CN102048885B - Extraction process for lychee seed saponin - Google Patents
Extraction process for lychee seed saponin Download PDFInfo
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- CN102048885B CN102048885B CN2011100034945A CN201110003494A CN102048885B CN 102048885 B CN102048885 B CN 102048885B CN 2011100034945 A CN2011100034945 A CN 2011100034945A CN 201110003494 A CN201110003494 A CN 201110003494A CN 102048885 B CN102048885 B CN 102048885B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
- A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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Abstract
The invention discloses an extraction process for lychee seed saponin. The process comprises the following steps: 1) lychee seeds are pulverized, a certain amount of lychee seed powder is weighted and is soaked with water, and combinative enzyme reagent, which accounts for 1 to 2 percent of the weight of the lychee seed powder, is added in for enzymolysis treatment; 2) ethanol solution is added in for ultrasonic extraction, so as to obtain ultrasonic extracting solution; 3) filtering treatment and vacuum concentration treatment are conducted to the ultrasonic extracting solution, so as to obtain lychee seed saponin coarse extractive; and 4) macroporous adsorption resin is adopted to sublimate the lychee seed saponin coarse extractive, so as to obtain the lychee seed saponin. In the process, cell walls are softened and degraded through enzymes; with the combination of ultrasonic cavitation, the cell walls are fully destroyed, and the dissolution of active ingredients is accelerated and increased; and through the nonpolar macroporous adsorption resin, saponin ingredients of the lychee seeds are concentrated and separated, so as to prepare the high-content lychee seed saponin. The process has the advantages of time and labor conservation, lower cost and the like.
Description
Technical field
The present invention relates to a kind of Semen Litchi saponin extraction process, belong to the Chinese medicine extraction technical field.
Background technology
Semen Litchi (Lychee Seed, Litchi Seed), another name Li Ren, litchi nuclear, Dali nuclear are the dry mature seed of sapindaceous plant Fructus Litchi (Litchi Chinensis Sonn), warm in nature, it is little sweet, bitter, puckery, nontoxic to distinguish the flavor of.Compendium of Material Medica record, Semen Litchi " quench the thirst, beneficial people's color, food end excessive thirst " (excessive thirst disease, modern medicine is called diabetes).Research shows that Semen Litchi has blood sugar lowering, blood lipid regulation, raising antioxidation, suppresses the effect of HBsAg.Experimentation and clinical treatment show Semen Litchi extract blood sugar lowering significantly, effectively treat diabetes.Make full use of Semen Litchi, further the medicine of diabetes is treated in exploitation, and increasing for diabetics, demand is treated diabetes medicament in a large number and had great social significance.
The main component of Semen Litchi has chemical constituents such as saponin, steroid compound, flavone compound, fatty acid, aminoacid, protein and sugar.Research confirms that the Semen Litchi saponin is the effective ingredient of treatment diabetes.Therefore, fully develop Semen Litchi, improve Semen Litchi saponin extraction ratio, have important economic benefit.
At present, Semen Litchi component separating preparation technology mainly adopts water extract-alcohol precipitation and solvent extraction method, and decoction and alcohol sedimentation technique is consuming time, extraction ratio is low; Solvent extraction method needs a large amount of solvents, and extract is impure many.These extraction processes are not high to the saponin extraction efficiency.The present invention is intended to the deficiency to existing Semen Litchi chemical constituent extraction process, and the process that a kind of extraction ratio is high, saponin is simply extracted in technological process from Semen Litchi is provided.
Summary of the invention
The object of the present invention is to provide a kind of Semen Litchi saponin extraction process.This technology in conjunction with ultransonic cavitation, is fully destroyed cell wall through enzyme bating degradation of cell wall; Quicken and increase the stripping of active component; Through nonpolar macroporous adsorbent resin,, prepare high-load Semen Litchi saponin to the saponin constituent concentration and separation of Semen Litchi.This technology have save time, advantage such as laborsaving and province's expense.
