CN105777848A - Method for preparing tea saponin with function of dispelling effects of alcohol from cakes of camellia oleifera - Google Patents
Method for preparing tea saponin with function of dispelling effects of alcohol from cakes of camellia oleifera Download PDFInfo
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- CN105777848A CN105777848A CN201610251905.5A CN201610251905A CN105777848A CN 105777848 A CN105777848 A CN 105777848A CN 201610251905 A CN201610251905 A CN 201610251905A CN 105777848 A CN105777848 A CN 105777848A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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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)
- A61K36/82—Theaceae (Tea family), e.g. camellia
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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Abstract
The invention discloses a method for preparing tea saponin with a function of dispelling effects of alcohol from cakes of camellia oleifera. The production flow comprises the following steps: crushing, drying and screening degreased cakes of camellia oleifera; adding hot water for extracting twice, and merging the filtrate, so as to obtain a crude extraction solution of tea saponin; adding 95% ethanol into the crude extraction solution so as to realize quick flocculating, filtering, and removing the filter residues (crude tea polysaccharides); concentrating the filtrate, adding CaO, reacting, precipitating and filtering; adding an ammonium bicarbonate solution into the precipitate, transforming the precipitate, and filtering; repeating the previous two steps for 1-3 times, discoloring, and performing vacuum freeze drying, so as to obtain the product. The tea saponin powder obtained by the method comes from a natural product, and the production process is green, environmental-friendly and safe. Through ethanol dehydrogenase acting on the gastrointestinal tract, the tea saponin has the effects of obviously enhancing the activity of ethanol dehydrogenase and enhancing a first-pass effect of the ethanol in the gastrointestinal tract.
Description
Technical field
The invention belongs to agriculture and forestry by-product field of deep, specifically one is with cake of camellia oleifera seeds for raw material, and the effective ingredient tea saponin that relieves the effect of alcohol therein is easily separated extraction, obtains the process with the tea saponin of activity of relieving the effect of alcohol.
Background technology
Spirits culture is a traditional culture of China, and China resident thus caused occurs that a large amount of excessive drinking and alcoholism event are increasing, thus having influence on the physical and mental health of people and the harmony of family, society.So developing the Medicament for Alcoholism of a kind of Nantural non-toxic or Medicament for Alcoholism raw material has extremely important value and significance.
Drunk is a kind of acute alcoholism, main manifestations central nervous excitation after drinking or suppression.The drunk mechanism having now been found that mainly includes 3 aspects: one be the absorption rate of ethanol more than oxidation rate, cause that internal ethanol content is too high, and then act on brain, affect central nervous system.Two is that the acetaldehyde produced after oxidation of ethanol has musclar toxicity, and bulk deposition can cause that internal organs are impaired.Three is that ethanol can produce substantial amounts of free radical in metabolism way, forms free chain reaction, destroys inside of human body balance, cause the symptoms such as dizziness, headache and gastrointestinal upset.
Natural product, according to its relieving mechanism, can be divided into ethanol gastrointestinal absorption inhibitor and metabolism reinforcing agent.The mechanism of ethanol gastrointestinal absorption inhibitor is by strengthening the ethanol first pass metabolism suppression ethanol absorption in gastrointestinal tract at gastric, thus reducing ethanol in blood concentration, alleviating the ethanol infringement to body.First pass metabolism is relevant with gastric alcohol dehydrogenase activity, can effectively alleviate the ethanol toxic action to body by improving alcohol dehydrogenase activity.The relieving mechanism of metabolism reinforcing agent is the supersession rate directly acting on liver metabolism enzyme system's accelerating alcohol and metabolite thereof, alleviates its damage to tissue and cell.
China is the country that Semen Camelliae yield is maximum, produces substantial amounts of cake of camellia oleifera seeds, containing tea saponin 10% ~ 20% in grouts after Semen Camelliae oil expression.Tea saponin is Triterpenoids sapogenins saponins mixture, and its basic structure is mainly made up of aglucon, sugar body, organic acid three part.Pertinent literature is reported, tea saponin has the effect suppressing ethanol to absorb.
At present, there is a lot of patent literature antialcoholic drugs and preparation method thereof, also have a lot of article to report the extracting method of tea saponin.As:
Patent CN101244084B discloses a kind of sobering-up agent of pearl oyster meat and preparation method thereof, this invention relates to a kind of sobering-up agent of pearl oyster meat and preparation method thereof, it is characterized in that with the by-product Carnis Margarita of pearl culture for raw material, adopt biological enzymolysis technology, sobering-up agent of pearl oyster meat obtain a kind of quickly can being absorbed by human body, making people relieve the effect of alcohol rapidly and preparation method thereof.These invention raw material sources are extensive, and Carnis Margarita is nutritious, has hepatoprotective and calms the nerves, effect of heat-clearing and toxic substances removing.This Medicament for Alcoholism has the advantages such as safe and nontoxic pair.Mouse experiment shows, sobering-up agent of pearl oyster meat, it is possible to reduce drunk number of elements, reduces concentration of alcohol in mouse blood, it is possible to anti-acute alcohol-induced hepatic injury, has effect of well relieving the effect of alcohol.
