the dregs of a decoction extract 2 hours with 50% alcohol heat reflux of 5 times of material quantities again, obtain secondary raffinate, united extraction liquid;
(2) concentrated: extracting solution vacuum is reclaimed to ethanol complete, liquid is concentrated into 3.5 times of material quantity, and cooled and filtered obtains filtrate;
(3) resin absorption: filtered liquid is through HPD100 macroporous resin adsorption, crossing column flow rate is 1VB/h, first with deionized water, effluent liquid is washed down, then use 50% ethanol elution, collect alcohol eluen, it is complete that vacuum concentration reclaims ethanol, liquid is concentrated into 0.5 times of amount of material quantity, standing cooling, 0 ℃~4 ℃ crystallizations, high speed centrifugation dehydration, obtains coarse-grain;
(4) recrystallization: by the phlorizin coarse-grain obtaining, by 8 times of deionized water heating for dissolving, the activated carbon decolorizing 40 minutes that adds phlorizin coarse-grain weight 5%, bleaching temperature is 70 ℃, filtered while hot, and it is 7.5 that filtrate adds Na2CO3 to adjust pH value while hot, 0 ℃~4 ℃ placement crystallizations of filtrate, high speed centrifugation dehydration, vacuum-drying, obtains phlorizin finished product; In phlorizin product, phlorizin content is 99.1%, and the effective constituent rate of recovery is 86.3%.

Claims (6)

1. from apple fruit root bark, extract a method for purifying phlorizin, comprise the following steps:
(1) extract: by apple fruit root bark raw material pulverizing, by 15%~50% alcohol immersion of 4~6 times of amounts 2~3 hours for the apple fruit root bark after pulverizing, drop in extractor and boil, keep micro-and boil 2~3 hours, for the first time extracting solution; Again the residue dregs of a decoction are extracted 2~3 hours with 15%~50% alcohol heat reflux of 3~5 times of amounts, extracting solution for the second time, merging for the first time with secondary extracting solution;
(2) concentrated: extracting solution vacuum is reclaimed to ethanol complete, liquid is concentrated into 3~4 times of former extracting solution, and cooled and filtered obtains filtrate;
(3) resin absorption: filtered liquid is through macroporous resin adsorption, first with deionized water, effluent liquid is washed down, use again 40%~60% ethanol elution, collect alcohol eluen, it is complete that vacuum concentration reclaims ethanol, and liquid is concentrated into 0.5~1 times of amount of material quantity, standing cooling, 0 ℃~4 ℃ crystallizations, high speed centrifugation dehydration, obtains phlorizin coarse-grain;
(4) recrystallization: by the phlorizin coarse-grain obtaining, deionized water heating for dissolving by 5~8 times of amounts, the activated carbon decolorizing 30~60 minutes that adds again phlorizin coarse-grain weight 1%~8%, bleaching temperature is 60 ℃~80 ℃, filtered while hot, and filtrate adds alkaline reagents to be adjusted to weakly alkaline while hot, 0 ℃~4 ℃ placement crystallizations of filtrate, high speed centrifugation dehydration, vacuum-drying, obtains phlorizin finished product.
2. the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the ethanol adding in step (1) is 30%.
3. the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the macroporous resin described in step (3) is HPD100, HPD400 or D101.
4. the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the alkaline reagents described in step (4) is sodium hydroxide, potassium hydroxide, sodium bicarbonate or sodium carbonate.
5. the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the alkaline reagents described in step (4) is the mixing of any two kinds in sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate.
6. the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the ionized water adding described in step (4) is 7 times of amounts, and gac is 5% times of amount, and bleaching time is 40 minutes, and bleaching temperature is 75 ℃.7, the method for extracting purifying phlorizin from apple fruit root bark according to claim 1, is characterized in that: the weakly alkaline described in step (4) is that pH is between 7.5~8.5.
CN201310108251.7A 2013-03-16 2013-03-16 Method for extracting and purifying phlorizin in apple root-bark Pending CN104045671A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104480080A (en) * 2014-11-21 2015-04-01 西北农林科技大学 Recombinant apple phlorizin glycosyl transferase and separation and purification method thereof
CN105111256A (en) * 2015-08-16 2015-12-02 李玉山 Integrated extracting and purifying method for active ingredients of apple pomace
CN106336441A (en) * 2015-07-07 2017-01-18 天津优利果蔬食品有限公司 Extraction process of high-purity phloridzin
CN107602638A (en) * 2017-09-27 2018-01-19 三原利华生物技术有限公司 The method that phloridzin is prepared using apple branches and leaves, root skin
CN109535208A (en) * 2018-12-27 2019-03-29 大理大学 The method of phloridzin is prepared from M. rockii
CN112409312A (en) * 2020-12-18 2021-02-26 天津市尖峰天然产物研究开发有限公司 Method for extracting and purifying quercetin from young apple fruits
CN113512082A (en) * 2021-08-10 2021-10-19 湖南绿蔓生物科技股份有限公司 Method for extracting phlorizin and phloretin in apple root bark and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1683382A (en) * 2005-03-11 2005-10-19 天津市尖峰天然产物研究开发有限公司 Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material
CN101297880A (en) * 2007-04-30 2008-11-05 常州高新技术产业开发区三维工业技术研究所有限公司 Active extract containing phlorizin and uses thereof
CN101392008A (en) * 2007-09-18 2009-03-25 兴化格林生物制品有限公司 Extraction technique of high-purity phlorizin
WO2010012153A1 (en) * 2008-07-29 2010-02-04 常州高新技术产业开发区三维工业技术研究所有限公司 Phlorizin derivatives and their preparation and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1683382A (en) * 2005-03-11 2005-10-19 天津市尖峰天然产物研究开发有限公司 Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material
CN101297880A (en) * 2007-04-30 2008-11-05 常州高新技术产业开发区三维工业技术研究所有限公司 Active extract containing phlorizin and uses thereof
CN101392008A (en) * 2007-09-18 2009-03-25 兴化格林生物制品有限公司 Extraction technique of high-purity phlorizin
WO2010012153A1 (en) * 2008-07-29 2010-02-04 常州高新技术产业开发区三维工业技术研究所有限公司 Phlorizin derivatives and their preparation and application

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104480080A (en) * 2014-11-21 2015-04-01 西北农林科技大学 Recombinant apple phlorizin glycosyl transferase and separation and purification method thereof
CN106336441A (en) * 2015-07-07 2017-01-18 天津优利果蔬食品有限公司 Extraction process of high-purity phloridzin
CN105111256A (en) * 2015-08-16 2015-12-02 李玉山 Integrated extracting and purifying method for active ingredients of apple pomace
CN107602638A (en) * 2017-09-27 2018-01-19 三原利华生物技术有限公司 The method that phloridzin is prepared using apple branches and leaves, root skin
CN107602638B (en) * 2017-09-27 2021-03-02 三原利华生物技术有限公司 Method for preparing phlorizin by using apple branches, leaves and root barks
CN109535208A (en) * 2018-12-27 2019-03-29 大理大学 The method of phloridzin is prepared from M. rockii
CN112409312A (en) * 2020-12-18 2021-02-26 天津市尖峰天然产物研究开发有限公司 Method for extracting and purifying quercetin from young apple fruits
CN113512082A (en) * 2021-08-10 2021-10-19 湖南绿蔓生物科技股份有限公司 Method for extracting phlorizin and phloretin in apple root bark and application thereof

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