CN102453038A - Method for extracting ellagic acid from pomegranate peels - Google Patents
Method for extracting ellagic acid from pomegranate peels Download PDFInfo
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- CN102453038A CN102453038A CN2010105294338A CN201010529433A CN102453038A CN 102453038 A CN102453038 A CN 102453038A CN 2010105294338 A CN2010105294338 A CN 2010105294338A CN 201010529433 A CN201010529433 A CN 201010529433A CN 102453038 A CN102453038 A CN 102453038A
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Abstract
The invention relates to the field of drug preparation, in particular a method for extracting ellagic acid from pomegranate peels, solving the problems existing in the prior art that the conversion rate is lower, and the yield is low and the product quality is bad. The process is as follows: treatment on raw materials; extraction; oxidative dehydrogenation; purification. The method disclosed by the invention largely raises the production efficiency and the conversion rate, and makes effective substances in the raw materials more converted into ellagic acid, and further raises the product quality and purity, and is suitable for industrialized 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
Reference: 200810056007.x; 200510002081.x; Cn101701234A; CN101768165; CN101747388A.
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) extract;
(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 3-10 water doubly in the pomegranate rind section with stir-bake to brown, 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 merges concentrated; 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.
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.
Remove special indicating among the present invention, be in mass mass parts, quality multiple, mass ratio, quality percentage composition etc.
The section of raw material is generally cut into slices to process the sheet that thickness is 0.1-5mm, pulverizes to processing the raw material powder about 80 orders.
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 employing is fried the extraction that is hydrolyzed behind the charcoal with raw material, and purifying gets final product after the oxydehydrogenation then.Greatly improved production efficiency and transformation efficiency through method of the present invention, impelled the active substance in the raw material more to be converted into trans gallogen, made quality product further improve, and product purity is high, is fit to suitability for industrialized production.
Present method is simple to operate; Avoided the strong acid and the solvent of acid hydrolyzation to use (200510002081.X) 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.
Utilize present method to prepare gallogen, compared with prior art, output can improve more than 20%.
Embodiment
Further specify the present invention below in conjunction with embodiment, but not as to qualification of the present invention.
Embodiment 1
The processing of raw material; Fry charcoal: will clean through removal impurity, section, exsiccant pomegranate rind crude drug is fried to the epidermis chocolate with heat pot interior 300, inner burnt brown, it is for use to cut into slices.
Section is for processing the sheet that thickness is 2mm.
Extract: in mass, in the raw material of handling, add 3 times tap water, soak at room temperature 3 hours; With both mixture heating up to 90 ℃, be incubated 2 hours, continuous twice then; Residue obtained liquid adds 80 ℃ of extractions of 8 times of 80% acetone then, and merging filtrate concentrates.
In mass, the proportion of extraction back liquid concentrator and raw material ratio are 1: 1.
Oxydehydrogenation: add the ydrogen peroxide 50 hydrolysis in the liquid concentrator, the proportion of ydrogen peroxide 50 and medicinal extract is 20: 1, and the time is 30 minutes, and filtered and recycled ydrogen peroxide 50 liquid concentrates and reclaims liquid, to about 1/8 of ydrogen peroxide 50 medicinal extract solution.
Purifying: liquid concentrator adds triethylamine purifying extraction 3 hours, and extraction liquid is concentrated into saturated, and crystallization gets product of the present invention.
Embodiment 2
The processing of raw material; Fry charcoal: will clean through removing impurity, section, exsiccant pomegranate rind crude drug is fried to the epidermis chocolate for interior 200 ℃ with the heat pot, and inner burnt brown is cut into slices or is pulverized for use.
Pulverize to processing the raw material powder about 80 orders.
Extract: in mass, in the raw material of handling, add 3 times tap water, soak at room temperature 6 hours with both mixture heating up to 80 ℃, is incubated 4 hours then, and continuous 3 times, residue obtained liquid, merging is concentrated.
In mass, the proportion of extraction back liquid concentrator and raw material ratio are 1: 1.
Oxydehydrogenation: add the ydrogen peroxide 50 hydrolysis in the medicinal extract liquid, the proportion of ydrogen peroxide 50 and medicinal extract is 20: 1, and the time is 5 minutes, and filtered and recycled ydrogen peroxide 50 liquid concentrates and reclaims liquid, to about 1/8 of ydrogen peroxide 50 medicinal extract solution.
Purifying: liquid concentrator adds triethylamine purifying extraction 2 hours, and extraction liquid is concentrated into saturated, and crystallization gets product of the present invention.
