CN101070334A - Process for separating tea sapogenin and tea polysaccharide from tea-oil cake - Google Patents
Process for separating tea sapogenin and tea polysaccharide from tea-oil cake Download PDFInfo
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- CN101070334A CN101070334A CN 200710042332 CN200710042332A CN101070334A CN 101070334 A CN101070334 A CN 101070334A CN 200710042332 CN200710042332 CN 200710042332 CN 200710042332 A CN200710042332 A CN 200710042332A CN 101070334 A CN101070334 A CN 101070334A
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Abstract
This invention relates to a method of taking tea oil residue as raw material to extract tea saponin and tea polyose. The preparation process includes: preparation of extract, dissolution of normal butyl alcohol and separating of solid; solid once again dissolve in higher temperature anhydrous normal butyl alcohol, cooling, filtration, gain tea saponin; reclaim normal butyl alcohol solution, gain hybrid containing tea polyose; add hydrous ethanol to the hybrid, the insoluble substance is tea polyose product. This invention has merits of simple craft, low cost and high yield, and low environmental pollution. The product purity is high , tea saponin is white, tea polyose is white.
Description
Technical field
The invention belongs to the food and medicine technical field, be specifically related to the separation method of a kind of tea saponin and tea polysaccharide.
Background technology
Scientific research has been found that vegetable polysaccharides has special physiologically active, and for example: heparin has anticoagulant effect, flows aching and limp ossein and can prevent arteriosclerosis; Lentinan, Pachymose, ganoderan all have significant anti-cancer activity.Tea polysaccharide mainly is made up of glucose, pectinose, wood sugar, Fucose, ribose, semi-lactosi etc.Modern medicine study shows, the main pharmaceutical component when tea polysaccharide is tealeaves treatment diabetes, and its main pharmacological has following several aspect:
(1) hypoglycemic activity.
Diabetes are to continue the syndrome of hyperglycemia for its basic biochemical character.A variety of causes causes the under-supply or Regular Insulin of the Regular Insulin physiological action of can't bringing into normal play, and makes that sugar, protein and metabolism of fat get muddled in the body, and sugared concentration rises in the blood, and diabetes have just taken place.Oral or abdominal injection tea polysaccharide has blood sugar decreasing effect, and this effect is being thrown to appearance in back about 10 hours.Blood sugar decreasing effect disappears after 24 hours.Tea polysaccharide is together used with promoting the insulin secretion medicine, can strengthen the blood sugar decreasing effect of medicine.Make tea with the warm water that is lower than 50 degree, tea polysaccharide content is higher in the millet paste, to hypoglycemic effective.
(2) reducing blood lipid.
Feed tea polysaccharide to mouse, total cholesterol in the blood, neutral fat, low density lipoprotein cholesterol isoconcentration are descended, high density lipoprotein cholesterol can both increase.Tea polysaccharide can play prevention hyperlipidemia, arteriosclerotic effect by regulating cholesterol and the fatty concentration in the blood.
(3) radiation resistance.
Tea polysaccharide has the effect of tangible radioresistance injury, hemopoietic function protecting.Mouse is taken tea polysaccharide and can keep hemochrome steady by behind the radiation exposure, and the red blood corpuscle fall reduces, and it is normal that hematoblastic variation is tending towards.Along with development of science and technology, a large amount of electrical equipment enter family, and the time of people's contact electricity magnetic radiation is more and more, the harm of drinking tea more and can prevent radiation long-time, low dosage that human body is caused.In addition, tea polysaccharide also has raise immunity, anticoagulation, antithrombotic, function such as hypotensive.
