CN102432578B - Method for extracting proanthocyanidins from seabuckthorm seeds - Google Patents
Method for extracting proanthocyanidins from seabuckthorm seeds Download PDFInfo
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- CN102432578B CN102432578B CN201110367195.XA CN201110367195A CN102432578B CN 102432578 B CN102432578 B CN 102432578B CN 201110367195 A CN201110367195 A CN 201110367195A CN 102432578 B CN102432578 B CN 102432578B
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- seabuckthorm
- proanthocyanidins
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- pycnogenols
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to a method for extracting proanthocyanidins from seabuckthorm seeds. The method is characterized in that: seabuckthorm seed oil is extracted by employing a supercritical CO2 extraction technology, and seabuckthorm seed proanthocyanidins extract is extracted from seabuckthorm seed meal by employing an ultrasonic method, then the proanthocyanidins in the seabuckthorm seeds is extracted by using a microwave drying technology. The method for extracting the proanthocyanidins from the seabuckthorm seeds comprises the following steps of: extracting the seabuckthorm seed oil by employing the supercritical CO2 extraction technology to obtain the seabuckthorm seed meal; extracting the seabuckthorm seed meal by employing the ultrasonic method at low temperature to obtain a seabuckthorm seed proanthocyanidins ethanol extracting solution, and recovering the ethanol under a negative pressure at low temperature to obtain a proanthocyanidins water solution; and drying the proanthocyanidins water solution by employing vacuum microwave to obtain the seabuckthorm seed proanthocyanidins extract product. According to the method disclosed by the invention, the production process temperature is low, the product with high content of the proanthocyanidins and high quality and without solvent residues is obtained, and the demands of various proanthocyanidins healthcare products and medicament development are satisfied.
Description
Technical field
The present invention relates to the extracting method of proanthocyanidins from seabuckthorm seeds
Background technology
Pycnogenols is the general name of the large class polyphenolic substance extensively existed in vegetable kingdom.20 middle of century, French scientist Maas chief strangles and has first found pycnogenols.Through the research of nearly 50 years, the understanding of people to pycnogenols pharmacological action improved constantly.In recent years, a host of facts prove, pycnogenols is not only a kind of good antioxidant, and can regulate body essential biological pathway, participate in the many redox chain reaction process in basic vital process.Experiment confirms, oligomeric procyanidolics has direct or indirect prevention, therapeutic action to nearly hundred kinds of damages and disease, has extensive use in fields such as healthcare products, medicine and makeup.
In numerous plant, grape is unfailing research topic always, at present, is still that raw material extracts pycnogenols both at home and abroad with Semen Vitis viniferae.Research shows, seed of Fructus Hippophae is better pycnogenols source, because its extract contains more dimer, tripolymer, and the more single aggressiveness of dimer, tripolymer and polymer have stronger oxidation-resistance.Semen Vitis viniferae extract composition is pycnogenols, and monomer whose is catechin, and mean polymerisation degree is lower.And the chemical structure of seed of Fructus Hippophae pycnogenols is significantly different from grape pip procyanidin, be mainly Prodelphinidins (monomer is Gallate catechin), mean polymerisation degree is 12.8.The effect of seed of Fructus Hippophae pycnogenols inhibited oxidation is better than grape pip procyanidin.
Summary of the invention
Technical problem to be solved by this invention is that conbined usage CO_2 supercritical technology extracts Seabuckthorm Seed Oil, its seed dregs of rice adopt ultrasonic method to extract seed of Fructus Hippophae procyanidin extract, adopt the dry three technology of microwave drying technology to extract the method for the pycnogenols in sea-buckthorn seed cake.
For solving the problem, a kind of method extracting proanthocyanidins from seabuckthorm seeds of the present invention, comprises the steps:
1., after seed of Fructus Hippophae removal of impurities fragmentation, supercritical CO is adopted
2abstraction technique obtains the sea-buckthorn seed cake in low temperature (50 DEG C) production process after extracting Seabuckthorm Seed Oil, and no solvent residue.
2. adopted by sea-buckthorn seed cake ultrasonic method (50 DEG C) to extract, obtain seed of Fructus Hippophae pycnogenols ethanol extract.
3. negative pressure low temperature reclaims edible ethanol, obtains the pycnogenols aqueous solution.
4. adopt vacuum microwave namely to obtain seed of Fructus Hippophae procyanidin extract by after the drying of the pycnogenols aqueous solution, its procyanidin content can reach 50%.
