CN102453039A - method for extracting ellagic acid from pomegranate bark by enzyme hydrolysis method - Google Patents
method for extracting ellagic acid from pomegranate bark by enzyme hydrolysis method Download PDFInfo
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- CN102453039A CN102453039A CN2010105294395A CN201010529439A CN102453039A CN 102453039 A CN102453039 A CN 102453039A CN 2010105294395 A CN2010105294395 A CN 2010105294395A CN 201010529439 A CN201010529439 A CN 201010529439A CN 102453039 A CN102453039 A CN 102453039A
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Abstract
The invention relates to the field of medicament preparation, provides a method for extracting ellagic acid from pomegranate bark by an enzyme hydrolysis method, and can be used for solving the problems of low conversion rate, low yield and poor product quality of ellagic acid preparation in the prior art. The method comprises the following steps: treating and extracting raw materials; performing oxidative dehydrogenation; and purifying. Enzyme hydrolysis operation is adopted, the production efficiency and conversion rate are greatly improved by adopting the method in the invention, more effective substances in the raw material can be converted into ellagic acid, the product quality is further improved, and the product has high purity, so that the product is suitable for industrial production.
Description
Technical field
The present invention relates to the Chinese medicine extraction of effective components, be specifically related to from pomegranate rind, extract the process for extracting of gallogen.
Background technology
Pomegranate rind extracts the method for gallogen
Pomegranate rind is the dry pericarp of Punicaceae plant pomegranate Punica Granatum L.; Have effects such as relieving diarrhea with astringents, hemostasis, expelling parasite; Be rich in the tannin constituents in the pomegranate rind, mainly contain gallic acid, gallogen, pomegranate woods, pomegranate glycosides, granatin A, granatin B, Nutgalls acyl dilactone etc.Gallogen wherein is the dimerization verivate of gallic acid, is a kind of polyphenol dilactone, and molecular formula is C14H6O8, as above shown in the molecular structure.
Modern study proof gallogen shows induces canceration and other multiple cancerations that the obvious suppression effect is arranged to chemical substance; Particularly colorectal carcinoma, the esophageal carcinoma, liver cancer, lung cancer, tongue and dermatoma etc. there are the good restraining effect, have effects such as antitumor, anti-oxidant, antibiotic and antiviral.[Angelika.Rommel, Ronald E.Wrolstad, Ellagic acid content of red raspberry juice as influenced by cultivar, processing; Andenvironmental factors, J.Agric.Food Chem., 1993,41 (11); Pp1951-1960] [Guo Zengjun, Tan Lin, Xu Ying, Wu Nan. the gallogen compounds is in botanic distribution and biologically active native Study on product and exploitation; 2010,22:519-524,540]
Summary of the invention
An object of the present invention is to solving above-mentioned prior art extraction time long; Transformation efficiency is low; Problems such as technological operation complicacy provide the safety, product recovery rate of a kind of simple operation, conversion high, can reach the process for extracting of the gallogen that suitability for industrialized production requires.
Extract the process for extracting of gallogen in a kind of pomegranate rind, adopt following process step:
1) processing of raw material;
2) hydrolysis is extracted;
3) oxydehydrogenation;
4) purifying.
Further, this method adopts following process step:
Said raw material be treated to the stir-fry charcoal: will clean through removing impurity, section is fried to the epidermis chocolate for 200-400 ℃ in the former medicinal heat pot of exsiccant pomegranate rind, and inner burnt brown is cut into slices or pulverized for use;
Extract: add 5-10 water doubly in the pomegranate rind section with stir-bake to brown, add 0.1-0.5 part enzyme solution, soak at room temperature 0.5-6 hour; Then with both mixture heating up to 80-100 ℃, be incubated 1-4 hour, continuous more than twice or twice; Residue obtained liquid; Merging concentrates, and the liquid concentrator weight ratio is pressed raw material ratio 1-3: 1, be medicinal extract liquid;
Oxydehydrogenation: above-mentioned medicinal extract liquid is used the ydrogen peroxide 50 hydrolysis, and the weight ratio of ydrogen peroxide 50 and medicinal extract liquid is 15-25: 1, and preferred 20: 1, get aqueous hydrogen peroxide solution, concentrate and reclaim liquid, the gained liquid volume is the 1/6-1/10 of hydrogen peroxide solution;
Purifying: liquid concentrator adds triethylamine purifying extraction 2-5 hour, and extraction liquid is concentrated into saturated, and crystallization gets the pure article of gallogen.