Patent CN102919834A discloses a kind of glutathione anti-alcoholic food, and this invention relates to a kind of glutathion and relieves the effect of alcohol food, belongs to the technical field of food processing industry.This kind of glutathion relieves the effect of alcohol food; the glutathion of reduced form, taurine, glucose, Semen Hoveniae (Fructus Hoveniae), Folium Bambusae, xylitol, oligofructose, stevioside etc. are adopted to be processed into alcohol detoxication candies and alcohol-decomposing beverage by the technology of food processing; glutathion, glucose, taurine all have Detoxication widely; Semen Hoveniae (Fructus Hoveniae) is good at dryout; therefore; the sugar that relieves the effect of alcohol of the application, alcohol-decomposing beverage has definite therapeutic efficiency.
Patent CN101974062A uses ether to be that precipitant makes tea saponin flocculation obtain product, the method is with cake of camellia oleifera seeds for raw material, first pulverized, it is container with enamel pot again, the ethanol using 65% ~ 75% concentration is extracting solution, backward extracting solution in add ether, obtain flocculent deposit, dry obtain tea saponin finished product.The ether that the method uses has very big danger, is not suitable for commercial production.
Patent CN102260316A discloses a kind of method that flocculent precipitation purifies tea saponin, with cake of camellia oleifera seeds for raw material, adopt petroleum ether that it is carried out defat, with the ethanol of 85% ~ 95%, it is carried out lixiviate again, extracting solution is initially charged Alumen flocculation and removes partial impurities, adds lime cream and tea saponin transfers to tea saponin calcium deposit separates, adds acetum, tea saponin calcium is turned molten in solution, and the tea saponin solution being filtrated to get obtains refined theasapogenin through decolouring, concentration, spray drying.Alumen and acetic acid that the method adds are difficult to remove, and commercial Application is restricted.
Patent CN1706863A describes a kind of method that ultrasound wave prepares tea saponin, with the cake of camellia oleifera seeds after defat for raw material, pulverizes, adds organic solvent, ultrasonic lixiviate, separation and solvent recovery, ultrafiltration purification, and the concentrated solution purification that decolours again obtains tea saponin product.The ultrasonic equipment that the method uses, but be chronically at ultrasound environments and human body had potentially hazardous, be not suitable for industrialized production.
Patent DE19522635A1 introduces a kind of tea saponin purification process, camellia oleosa seed is used to replace soapbark as raw material, improve quality and the yield rate of product, reduce cost, comprise the following steps: camellia oleosa seed pulverizing, 70% ~ 95% ethanol extraction, concentration, addition butanol purification and dry, obtain final tea saponin powder.
Water extraction, organic solvent method, supercritical extraction, water extracting alcohol extraction method, microwave-assisted extraction, ultrasound assisted extraction method, homogenate extraction method and two-stage foam separation etc. are had at present about the extraction of tea saponin, but these methods have respective deficiency and limitation, and it is not strong to produce purposiveness.Such as, the tea saponin purity that simple water raises is very low；Organic solvent method, if use methanol can be poisonous, if using ethanol, the cost once put into is huge；Microwave radiation exaraction, main equipment produces difficulty, it is difficult to for industrialized production.
Summary of the invention
The invention provides a kind of method prepared from cake of camellia oleifera seeds and there is antialcoholism function tea saponin.
Applicant shows through substantial amounts of research, tea saponin can strengthen alcohol dehydrogenase activity preferably under alkalescence or neutral environment, find based on this, imagination adopts water to put forward (neutrality), ethanol rapid flocculation precipitates (alkalescence) in conjunction with CaO many times (1 ~ 3 time), ammonium hydrogen carbonate (alkalescence), is specifically had the tea saponin preparation technology of activity of relieving the effect of alcohol.This method production cost is low, non-environmental-pollution, and the tea saponin obtained can be obviously enhanced alcohol dehydrogenase activity, safety non-toxic, and stable processing technique, is beneficial to large industrialized and produces.