Tea saponin can have the application of following 8 aspects; (1) because of having the dual-use function of defending the doctrine of having one's hair wash, washing back gloss, feel and combing etc. are good, and, sensitization non-stimulated to skin, tea saponin are used to produce tea saponin wash the reason shampoo; (2) tea saponin as not only can have one's hair wash, but also one of the clean raw material of tea saponin bathing that can bathing; (3) natural sex of tea saponin and to the non-invasi of protein fibre class makes it to become to the New-type detergent raw material of sending out, washings such as hair, silk, eider down have obvious superiority; (4) tea saponin has stronger absorption CO2 characteristic because of it, and as the foaming aids of refreshment drink and beer production; (5) because of the selectivity haematolysis property of tea saponin as the prawn culturing protective material; (6), increase secretion, and use it for the medicine that exploitation has the expelling phlegm for arresting cough effect because of tea saponin can stimulate tunica mucosa bronchiorum; (7) because of the special efficacy of tea saponin to treatment all kinds edema disease, and as the exploitation raw material of this kind new medicine; (8) with tea saponin as the emulsifying agent of diuretic(s), fish liver oil emulsion etc.
As from the foregoing, tea saponin can be used for making products such as various types of emulsifying agents, washing composition, sanitas, sterilant or sterilant, be that to have the natural surface active agent of DEVELOPMENT PROSPECT in current household chemicals, cosmetic skin care, medicine and the food service industry present, following patent arranged for the separation of tea saponin:
CN1038427 the present invention is a kind of grease and tea saponin processing method extracted from oil tea or tea waste.The present invention proposes with single moisture lower alcohol and make solvent, adopt the gradient leaching method, a step is extracted grease and the tea saponin in the grouts.Present method technology is simple, and facility investment is few, and extraction efficiency is high and stable, and extracting solvent reclaims and recycles conveniently.Present method can obtain three kinds of products of the residual dregs of rice of tea oil, tea saponin and detoxification, makes grouts obtain comprehensive utilization.Shortcoming of the present invention: because used moisture lower alcohol to make solvent, contain pectin and tea sugar in the tea saponin, therefore, purity is not high.
Application number 93107839 the present invention relates to a kind of solvent extracts tea saponin from the tea bran method that uses water as.Earlier tea bran raw material is inserted in the closed container, make the pressure in the container to 0.2-1.2MPa, stop heating, take out in the processing tea bran input lixiviate container and use water as the solvent lixiviate, extract tea saponin from the gained vat liquor by heating.The facility investment of employing present method is little, production cost is low, the pure height of product, the extraction yield of tea saponin can reach 45-90%, particularly solved and in industrial production, to have used water as solvent extracts tea saponin from the tea bran a difficult problem for a long time, be suitable for tea saponin manufacturer and carry out industrial production.Shortcoming of the present invention: because used water as solvent, contain pectin and tea sugar in the tea saponin, therefore, purity is not high; When concentrating in addition, the equipment funds height that needs; The energy height that consumes.
It is raw material with the tea cake that application number 95113044 the present invention relates to a kind of, handles tea cake leaching liquid with domestic resin, thereby makes the method for refined theasapogenin.This method adopts the tea saponin in the styrene type copolymer resins absorption tea cake leaching liquid, remove pigment and the impurity that is adsorbed with the organic or inorganic alkali aqueous solution, with moisture low-carbon alcohol is elutriant, the underpressure distillation elutriant reclaims alcohol, residue is concentrated oven dry, can obtain purity and be the solid tea saponin more than 98%.The tea saponin purity height that this method is produced, quality is good, and cost is low, for the application of the tea saponin that enlarges natural surface active agent provides wide prospect, can be used for fields such as medicine, food, daily use chemicals and biochemical reagents.Shortcoming of the present invention: because of the tea saponin that has used in the styrene type copolymer resins absorption tea cake leaching liquid, complex process, production cost height; The market value of tea saponin is low, lacks the commercial competition advantage.