The present invention compared with prior art has following advantage:
1, with extract by solvents Seabuckthorm Seed Oil, circumfluence method extracts the pycnogenols in sea-buckthorn seed cake, and spraying dry pycnogenols extracting solution and a few situation of resin absorption refining crude extract are compared, and the present invention is conbined usage supercritical CO
2abstraction technique, ultrasonic method extractive technique, vacuum microwave drying technology, its production process is carried out under being in lower temperature all the time, avoid the impact of high temperature on heat-sensitive substance pycnogenols as far as possible, meanwhile, supersound extraction and vacuum microwave drying not only carry out at low temperatures, also substantially reduce the time of production process, also considerably reduce the loss of pycnogenols.The inventive method, without resin absorption refining crude extract, has been evaded resin completely and may to have been come off the toxic action brought.The real no solvent residue of seed of Fructus Hippophae procyanidin extract, high-content, high-quality that the inventive method obtains.And application for a patent for invention number: the method for 200810176033.6 and " international sea-buckthorn research and development " September the 8th in 2010 volume the 3rd phase P11 page method, the seed of Fructus Hippophae procyanidin extract crude extract procyanidins content obtained, all about 30%, can only adopt resin refining its content of raising further again.Increase its production cost undoubtedly, also may occur the risk of toxicity that resin wear brings.
2, the present invention adopts vacuum microwave drying pycnogenols extracting solution, temperature low (less than 50 DEG C), time short (within 2 hours), and the quality product obtained is completely suitable with cryodesiccated quality.And the spraying dry of application for a patent for invention numbers 200810176033.6, because temperature is high, the pycnogenols of thermo-sensitivity will inevitably significantly sacrificing; And the cryodesiccated time (extracting liquid measure on an equal basis) is more than 20 times of the microwave drying time, its production cost is more than 2.7 times of microwave drying production cost.
Embodiment
Embodiment 1: a kind of method extracting proanthocyanidins from seabuckthorm seeds, comprises the steps:
1. supercritical CO is adopted
2extraction Seabuckthorm Seed Oil after sea-buckthorn seed cake 1kg, with 8L, 30% ethanolic soln at 30 DEG C, extract 3 times through ultrasonic method, 0.35 hour each extraction time.Merge No. three extracting solutions, obtain filtrate with 200 order filter-cloth filterings.Negative pressure low temperature reclaims edible ethanol, obtains the seed of Fructus Hippophae pycnogenols aqueous solution.
2. obtain powdery seed of Fructus Hippophae procyanidin extract product 82g after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted vacuum microwave cryodrying, its procyanidin content is 49.6%.
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to produce
2seed oil in extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45-50 DEG C, and extracting pressure is 26-32MPa, extraction time 2.5-3.5h.
Embodiment 2: a kind of method extracting proanthocyanidins from seabuckthorm seeds, comprises the steps:
1. supercritical CO is adopted
2extraction Seabuckthorm Seed Oil after sea-buckthorn seed cake 10kg, with 100L, 80% ethanolic soln at 50 DEG C, extract 2 times through ultrasonic method, 0.5 hour each extraction time.Merge secondary raffinate, obtain filtrate with 200 order filter-cloth filterings.Negative pressure low temperature reclaims edible ethanol, obtains the seed of Fructus Hippophae pycnogenols aqueous solution.
2. obtain powdery seed of Fructus Hippophae procyanidin extract product 0.95kg after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted vacuum microwave cryodrying, its procyanidin content is 50.6%.
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to produce
2seed oil in extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45-50 DEG C, and extracting pressure is 26-32MPa, extraction time 2.5-3.5h.
Accompanying drawing illustrates:
Accompanying drawing is process diagram of the present invention.
Claims (2)
1. extract a method for proanthocyanidins from seabuckthorm seeds, it is characterized in that: use supercritical CO
2abstraction technique extracts the Seabuckthorm Seed Oil in seed of Fructus Hippophae, then adopts ultrasonic method to extract pycnogenols in sea-buckthorn seed cake, then adopt vacuum microwave drying technology dry extract pycnogenols in sea-buckthorn seed cake;
Specifically comprise the steps:
1. supercritical CO is adopted
2extraction Seabuckthorm Seed Oil after sea-buckthorn seed cake 1kg, with 8L, 30% ethanolic soln at 30 DEG C, extract 3 times through ultrasonic method, 0.35 hour each extraction time, merge No. three extracting solutions, obtain filtrate with 200 order filter-cloth filterings, negative pressure low temperature reclaims edible ethanol, obtains the seed of Fructus Hippophae pycnogenols aqueous solution;
2. obtain powdery seed of Fructus Hippophae procyanidin extract product 82g after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted vacuum microwave cryodrying, its procyanidin content is 49.6%;
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to produce
2seed oil in extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45 ~ 50 DEG C, and extracting pressure is 26 ~ 32MPa, extraction time 2.5 ~ 3.5h.