After enzymolysis also concentrates in extraction step, can also liquid concentrator be added 2-5 times of 80% acetone and under 80 ℃ of conditions, be incubated 0.5-2 hour, continuous more than twice or twice, residue obtained liquid merges concentrated; Obtain medicinal extract liquid.
Said enzyme solution is a composite enzyme solution, and concentration is 0.1-0.5%.
Said prozyme is the mixture of cellulase and distiller's yeast, glycase, milk-acid bacteria; Cellulase and distiller's yeast, glycase, milk-acid bacteria are according to Mass Calculation, and ratio is 1: 0.1-2: 0.1-0.5: 0.1-1; Enzymolysis time is 0.5-10 hour, and hydrolysis temperature is 15-70 ℃, Ph value 4-6 during enzymolysis.
Said enzymolysis time 1-2 hour, hydrolysis temperature 40-50 ℃.Utilize accent Ph values such as common acid example hydrochloric acid acetic acid.
Remove special indicating among the present invention, be in mass mass parts, quality multiple, mass ratio, quality percentage composition etc.
Beneficial effect of the present invention is:
The present invention improves through repeatedly research on the work of summing up forefathers and the own basis of exploring, and adopts the raw material enzymolysis after the frying after carry out oxydehydrogenation after the hydrolysis extraction, extracts then; Present method is simple to operate; Avoided the strong acid and the solvent of acid hydrolyzation to use in a large number, avoided microbial method to produce the difficulty that cause the later separation purifying difficult, can carry out under the equipment situation such as UW, column chromatography not having a large amount of mycelium; Technology is simple; Three waste discharge is few, is fit to large-scale production, and quality product is fine.Temperature and time through the control heating; Under the situation that does not influence gallogen character; With pomegranate rind in advance after frying charcoal; Promote the glycosidic bond or the ester linkage breaking of hydrolysable tannin in the pomegranate rind, be increased in the follow-up hydrolytic process compositions such as free gallogen, the content and the extraction efficiency of relatively large increase gallogen.
Greatly improved production efficiency and transformation efficiency through method of the present invention, impelled the active substance in the raw material more to be extracted out, made quality product further improve, and product purity is high, is fit to suitability for industrialized production.
Embodiment
Further specify the present invention below in conjunction with embodiment, but not as to qualification of the present invention.
Embodiment 1
Said raw material be treated to the stir-fry charcoal: will clean through removing impurity, section is fried to the epidermis chocolate for 300 ℃ in the former medicinal heat pot of exsiccant pomegranate rind, and inner burnt brown is cut into slices or pulverized for use;
Extract: add 8 times water in the pomegranate rind section with stir-bake to brown, add 0.3 part of enzyme solution, soak at room temperature 2 hours; With both mixture heating up to 90 ℃, be incubated 2 hours then, continuous more than twice or twice; Residue obtained liquid; Merge to concentrate, the liquid concentrator weight ratio is medicinal extract liquid by raw material ratio 2: 1;
Oxydehydrogenation: above-mentioned medicinal extract liquid is used the ydrogen peroxide 50 hydrolysis, and the weight ratio of ydrogen peroxide 50 and medicinal extract liquid is 20: 1, gets aqueous hydrogen peroxide solution, concentrates to reclaim liquid, and the gained liquid volume is 1/8 of a hydrogen peroxide solution;
Purifying: liquid concentrator adds triethylamine purifying extraction 3 hours, and extraction liquid is concentrated into saturated, and crystallization gets the pure article of gallogen.
Said enzyme solution is a composite enzyme solution, and concentration is 0.2%.
Said ydrogen peroxide 50 is a reagent specification ydrogen peroxide 50, and concentration is 30% specification.This concentration is the quality percentage composition.
Embodiment 2
After enzymolysis also concentrates in extraction step, get 1 times of volume 80% acetone, with under 80 ℃ of conditions, being incubated 1 hour in 1 times of volume 80% acetone of liquid concentrator adding; Filter residue adds acetone in filter residue, be incubated once more and filter; And then repeat this process, carry out acetone extraction altogether three times; Residue obtained liquid merges concentrated; Obtain medicinal extract liquid.