Application number 98107566 invention proposed a kind of with Camellia fruit or seed extract grouts behind the vegetables oil or seed, pericarp, shell is a raw material, employing contains or does not contain 1～3 carbon monohydroxy-alcohol lixiviate raw materials such as the methyl alcohol, ethanol, propyl alcohol of mineral acid, alkali, salt, vat liquor is through concentrating evaporate to dryness or near doing, and operations such as that water changes is molten, monohydroxy-alcohol extraction, precipitation and drying prepare the new process of tea saponin.Belong to farming, secondary product of forestry deep processing field.Compare with existing tea saponin extracting method, the present invention has that technology is simple, cost is low, pollution is little, system rate height, commodity purity is good, color and luster is more shallow, be suitable for industrial advantage.Can produce the tea saponin pulvis or the liquor that are fit to different needs.The present invention's technology really is simple, but the extraction of tea saponin, and it can further be simplified.
Application number 99115525 usefulness propyl carbinols extract the technology of tea saponin from CHAKUBING, its step comprises: will add propyl carbinol in the CHAKUBING and heat and carry out 4 lixiviates; Vat liquor is distilled under decompression state to reclaim propyl carbinol; In still kettle, add an amount of water and lipase, be incubated, stirring operation, leave standstill the clarification after-filtration, to remove Residual oil with lipase; Adopt No. 6 gasoline vapour to wash tea saponin, remove impurity; Tea saponin drying after the washing, pulverizing, pack finished product.Can be with the tea saponin purity that this technology makes up to more than 80%, the propyl carbinol recyclability is good simultaneously, has reduced product cost.Propyl carbinol is nonflammable, and is to the healthy nothing influence of humans and animals, safe.Nutritive ingredients such as protein, carbohydrate keep fully in the tea dregs of rice after the lixiviate, are easy to be processed into high protein feed etc.Shortcoming of the present invention: the present invention uses gasoline vapour to wash tea saponin, and its security is not high.
The preparation method of application number 01113794 tea saponin is a kind ofly to extract the method for tea saponin with chemical process from the tea-seed dregs of rice, and the method for extraction is: (1) was with leached tea oil slag bubble under water 24～48 hours; (2) heated and boiled stirs simultaneously; (3) filter undissolved impurity, and wash this undissolved impurity 1-5 time with boiling water; (4) add yeast in solution, the vibration fermentation is 24～72 hours under 25-32 ℃ of temperature; (5) remove impurity with the method for centrifugation, obtain clear liquid; (6) in above-mentioned clear liquid, add 3 times ethanol, stirred 15 minutes; (7) cooling back centrifugation; (8) after concentrated, decolouring, drying, obtain product.When being soaked in water leached tea oil slag, the per kilogram leached tea oil slag adds 10～20 liters in water.Shortcoming of the present invention: because used water as solvent, contain pectin and tea sugar in the tea saponin, therefore, purity is not high; When concentrating in addition, the equipment funds height that needs; The energy height that consumes.
200,410,046,824 1 kinds of application numbers use water as solvent extracts tea saponin from cake of camellia oleifera seeds (or oil tea fruit, tea-seed) production method, comprise pulverizings, dezymotize, technical process such as lixiviate, centrifugal solid-liquid separation, settlement separate, video disc centrifugation, pre-filtering separation, nanofiltration membrane are concentrated, drying.Before the lixiviate material is suppressed, eliminates the activity of lytic enzyme by method of chemical treatment, improve the penetrating power of tea saponin during lixiviate by insulated and stirred, add flocculation agent in the vat liquor that after solid-liquid separation, obtains, settlement separate back disk plate centrifuge separating clarifying liquid, isolate heavy phase (flocculation sediment), use the pressure filter press filtration, concentrate light phase (tea saponin solution), the flaxen tea saponin of the last spray-dried powdering of concentrated liquid with nanofiltration membrane.Commercial run of the present invention is simple, facility investment and production cost is low, less energy consumption, and the yield of gained tea saponin product surpasses 70%, purity reaches 85%, faint yellow, is suitable for suitability for industrialized production.Shortcoming of the present invention: because used water as solvent, contain pectin and tea sugar in the tea saponin, therefore, purity is not high; When concentrating in addition, the equipment funds height that needs; The energy height that consumes.