The objective of the invention is to realize through following technical scheme:
A kind of Semen Litchi saponin extraction process may further comprise the steps:
1) Semen Litchi is pulverized, taken by weighing a certain amount of Lychee Seed and add water infiltration, the combination enzyme reagent that adds weight then and be Lychee Seed weight 1/100～1/50 carries out enzymolysis processing;
2) add alcoholic solution and carry out supersound extraction, obtain supersound extraction liquid;
3) supersound extraction liquid is filtered and the concentrating under reduced pressure processing, obtain Semen Litchi saponin crude extract;
4) adopt macroporous adsorbent resin that Semen Litchi saponin crude extract is carried out purification, obtain described Semen Litchi saponin.
In the present invention, described combination enzyme reagent is selected from two or more the combination in cellulase, hemicellulase, pectase, glucanase and the papain.
In above-mentioned step 1), when adding the water infiltration processing, amount of water is 2～6 times of Lychee Seed weight, and the time that adds water infiltration is 5～30min.
In above-mentioned step 1), when carrying out enzymolysis processing, hydrolysis temperature is controlled at 30 ℃～50 ℃, and enzymolysis time is 1～3 hour.
In above-mentioned step 2) in, the concentration of alcoholic solution is 50%～70% (percent by volume), the consumption of alcoholic solution is 2～3 times of Lychee Seed weight.
In above-mentioned step 2) in, when carrying out supersound extraction, supersonic frequency is controlled at 20KHz～50KHz, and the time of supersound extraction is 20～40min.
In above-mentioned step 4), when adopting macroporous adsorbent resin to carry out purification, adopting concentration is that the alcoholic solution of 50%～80% (percent by volume) is as eluent; It is the macroporous adsorbent resin of AB-8, D201, D101, X-5 that said macroporous adsorbent resin adopts model.
The present invention only needs a spot of solvent through combination enzyme reagent enzymolysis processing and ultrasonic cavitation, and the effective ingredient of Semen Litchi is leached fast, has advantages such as extraction ratio height, solvent-oil ratio are few; Through the eluting of macroporous adsorbent resin, can remove a large amount of impurity, enrichment saponin content.Compare with decoction and alcohol sedimentation technique, technology of the present invention extraction time minimizing, extraction ratio increases; Compare with solvent extraction method, technology of the present invention reduces at the solvent-oil ratio of unit medical material, and extraction time reduces, and extraction ratio increases.Adopt technology of the present invention to extract the Semen Litchi effective ingredient, extraction ratio is up to 9.05%, and the Semen Litchi saponin content is up to 85.0%.This shows that technology of the present invention is used for the extraction of Semen Litchi saponin, have the extraction efficiency height, save time and remarkable advantage such as solvent.
The specific embodiment
Embodiment one:
Semen Litchi is pulverized, and granule size is 20～30 orders.Get 50g Semen Litchi powder, add 150ml water (be equivalent to Lychee Seed weight 3 times) and soak into 10min, take by weighing 0.5g cellulase, 0.5g pectase and 0.5g glucanase and add wherein, abundant mixing, 50 ℃ of control temperature, enzymolysis processing 3 hours.The alcoholic solution that adds 150ml 70% then is to extract 40min under the condition of 20KHz in supersonic frequency.With extracting liquid filtering and concentrating under reduced pressure, get Semen Litchi saponin crude extract 4.53g.Through macroporous adsorptive resins, 3 column volumes of the alcoholic solution eluting with 70% get Semen Litchi saponin 3.85g with Semen Litchi saponin crude extract.Through measuring, the Semen Litchi saponin content is 85.0%.