The technical solution used in the present invention is as follows:
A kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds, its feature is as follows:
A, the cake of camellia oleifera seeds of defat is pulverized, dry, cross 20 ~ 200 mesh sieves；
B, step a is pulverized after grouts, add flooding by 1:5 ~ 20, extraction temperature 40 DEG C ~ 90 DEG C, extraction time 20 ~ 60min, point 2 ~ 3 lixiviates, filter, merging filtrate；
C, take step b filtrate, be added thereto to flocculant, rapid flocculation 0.5 ~ 1h, filter；
D, take step c filtrate, add precipitant, to be precipitated completely, filter；
E, taking step d gained precipitation, add precipitation transforming agent, stirring, stand, conversion to be precipitated is complete, filters；
F, take step e filtrate, repeat d, e two step 1 ~ 3 time；
G, take the concentration of step f filtrate, add decolorising agent, dry, obtain flaxen tea saponin powder.
Described flocculant is 95% ethanol, and the volume ratio of filtrate and ethanol is 1:1 ~ 3.
Described precipitant is CaO；Described precipitation transforming agent is ammonium hydrogen carbonate；Decolorising agent described in step g is hydrogen peroxide, and described drying means is vacuum lyophilization.
The present invention separates the tea saponin with activity of relieving the effect of alcohol from cake of camellia oleifera seeds, has the advantage that
1, use ethanol as flocculant, both can play good flocculating effect, and effectively removes the tea polysaccharide in cake of camellia oleifera seeds, decrease the tea polysaccharide impact on alcohol dehydrogenase activity, can recycle again simultaneously, decrease the consumption of resource.
2, the activity of relieving the effect of alcohol that tea saponin has is utilized, it is contemplated that alkaline environment is beneficial to its activity of relieving the effect of alcohol of maintenance, devises specific process route, and the tea saponin obtained can significantly improve alcohol dehydrogenase activity.
3, technique is on practical basis, and design is simple as far as possible, reduces production cost.Gained tea saponin powder remains without reagent, except tea saponin, mainly contains some tea polysaccharide, fat etc., safety non-toxic.
Accompanying drawing explanation
Fig. 1 is the process chart of this method；
Fig. 2 is the tea saponin infrared spectrogram that the present invention extracts.
Detailed description of the invention
Embodiment 1, a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds, step is as follows:
A, take removing oil fatty oil tea-cake dregs and put in mechanical crusher and pulverize, dry, cross 40 mesh sieves；
B, taking powder 20g in above-mentioned steps, add 200ml water, extract at twice, water temperature is maintained at 80 DEG C, each 30min, filters, merging filtrate.
C, take step b filtrate, add 95% ethanol of 200ml, rapid flocculation 0.5 ~ 1h, filter.
D, take step c filtrate, add CaO, place 2 ~ 3h, treat to precipitate completely, filter.
E, taking step d gained precipitation, add ammonium hydrogen carbonate, stirring, stands 3 ~ 4 hours, conversion to be precipitated is complete, filtration.
F, take step e filtrate, repeat d, e two step 2 times
G, take step f filtrate concentration, add hydrogen peroxide for decoloration, vacuum lyophilization, obtain yellow tea saponin powder 2.62g, purity is 80.5%, extraction ratio 61.7%.
H, take the step g tea saponin powder obtained, carry out experiment in vitro, adopt Wa Lehuohe (Valle&Hoch) method to improve, measure alcohol dehydrogenase activity.It is separately added into, in measuring pipe, the sodium pyrophosphate buffer solution 1.5mL that pH value is 8.8, 27mmol/L oxidized form of nicotinamide-adenine dinucleotide (NAD+) 1.0mL, alcoholic solution (v/v) 0.5mL of 11.5%, 1mg/mL tea saponin solution 0.1mL, after mixing, put into incubation 5min in the water-bath of 25 DEG C, add ADH (0.25U/mL) afterwards O.1mL, in 340nm place, light absorption value is measured every one minute, matched group 0.1mL distilled water replaces tea saponin solution, blank group replaces the alcoholic solution of 11.5% with 0.5mL distilled water, found that relative to matched group, its alcohol dehydrogenase activity improves 37%.
Embodiment 2, a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds, step is as follows:
Preceding step is with embodiment 1, to step f, repeats d, e two step 3 times, the filtrate concentration that will obtain, and adds hydrogen peroxide for decoloration, vacuum lyophilization, obtains faint yellow tea saponin powder 2.33g, and purity is 87.6%, extraction ratio 58.7%.
Taking the step g tea saponin powder obtained, carry out experiment in vitro, step is with example one, it has been found that relative to matched group, and its alcohol dehydrogenase activity improves 51.4%.