Application number 200510018694 the present invention relates to a kind of method of utilizing ultrasonic wave to prepare tea saponin, belongs to farming, secondary product of forestry deep processing field.Technical scheme is: will extract that cake of camellia oleifera seeds behind the grease is pulverized, added organic solution mixings, ultrasonic lixiviate, separation and solvent recuperation then, ultrafiltration purification obtains the tea saponin concentrated solution, and decolour and drying treatment obtains the tea saponin product again.Beneficial effect of the present invention is: 1. adopt the physics extractive technique of ultrasonic wave and ultrafiltration purification to be applied to producing of tea saponin, improved the extraction efficiency of tea saponin, one time extraction yield can reach more than 90%, and the purity height of extract, and quality is good; 2. preparation technology is comparatively easy, has shortened process cycle, has reduced energy consumption and production cost, can be suitable for commercial scale production; 3. technological process is provided with rationally, pollutes for a short time, and extracting solution can recycle repeatedly, and the cake of camellia oleifera seeds that extracts behind the tea saponin can also utilize as feed again, can make the cake of camellia oleifera seeds resource be used fully and develop.Shortcoming of the present invention: the equipment requirements that needs is higher; And during suitability for industrialized production, whether powerful ultrasonic wave is harmful, requires study.
Summary of the invention
It is simple to the objective of the invention is to set up a kind of technology, and production cost is low, and the added value height is easy to the method for big suitability for industrialized production tea saponin and tea polysaccharide.
Purpose of the present invention can be achieved through the following technical solutions: with the tea oil cake is raw material, the employing low-boiling point alcohol is a solvent, reflux heat is carried, the mixture that must contain tea saponin and tea polysaccharide, mixture dissolves through the secondary anhydrous normal butyl alcohol, separate purity greater than 90% tea saponin, separate purity greater than 95% tea polysaccharide.
Concrete steps of the present invention are as follows:
(1). with the tea oil rake is raw material, and the employing low-boiling point alcohol is a solvent, and reflux heat is put forward tea saponin and tea polysaccharide.
(2). reclaim solvent and get medicinal extract, solvent can be reused.
(3). medicinal extract adopts anhydrous normal butyl alcohol heat to put forward tea saponin and tea polysaccharide, cool off tea saponin solid and butanol solution; Reclaim butanol solution, must contain the mixture of tea polysaccharide.
(4). the tea saponin by step (3) gained adopts anhydrous normal butyl alcohol heat to put forward tea saponin and tea polysaccharide again, cool off tea saponin solid and butanol solution; Reclaim butanol solution, must contain the mixture of tea polysaccharide.
(5). merge the mixture of tea polysaccharide, add aqueous ethanol, the indissoluble material is the tea polysaccharide product.
Employed low-boiling point alcohol is dehydrated alcohol or anhydrous methanol among the present invention, or ethanol and methanol mixture.
When the present invention put forward tea saponin and tea polysaccharide with anhydrous normal butyl alcohol heat, its temperature was at+600C---+1500C; During the cooling of the tea saponin solution of anhydrous normal butyl alcohol, its temperature is at-100C---+300C.
It is that solution and solid reclaim under vacuum or decompression by after centrifugation or filtering that the present invention reclaims solvent, and solvent can be reused.
Anhydrous solvent of the present invention is moisture 0.5% the solvent that is not more than; Industrial common anhydrous solvent or solvent needn't pass through processed after separating use through tea saponin, can directly use.
Aqueous ethanol of the present invention, water and alcoholic acid volume ratio are 1: 10 to 1: 50 scope
Key instrument used in the present invention and equipment:
1). Rotary Evaporators
2). circulation ability of swimming vacuum pump
3). reflux
Compare with present industry and the described tea saponin of patent, method technology of the present invention is simple, and production cost is low, and the added value height is easy to big suitability for industrialized production, the efficient height; Tea saponin product of the present invention, white purity height is compared with present faint yellow or xanchromatic tea saponin, and the commercial competition advantage is all arranged on price and quality.