Embodiment two:
Semen Litchi is pulverized, and granule size is 20～30 orders.Get 50g Semen Litchi powder, add 150ml water infiltration 5min, take by weighing 0.5g cellulase and 0.5g pectase and add wherein, fully mixing is controlled 50 ℃ of temperature, enzymolysis processing 3 hours.The alcoholic solution that adds 150ml 70% then is to extract 40min under the condition of 20KHz in supersonic frequency.With extracting liquid filtering and concentrating under reduced pressure, get Semen Litchi saponin crude extract 4.20g.Through macroporous adsorptive resins, 3 column volumes of the alcoholic solution eluting with 70% get Semen Litchi saponin 3.55g with Semen Litchi saponin crude extract.Through measuring, the Semen Litchi saponin content is 83.5%.
Embodiment three:
Semen Litchi is pulverized, and granule size is 10～20 orders.Get 50g Semen Litchi powder, add 150ml water infiltration 10min, take by weighing 0.5g cellulase and 0.5g glucanase and add wherein, fully mixing is controlled 50 ℃ of temperature, enzymolysis processing 3 hours.The alcoholic solution that adds 150ml 70% then is to extract 40min under the condition of 20KHz in supersonic frequency.With extracting liquid filtering and concentrating under reduced pressure, get Semen Litchi saponin crude extract 4.03g.Through macroporous adsorptive resins, 3 column volumes of the alcoholic solution eluting with 70% get Semen Litchi saponin 3.48g with Semen Litchi saponin crude extract.Through measuring, the Semen Litchi saponin content is 83.9%.
Embodiment four:
Semen Litchi is pulverized, and granule size is 10～20 orders.Get 50g Semen Litchi powder, add 150ml water infiltration 10min, take by weighing 0.5g pectase and 0.5g glucanase and add wherein, fully mixing is controlled 30 ℃ of temperature, enzymolysis processing 2 hours.The alcoholic solution that adds 150ml 50% then is to extract 40min under the condition of 50KHz in supersonic frequency.With extracting liquid filtering and concentrating under reduced pressure, get Semen Litchi saponin crude extract 3.83g.Through macroporous adsorptive resins, 3 column volumes of the alcoholic solution eluting with 70% get Semen Litchi saponin 3.05g with Semen Litchi saponin crude extract.Through measuring, the Semen Litchi saponin content is 82.6%.
Embodiment five:
Semen Litchi is pulverized, and granule size is 10～20 orders.Get 50g Semen Litchi powder, add 100ml water infiltration 5min, take by weighing 0.5g cellulase, 0.5g pectase and 0.5g glucanase and add wherein, fully mixing is controlled 30 ℃ of temperature, enzymolysis processing 1 hour.The alcoholic solution that adds 100ml 50% then is to extract 20min under the condition of 20KHz in supersonic frequency.With extracting liquid filtering and concentrating under reduced pressure, get Semen Litchi saponin crude extract 4.23g.Through macroporous adsorptive resins, 3 column volumes of the alcoholic solution eluting with 70% get Semen Litchi saponin 3.20g with Semen Litchi saponin crude extract.Through measuring, the Semen Litchi saponin content is 84.5%.
Claims (7)
1. Semen Litchi saponin extraction process may further comprise the steps:
1) Semen Litchi is pulverized, taken by weighing a certain amount of Lychee Seed and add water infiltration, the combination enzyme reagent that adds weight then and be Lychee Seed weight 1/100～1/50 carries out enzymolysis processing;
2) add alcoholic solution and carry out supersound extraction, obtain supersound extraction liquid;
3) supersound extraction liquid is filtered and the concentrating under reduced pressure processing, obtain Semen Litchi saponin crude extract;
4) adopt macroporous adsorbent resin that Semen Litchi saponin crude extract is carried out purification, obtain described Semen Litchi saponin;
Wherein, described combination enzyme reagent is selected from two or more the combination in cellulase, pectase and the glucanase.
2. Semen Litchi saponin extraction process according to claim 1 is characterized in that: in step 1), when adding the water infiltration processing, amount of water is 2～6 times of Lychee Seed weight, and the time that adds water infiltration is 5～30min.