Embodiment 3
Said raw material be treated to the stir-fry charcoal: will clean through removing impurity, section is fried to the epidermis chocolate for 200 ℃ in the former medicinal heat pot of exsiccant pomegranate rind, and inner burnt brown is cut into slices or pulverized for use;
Extract: add 5 times water in the pomegranate rind section with stir-bake to brown, add 0.1 part of enzyme solution, soak at room temperature 6 hours; With both mixture heating up to 100 ℃, be incubated 4 hours then, continuous more than twice or twice; Residue obtained liquid; Merge to concentrate, the liquid concentrator weight ratio is medicinal extract liquid by raw material ratio 3: 1;
Oxydehydrogenation: above-mentioned medicinal extract liquid is used the ydrogen peroxide 50 hydrolysis, and the weight ratio of ydrogen peroxide 50 and medicinal extract liquid is 20: 1, gets aqueous hydrogen peroxide solution, concentrates to reclaim liquid, and the gained liquid volume is 1/6 of a hydrogen peroxide solution;
Purifying: liquid concentrator adds triethylamine purifying extraction 5 hours, and extraction liquid is concentrated into saturated, and crystallization gets the pure article of gallogen.
Said enzyme solution is a composite enzyme solution, and concentration is 0.1%, and this concentration is the quality percentage composition.
Said prozyme is the mixture of cellulase and distiller's yeast, glycase, milk-acid bacteria; Cellulase and distiller's yeast, glycase, milk-acid bacteria are according to Mass Calculation, and ratio is 1: 0.1: 0.1: 0.1; Enzymolysis time is 10 hours, and hydrolysis temperature is 70 ℃, Ph value 6 during enzymolysis.
Embodiment 4
Said raw material be treated to the stir-fry charcoal: will clean through removing impurity, section is fried to the epidermis chocolate for 400 ℃ in the former medicinal heat pot of exsiccant pomegranate rind, and inner burnt brown is cut into slices or pulverized for use;
Extract: add 10 times water in the pomegranate rind section with stir-bake to brown, add 0.5 part of enzyme solution, soak at room temperature 0.5 hour is then with both mixture heating up to 80 ℃; Be incubated 1 hour, continuous more than twice or twice, residue obtained liquid; Merging concentrates, and the liquid concentrator weight ratio was pressed raw material ratio 1: 1, liquid concentrator is added 5 times of 80% acetone under 80 ℃ of conditions, be incubated 0.5 hour; Continuous 5 times, residue obtained liquid merges concentrated; Obtain medicinal extract liquid;
Oxydehydrogenation: above-mentioned medicinal extract liquid is used the ydrogen peroxide 50 hydrolysis, and the weight ratio of ydrogen peroxide 50 and medicinal extract liquid is 20: 1, gets aqueous hydrogen peroxide solution, concentrates to reclaim liquid, and the gained liquid volume is 1/10 of a hydrogen peroxide solution;
Purifying: liquid concentrator adds triethylamine purifying extraction 2 hours, and extraction liquid is concentrated into saturated, and crystallization gets the pure article of gallogen.
After enzymolysis also concentrates in extraction step, can also said enzyme solution be composite enzyme solution, concentration be 0.5%.
Said prozyme is the mixture of cellulase and distiller's yeast, glycase, milk-acid bacteria; Cellulase and distiller's yeast, glycase, milk-acid bacteria are according to Mass Calculation, and ratio is 1: 2: 0.5: 1; Enzymolysis time is 0.5 hour, and hydrolysis temperature is 15 ℃, Ph value 4 during enzymolysis.
Embodiment 5
Said enzyme solution is a composite enzyme solution, and consumption is 0.3 times of raw material, and concentration is counted 0.1-0.5% with the quality percentage composition.
Said prozyme is the mixture of cellulase and distiller's yeast, glycase, milk-acid bacteria; Cellulase and distiller's yeast, glycase, milk-acid bacteria are according to Mass Calculation, and ratio is 1: 1: 0.3: 0.5; Enzymolysis time is 4 hours, and hydrolysis temperature is 50 ℃, Ph value 5 during enzymolysis.All the other are with embodiment 1.
Embodiment 6-13
Said prozyme is the combination of the prozyme following table ratio of cellulase, glycase, proteolytic enzyme, lypase and N,O-Diacetylmuramidase; Hydrolysis temperature, enzymolysis time are also as shown in the table, and all the other are with embodiment 2.
Claims (6)
1. an enzymolysis process extracts the method for gallogen in pomegranate rind, it is characterized in that said technology is following: the processing of raw material, extract; Oxydehydrogenation; Purifying.