The tea saponin of gained is carried out infrared spectrum characterization, it can be seen that at 3500cm from accompanying drawing 2-1Left and right is the stretching vibration peak of hydroxyl；At 2942cm-1Place is expressed as the stretching vibration peak of methyl, methylene；At 2500cm-1~1900cm-1Left and right does not absorb, it was shown that do not have three keys and cumulated double bond；At 1717cm-1~1616cm-1There is the stretching vibration peak of carbonyl at place；At 1419cm-1And 1375cm-1The antisymmetry deformation vibration peak of place respectively-CH-and symmetrical deformation vibration peak；At 1261cm-1Place is the in-plane bending vibration peak of C-O-H；1076cm-1Place is the stretching vibration peak of C-O-C.
Comparative example
A kind of method that in Semen Camelliae grouts, main component is comprehensively extracted, comprises the steps of
1, raw material chooses raw material from Da Bie Mountain area, records raw material containing tea saponin 17.5%.
2, pulverizing goes fat that Semen Camelliae grouts are crushed to 40 orders, adds petroleum ether, 60 DEG C of backflow 2h.
3, the ethanol extraction of alcohol extraction 85% three times, concentration
4, acetone precipitation concentrated solution adds 2 times of vol acetone, produces flocculent deposit.
5, dry vacuum lyophilization, obtains tea saponin powder, and purity is 81.5%.
6, carry out experiment in vitro step with example one, do not find that tea saponin powder substantially activates alcohol dehydrogenase activity.
Relatively above-described embodiment and comparative example, it is seen that under close purity, the tea saponin that this method obtains can significantly improve alcohol dehydrogenase activity, and tool has great advantage.
Claims (5)
1. from cake of camellia oleifera seeds, prepare the method with antialcoholism function tea saponin for one kind, it is characterised in that comprise the following steps:
A, the cake of camellia oleifera seeds of defat is pulverized, dry, cross 20 ~ 200 mesh sieves；
B, step a is pulverized after grouts, add flooding by 1:5 ~ 20, extraction temperature 40 DEG C ~ 90 DEG C, extraction time 20 ~ 60min, point 2 ~ 3 lixiviates, filter, merging filtrate；
C, take step b filtrate, be added thereto to flocculant, rapid flocculation 0.5 ~ 1h, filter；
D, take step c filtrate, add precipitant, to be precipitated completely, filter；
E, taking step d gained precipitation, add precipitation transforming agent, stirring, stand, conversion to be precipitated is complete, filters；
F, take step e filtrate, repeat d, e two step 1 ~ 3 time；
G, take the concentration of step f filtrate, add decolorising agent, dry, obtain flaxen tea saponin powder.
2. a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds according to claim 1, it is characterised in that: described flocculant is 95% ethanol, and the volume ratio of filtrate and ethanol is 1:1 ~ 3.
3. a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds according to claim 1, it is characterised in that: described precipitant is CaO.
4. a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds according to claim 1, it is characterised in that: described precipitation transforming agent is ammonium hydrogen carbonate.
5. a kind of method that preparation has antialcoholism function tea saponin from cake of camellia oleifera seeds according to claim 1, it is characterised in that: the decolorising agent described in step g is hydrogen peroxide, and described drying means is vacuum lyophilization.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110916032A (en) * | 2019-11-04 | 2020-03-27 | 合肥工业大学 | Tea saponin beverage for relieving alcoholism and protecting liver and preparation method thereof |
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830948A (en) * | 2010-05-11 | 2010-09-15 | 武汉工业学院 | Method for preparing tea saponin by using tea seed degreased dreg |
| CN101880307A (en) * | 2010-06-17 | 2010-11-10 | 安徽省农业科学院茶叶研究所 | Method for extracting tea saponin by utilizing microbes |
| CN103304621A (en) * | 2013-06-06 | 2013-09-18 | 湖南新泰裕农业科技投资有限公司 | Process for extracting high-purity tea saponin from camellia seed cakes |
-
2016
- 2016-04-20 CN CN201610251905.5A patent/CN105777848A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830948A (en) * | 2010-05-11 | 2010-09-15 | 武汉工业学院 | Method for preparing tea saponin by using tea seed degreased dreg |
| CN101880307A (en) * | 2010-06-17 | 2010-11-10 | 安徽省农业科学院茶叶研究所 | Method for extracting tea saponin by utilizing microbes |
| CN103304621A (en) * | 2013-06-06 | 2013-09-18 | 湖南新泰裕农业科技投资有限公司 | Process for extracting high-purity tea saponin from camellia seed cakes |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110916032A (en) * | 2019-11-04 | 2020-03-27 | 合肥工业大学 | Tea saponin beverage for relieving alcoholism and protecting liver and preparation method thereof |
| CN111449090A (en) * | 2020-04-13 | 2020-07-28 | 湖南润农生态茶油有限公司 | Preparation method of tea seed cake extract |
| CN113018896A (en) * | 2021-03-03 | 2021-06-25 | 北京林业大学 | Natural saponin decoloring method |
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