3. Semen Litchi saponin extraction process according to claim 1 is characterized in that: in step 1), when carrying out enzymolysis processing, hydrolysis temperature is controlled at 30 ℃～50 ℃, and enzymolysis time is 1～3 hour.
4. Semen Litchi saponin extraction process according to claim 1 is characterized in that: in step 2) in, the concentration of said alcoholic solution is 50%～70%, the consumption of said alcoholic solution is 2～3 times of Lychee Seed weight.
5. Semen Litchi saponin extraction process according to claim 1 is characterized in that: in step 2) in, when carrying out supersound extraction, supersonic frequency is controlled at 20KHz～50KHz, and the time of supersound extraction is 20～40min.
6. Semen Litchi saponin extraction process according to claim 1 is characterized in that: in step 4), when adopting macroporous adsorbent resin to carry out purification, adopting concentration is that 50%～80% alcoholic solution is as eluent.
7. Semen Litchi saponin extraction process according to claim 1 is characterized in that: it is the macroporous adsorbent resin of AB-8, D201, D101, X-5 that said macroporous adsorbent resin adopts model.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100034945A CN102048885B (en) | 2011-01-10 | 2011-01-10 | Extraction process for lychee seed saponin |
| PCT/CN2011/071992 WO2012094849A1 (en) | 2011-01-10 | 2011-03-21 | A process for extracting lychee seed saponins |
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| CN2011100034945A CN102048885B (en) | 2011-01-10 | 2011-01-10 | Extraction process for lychee seed saponin |
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| CN102048885B true CN102048885B (en) | 2012-01-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102836265A (en) * | 2012-09-24 | 2012-12-26 | 广州市中医医院 | Litchi seed dropping pill and preparation method thereof |
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| CN102204985A (en) * | 2011-06-10 | 2011-10-05 | 广东省农业科学院蚕业与农产品加工研究所 | Compound lychee seed hpyerglycemic particles and preparation method thereof |
| CN102499434B (en) * | 2011-10-31 | 2014-03-26 | 广东中烟工业有限责任公司 | Preparation method for litchi pericarp extract and application of same in production of cigarette |
| CN102526315B (en) * | 2012-01-13 | 2013-04-24 | 广州市中医医院 | Preparation method of extracts of effective fractions of lychee seeds |
| CN103638177A (en) * | 2013-06-30 | 2014-03-19 | 金玛瑙香水（明光）有限公司 | Extraction process of lychee seed saponin |
| DE102013114572A1 (en) | 2013-12-19 | 2015-06-25 | Leibniz-Institut Für Neue Materialien Gemeinnützige Gmbh | Process for producing structured metallic coatings |
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| CN108338359B (en) * | 2018-06-25 | 2018-09-11 | 上海欣百诺生物科技有限公司 | The production technology and application thereof of Stigma Maydis total saponins highly finished product |
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| CN1660172A (en) * | 2004-02-23 | 2005-08-31 | 广西师范大学 | New drug for treating hepatitis B virus and preparing method |
| CN100391495C (en) * | 2005-09-01 | 2008-06-04 | 桂林莱茵生物科技股份有限公司 | Process for extracting litchi polyphenol from litchi |
| WO2007124102A2 (en) * | 2006-04-21 | 2007-11-01 | Western Holdings, Llc | Preparation and use of phlorizin compositions |
| CN101440118B (en) * | 2008-12-26 | 2011-03-30 | 广西壮族自治区中国科学院广西植物研究所 | Saponin compound extracted from Momordica grosvenori root, preparation and use thereof |
| CN101889709B (en) * | 2010-08-17 | 2012-06-06 | 济南康森生物科技有限公司 | Wild jujube juice beverage for tranquilization and health care and production method thereof |
| CN102028165A (en) * | 2010-12-15 | 2011-04-27 | 吴剑生 | Method for processing lychee seeds |
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| CN102836265A (en) * | 2012-09-24 | 2012-12-26 | 广州市中医医院 | Litchi seed dropping pill and preparation method thereof |
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