2. a kind of enzymolysis process as claimed in claim 1 extracts the method for gallogen in pomegranate rind; It is characterized in that, said raw material be treated to the stir-fry charcoal: will clean through removing impurity; Section; Fry to the epidermis chocolate for 200-400 ℃ in the former medicinal heat pot of exsiccant pomegranate rind, inner burnt brown is cut into slices or is pulverized for use;
Extract: add 5-10 water doubly in the pomegranate rind section with stir-bake to brown, add 0.1-0.5 part enzyme solution, soak at room temperature 0.5-6 hour; Then with both mixture heating up to 80-100 ℃, be incubated 1-4 hour, continuous more than twice or twice; Residue obtained liquid; Merging concentrates, and the liquid concentrator weight ratio is pressed raw material ratio 1-3: 1, be medicinal extract liquid;
Oxydehydrogenation: above-mentioned medicinal extract liquid is used the ydrogen peroxide 50 hydrolysis, and the weight ratio of ydrogen peroxide 50 and medicinal extract liquid is 15-25: 1, get aqueous hydrogen peroxide solution, and concentrate and reclaim liquid, the gained liquid volume is the 1/6-1/10 of hydrogen peroxide solution;
Purifying: liquid concentrator adds triethylamine purifying extraction 2-5 hour, and extraction liquid is concentrated into saturated, and crystallization gets the pure article of gallogen.
3. a kind of enzymolysis process as claimed in claim 2 extracts the method for gallogen in pomegranate rind; It is characterized in that: after enzymolysis also concentrates in extraction step; Liquid concentrator is added 2-5 times of 80% acetone under 80 ℃ of conditions, be incubated 0.5-2 hour; Continuous more than twice or twice, residue obtained liquid merges concentrated; Obtain medicinal extract liquid.
4. a kind of enzymolysis process as claimed in claim 2 extracts the method for gallogen in pomegranate rind, it is characterized in that: said enzyme solution is a composite enzyme solution, and concentration is 0.1-0.5%.
5. a kind of enzymolysis process as claimed in claim 4 extracts the method for gallogen in pomegranate rind, it is characterized in that: said prozyme is the mixture of cellulase and distiller's yeast, glycase, milk-acid bacteria; Cellulase and distiller's yeast, glycase, milk-acid bacteria are according to Mass Calculation, and ratio is 1: 0.1-2: 0.1-0.5: 0.1-1; Enzymolysis time is 0.5-10 hour, and hydrolysis temperature is 15-70 ℃, Ph value 4-6 during enzymolysis.
6. a kind of enzymolysis process as claimed in claim 5 extracts the method for gallogen in pomegranate rind, it is characterized in that: said enzymolysis time 1-2 hour, and hydrolysis temperature 40-50 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102861116A (en) * | 2012-10-18 | 2013-01-09 | 中国科学院新疆理化技术研究所 | Method for preparing pericarpium granati polyphenol gel for treating gynecological inflammation |
| CN113476362A (en) * | 2021-06-23 | 2021-10-08 | 植物医生(广东)生物科技有限公司 | Facial skin cutin renewal promoter and application thereof |
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| WO2006127832A2 (en) * | 2005-05-24 | 2006-11-30 | Pom Wonderful, Llc | Processes for extracting phytochemicals from pomegranate solids and compositions and methods of use thereof |
| CN101434608A (en) * | 2008-12-12 | 2009-05-20 | 桂林莱茵生物科技股份有限公司 | Preparation of high-purity ellagic acid |
| CN101481714A (en) * | 2008-01-11 | 2009-07-15 | 北京化工大学 | Method for preparing ellagic acid from pomegranate bark by enzyme process |
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2010
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| WO2006127832A2 (en) * | 2005-05-24 | 2006-11-30 | Pom Wonderful, Llc | Processes for extracting phytochemicals from pomegranate solids and compositions and methods of use thereof |
| CN101481714A (en) * | 2008-01-11 | 2009-07-15 | 北京化工大学 | Method for preparing ellagic acid from pomegranate bark by enzyme process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102861116A (en) * | 2012-10-18 | 2013-01-09 | 中国科学院新疆理化技术研究所 | Method for preparing pericarpium granati polyphenol gel for treating gynecological inflammation |
| WO2014059880A1 (en) * | 2012-10-18 | 2014-04-24 | 中国科学院新疆理化技术研究所 | Method for preparation of pomegranate-peel polyphenol gel used to treat gynecological inflammation |
| CN102861116B (en) * | 2012-10-18 | 2015-02-25 | 中国科学院新疆理化技术研究所 | Method for preparing pericarpium granati polyphenol gel for treating gynecological inflammation |
| EA029649B1 (en) * | 2012-10-18 | 2018-04-30 | Синьцзян Текникал Инститьют Оф Физикс Энд Кемистри, Чайниз Экэдеми Оф Сайенсиз | Pomegranate-peel polyphenol gel used to treat gynecological inflammation diseases and method for preparation thereof |
| CN113476362A (en) * | 2021-06-23 | 2021-10-08 | 植物医生(广东)生物科技有限公司 | Facial skin cutin renewal promoter and application thereof |
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Application publication date: 20120516 |