Embodiment 3
The processing of raw material; Fry charcoal: will clean through removing impurity, section, exsiccant pomegranate rind crude drug is fried to the epidermis chocolate for interior 400 ℃ with the heat pot, and inner burnt brown is cut into slices or is pulverized for use.
Section is for processing the sheet that thickness is 1mm.
Extract: in mass, the tap water of 10 times of addings in the raw material of handling, soak at room temperature 0.5 hour is then with both mixture heating up to 100 ℃; Be incubated 4 hours, continuous 4 times, residue obtained liquid; In filtrating, add 80 ℃ of extractions of 5 times of 80% acetone, united extraction liquid also concentrates
In mass, the proportion of extraction back liquid concentrator and raw material ratio are 1: 1.
Oxydehydrogenation: add the ydrogen peroxide 50 hydrolysis in the medicinal extract liquid, the proportion of ydrogen peroxide 50 and medicinal extract is 20: 1, and the time is 5 minutes, and filtered and recycled ydrogen peroxide 50 liquid concentrates and reclaims liquid, to about 1/8 of ydrogen peroxide 50 medicinal extract solution.
Purifying: liquid concentrator adds triethylamine purifying extraction 5 hours, and extraction liquid is concentrated into saturated, and crystallization gets product of the present invention.
Claims (3)
1. the process for extracting of gallogen in the pomegranate rind is characterized in that, adopts following process step:
1) processing of raw material;
2) extract;
3) oxydehydrogenation;
4) 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 3-10 water doubly in the pomegranate rind section with stir-bake to brown, 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 merges concentrated; 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010105294338A CN102453038A (en) | 2010-11-03 | 2010-11-03 | Method for extracting ellagic acid from pomegranate peels |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105294338A CN102453038A (en) | 2010-11-03 | 2010-11-03 | Method for extracting ellagic acid from pomegranate peels |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103505480A (en) * | 2012-06-21 | 2014-01-15 | 新疆医科大学 | Punica granatum peel antitumor polyphenol effective part, its preparation method and application |
| CN104341431A (en) * | 2014-09-30 | 2015-02-11 | 桂林三宝生物科技有限公司 | Method for extracting ellagic acid from pomegranate peel |
| CN106124684A (en) * | 2016-06-02 | 2016-11-16 | 浙江金大康动物保健品有限公司 | A kind of qualitative and quantitative detection method of Pericarpium Granati ZHIXIE SAN |
| CN110292592A (en) * | 2012-09-21 | 2019-10-01 | 雀巢产品有限公司 | Plant phenols and its purposes in treatment or prevention eosinophilic esophagitis |
| CN114533750B (en) * | 2022-01-04 | 2023-10-20 | 广东工业大学 | Application of pericarpium Granati tannin in preparing medicine for treating enterotoxigenic escherichia coli intestinal diseases |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803801A (en) * | 2005-01-14 | 2006-07-19 | 北京化工大学 | Method for preparing ellagic acid by pomegranate rind |
| 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 |
-
2010
- 2010-11-03 CN CN2010105294338A patent/CN102453038A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803801A (en) * | 2005-01-14 | 2006-07-19 | 北京化工大学 | Method for preparing ellagic acid by pomegranate rind |
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
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| 李海霞，等: "石榴皮中鞣花酸的提取工艺研究", 《中国医药导报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103505480A (en) * | 2012-06-21 | 2014-01-15 | 新疆医科大学 | Punica granatum peel antitumor polyphenol effective part, its preparation method and application |
| CN110292592A (en) * | 2012-09-21 | 2019-10-01 | 雀巢产品有限公司 | Plant phenols and its purposes in treatment or prevention eosinophilic esophagitis |
| US11382891B2 (en) | 2012-09-21 | 2022-07-12 | Societe Des Produits Nestle S.A. | Plant phenols and their use in the treatment or prevention of eosinophilic esophagitis |
| CN104341431A (en) * | 2014-09-30 | 2015-02-11 | 桂林三宝生物科技有限公司 | Method for extracting ellagic acid from pomegranate peel |
| CN106124684A (en) * | 2016-06-02 | 2016-11-16 | 浙江金大康动物保健品有限公司 | A kind of qualitative and quantitative detection method of Pericarpium Granati ZHIXIE SAN |
| CN114533750B (en) * | 2022-01-04 | 2023-10-20 | 广东工业大学 | Application of pericarpium Granati tannin in preparing medicine for treating enterotoxigenic escherichia coli intestinal diseases |
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Application publication date: 20120516 |