With the tea oil cake is patent and the document that raw material extracts tea polysaccharide, does not appear in the newspapers; The content that separates tea polysaccharide from tealeaves all is not more than 60%; And its content of tea polysaccharide product of the present invention is greater than 95%; Tea polysaccharide product of the present invention can be used as protective foods, and further exploitation has the medicine of becoming.
Embodiment
Embodiment 1
Tea oil cake 200---300 order 615 grams place 2 liters of round-bottomed flasks, are incorporated as 1500 milliliters of dehydrated alcohols, and water-bath refluxed 4.5 hours; Filter, filter residue repeats above-mentioned alcohol reflux totally 8 times.Merge ethanolic soln, under the reduced pressure, be condensed into medicinal extract in 600C; Medicinal extract in the 1200C extracting, in the 00C cooling, gets tea saponin solid and butanol solution with propyl carbinol; Under the reduced pressure, reclaim butanol solution, must contain the mixture of tea polysaccharide.Above-mentioned tea saponin solid uses propyl carbinol in the 1200C extracting again, in the 00C cooling, filters, and gets tea saponin white solid 78 grams, and content is 91%; Reclaim butanol solution, must contain the mixture of tea polysaccharide.Merge the mixture that contains tea polysaccharide, 1200 milliliters of the chemical pure ethanol of adding (V/V) 95% left standstill 1 day, filtered to such an extent that tea polysaccharide 2.5 restrains, and content is 96%.
Embodiment 2
Tea oil cake 200---300 order 605 grams place 2 liters of round-bottomed flasks, and adding concentration is 1500 milliliters of anhydrous methanols, and water-bath refluxed 4.5 hours; Filter, filter residue repeats above-mentioned methanol eddy totally 8 times.Merge methanol solution, under the reduced pressure, be condensed into medicinal extract in 600C; Medicinal extract in the 1300C extracting, in the 100C cooling, gets tea saponin solid and butanol solution with propyl carbinol; Under the reduced pressure, reclaim butanol solution, must contain the mixture of tea polysaccharide.Above-mentioned tea saponin solid uses propyl carbinol in the 1300C extracting again, in the 100C cooling, filters, and gets tea saponin white solid 70.5 grams, and content is 92.5%; Reclaim butanol solution, must contain the mixture of tea polysaccharide.Merge the mixture that contains tea polysaccharide, 1200 milliliters of the chemical pure ethanol of adding (V/V) 90% left standstill 1 day, filtered to such an extent that tea polysaccharide 2.8 restrains, and content is 95.5%.
Embodiment 3
Tea oil cake 200---300 order 608 grams place 2 liters of round-bottomed flasks, and adding concentration is 1500 milliliters of dehydrated alcohols, and water-bath refluxed 4.5 hours; Filter, filter residue repeats above-mentioned alcohol reflux totally 8 times.Merge ethanolic soln, under the reduced pressure, be condensed into medicinal extract in 600C; Medicinal extract in the 900C extracting, in the 200C cooling, gets tea saponin solid and butanol solution with propyl carbinol; Under the reduced pressure, reclaim butanol solution, must contain the mixture of tea polysaccharide.Above-mentioned tea saponin solid uses propyl carbinol in the 900C extracting again, in the 200C cooling, filters, and gets tea saponin white solid 72 grams, and content is 90%; Reclaim butanol solution, must contain the mixture of tea polysaccharide.Merge the mixture that contains tea polysaccharide, 1200 milliliters of the chemical pure ethanol of adding (V/V) 99% left standstill 1 day, filtered to such an extent that tea polysaccharide 3.1 restrains, and content is 95.1%.