2. extract a method for proanthocyanidins from seabuckthorm seeds, it is characterized in that: use supercritical CO
2abstraction technique extracts the Seabuckthorm Seed Oil in seed of Fructus Hippophae, then adopts ultrasonic method to extract pycnogenols in sea-buckthorn seed cake, then adopt vacuum microwave drying technology dry extract pycnogenols in sea-buckthorn seed cake;
Specifically comprise the steps:
1. supercritical CO is adopted
2extraction Seabuckthorm Seed Oil after sea-buckthorn seed cake 10kg, with 100L, 80% ethanolic soln at 50 DEG C, extract 2 times through ultrasonic method, 0.5 hour each extraction time, merge secondary raffinate, obtain filtrate with 200 order filter-cloth filterings, negative pressure low temperature reclaims edible ethanol, obtains the seed of Fructus Hippophae pycnogenols aqueous solution;
2. obtain powdery seed of Fructus Hippophae procyanidin extract product 0.95kg after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted vacuum microwave cryodrying, its procyanidin content is 50.6%;
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to produce
2seed oil in extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45 ~ 50 DEG C, and extracting pressure is 26 ~ 32MPa, extraction time 2.5 ~ 3.5h.
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| CN201110367195.XA CN102432578B (en) | 2011-11-18 | 2011-11-18 | Method for extracting proanthocyanidins from seabuckthorm seeds |
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| CN102432578B true CN102432578B (en) | 2015-06-10 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102755359B (en) * | 2012-07-19 | 2014-04-02 | 中国科学院研究生院 | Hippophae extract and preparation method and application thereof for inhibiting activity of fatty acid synthase |
| CN104997109B (en) * | 2015-08-06 | 2018-04-10 | 贵州三农楮桃产业开发有限公司 | Paper mulberry peach pulp rich in OPC and its preparation method and application |
| CN105440003B (en) * | 2016-01-12 | 2017-11-17 | 北京宝得瑞健康产业有限公司 | A kind of method of low temperature low-energy-consumption high-efficiency extraction proanthocyanidins from seabuckthorm seeds |
| CN109133272A (en) * | 2018-08-24 | 2019-01-04 | 青海清华博众生物技术有限公司 | A kind of purification process of plateau ecology hard water |
| CN109593075A (en) * | 2018-09-25 | 2019-04-09 | 宝得瑞（湖北）健康产业有限公司 | A kind of method that room temperature efficient high-pressure difference continous way extracts seabuckthorn seeds procyanidine |
Citations (7)
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| JPH08205818A (en) * | 1995-02-01 | 1996-08-13 | Nonogawa Shoji Kk | Health food and medicine formulated with procyanidin |
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| EP1388343A1 (en) * | 2002-08-09 | 2004-02-11 | Eromlife Co., Ltd. | Antioxidant composition and method of preparation thereof |
| CN101386615A (en) * | 2008-11-05 | 2009-03-18 | 中国科学院西北高原生物研究所 | Method for extracting procyanidine from sea-buckthorn seed |
| CN101496581A (en) * | 2008-02-03 | 2009-08-05 | 于珩 | Health-care food for adjusting blood fat |
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| CN101768621A (en) * | 2010-02-11 | 2010-07-07 | 青海康普生物科技股份有限公司 | Method for preparing sea-buckthorn enzymes from seabuckthorn fruit mud |
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| JPH08205818A (en) * | 1995-02-01 | 1996-08-13 | Nonogawa Shoji Kk | Health food and medicine formulated with procyanidin |
| JPH10218769A (en) * | 1997-02-06 | 1998-08-18 | Kikkoman Corp | Antiulcer agent |
| EP1388343A1 (en) * | 2002-08-09 | 2004-02-11 | Eromlife Co., Ltd. | Antioxidant composition and method of preparation thereof |
| CN101496581A (en) * | 2008-02-03 | 2009-08-05 | 于珩 | Health-care food for adjusting blood fat |
| CN101386615A (en) * | 2008-11-05 | 2009-03-18 | 中国科学院西北高原生物研究所 | Method for extracting procyanidine from sea-buckthorn seed |
| CN101701013A (en) * | 2009-11-05 | 2010-05-05 | 中国林业科学研究院林产化学工业研究所 | Method for extracting proanthocyanidin from pine bark by taking water as solvent |
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Owner name: MA YINGYUAN Effective date: 20120525 Owner name: BEIJING POWDERY FOOD CO., LTD. Free format text: FORMER OWNER: MA YINGYUAN Effective date: 20120525 |
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Free format text: CORRECT: ADDRESS; FROM: 100123 CHAOYANG, BEIJING TO: 101117 TONGZHOU, BEIJING |
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Effective date of registration: 20120525 Address after: 101117 Beijing City Lucheng town Tongzhou District City Industrial Zone No. 15 Applicant after: Beijing Powdery Food Co., Ltd. Co-applicant after: Ma Yingyuan Address before: 100123, room 1, unit 5, 102 middle building, Chaoyang District manna garden, Beijing Applicant before: Ma Yingyuan |
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