Claims (6)
1. one kind is separated the method for tea saponin and tea polysaccharide from the tea oil cake, it is characterized in that concrete steps are:
(1). with the tea oil rake is raw material, and the employing low-boiling point alcohol is a solvent, and reflux heat is put forward tea saponin and tea polysaccharide;
(2). reclaim solvent, get medicinal extract, solvent is reused;
(3). medicinal extract adopts anhydrous normal butyl alcohol heat to put forward tea saponin and tea polysaccharide, and cooling gets tea saponin solid and butanol solution; Reclaim butanol solution, must contain the mixture of tea polysaccharide;
(4). the tea saponin by step (3) gained adopts anhydrous normal butyl alcohol heat to put forward tea saponin and tea polysaccharide again, and cooling gets tea saponin solid and butanol solution; Reclaim butanol solution, must contain the mixture of tea polysaccharide;
(5). merge the mixture of tea polysaccharide, add aqueous ethanol, the indissoluble material is the tea polysaccharide product.
2. according to the described method of claim 1, it is characterized in that described low-boiling point alcohol is dehydrated alcohol or anhydrous methanol from tea oil cake separation tea saponin and tea polysaccharide, or ethanol and methanol mixture.
3. according to the described method from tea oil cake separation tea saponin and tea polysaccharide of claim 1, when it is characterized in that described anhydrous normal butyl alcohol heat is put forward tea saponin and tea polysaccharide, its temperature is at+60 ℃--and-+150 ℃; When the tea saponin solution of anhydrous normal butyl alcohol cooled off, its temperature was-10 ℃----+30 ℃.
4. according to the described method from tea oil cake separation tea saponin and tea polysaccharide of claim 1, it is characterized in that reclaiming described in step (3) and (4) solvent is that solution and solid reclaim under vacuum or decompression by after centrifugation or filtering.
5. according to the described method of claim 1, it is characterized in that described anhydrous solvent is moisture 0.5% the solvent that is not more than from tea oil cake separation tea saponin and tea polysaccharide.
6. according to the described method of claim 1, it is characterized in that in the described aqueous ethanol that water and alcoholic acid volume ratio are 1: 10 to 1: 50 from tea oil cake separation tea saponin and tea polysaccharide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100423326A CN101070334B (en) | 2007-06-21 | 2007-06-21 | Process for separating tea sapogenin and tea polysaccharide from tea-oil cake |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007100423326A CN101070334B (en) | 2007-06-21 | 2007-06-21 | Process for separating tea sapogenin and tea polysaccharide from tea-oil cake |
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| CN101070334A true CN101070334A (en) | 2007-11-14 |
| CN101070334B CN101070334B (en) | 2010-12-29 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102535178A (en) * | 2010-12-31 | 2012-07-04 | 巫峻维 | Antibacterial environment-friendly down feather making method |
| CN102925292A (en) * | 2012-10-19 | 2013-02-13 | 伊国群 | Method for comprehensively extracting tea oil, flavonoids compounds, tea saponin and tea polysaccharide |
| CN107118253A (en) * | 2017-06-20 | 2017-09-01 | 中国科学院青岛生物能源与过程研究所 | The preparation method of Tea Saponin |
| CN113527403A (en) * | 2021-07-31 | 2021-10-22 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100522982C (en) * | 2004-10-01 | 2009-08-05 | 南华大学 | Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent |
-
2007
- 2007-06-21 CN CN2007100423326A patent/CN101070334B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102535178A (en) * | 2010-12-31 | 2012-07-04 | 巫峻维 | Antibacterial environment-friendly down feather making method |
| CN102925292A (en) * | 2012-10-19 | 2013-02-13 | 伊国群 | Method for comprehensively extracting tea oil, flavonoids compounds, tea saponin and tea polysaccharide |
| CN102925292B (en) * | 2012-10-19 | 2014-11-05 | 伊国群 | Method for comprehensively extracting tea oil, flavonoids compounds, tea saponin and tea polysaccharide |
| CN107118253A (en) * | 2017-06-20 | 2017-09-01 | 中国科学院青岛生物能源与过程研究所 | The preparation method of Tea Saponin |
| CN113527403A (en) * | 2021-07-31 | 2021-10-22 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
| CN113527403B (en) * | 2021-07-31 | 2022-08-30 | 海南黎草纪新生物科技有限公司 | Extraction method for camellia saponin |
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