CN103005162A - Method for extracting antivirus growth promoter of saccharicterpenin - Google Patents
Method for extracting antivirus growth promoter of saccharicterpenin Download PDFInfo
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- CN103005162A CN103005162A CN2012105821180A CN201210582118A CN103005162A CN 103005162 A CN103005162 A CN 103005162A CN 2012105821180 A CN2012105821180 A CN 2012105821180A CN 201210582118 A CN201210582118 A CN 201210582118A CN 103005162 A CN103005162 A CN 103005162A
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Abstract
The invention provides an efficient method for extracting an antivirus growth promoter of saccharicterpenin, in particular using a method of hot water ultrasonic extraction in combination with fluidized spray drying. Saccharicterpenin is extracted from an oil tea cake. The method is simple and easy to operate, high in efficiency, the used raw material is easily available, the efficiency of extracting the saccharicterpenin in the prior art is improved, the raw material range of the saccharicterpenin is broadened, and the economic benefit of oil tea as an economic crop is improved.
Description
Technical field
The present invention relates to technical field of feed additive production, relate more specifically to a kind of extracting method of saccharicter-penin.
Background technology
FDA (FDA) ratifies antibiotic as feed addictive first in nineteen fifty, and after this, countries in the world are carried out antibiotic feeding experiment in succession, and is used for herding production.Antibiotic has improved the conversion ratio of feed greatly as additive in the feed, has promoted the production performance of letting animals feed.Yet along with antibiotic long-term a large amount of the use, bring unprecedented promotion to aquaculture development, but also can cause negative effect, the resistance to the action of a drug, animal alimentary canal flora imbalance, autoimmunity such as pathogenic microorganism reduce, and antibiotic is residual in livestock products, direct harm humans health etc.In succession promulgated in European Union, Japanese developed country and to have forbidden and limit and use the application of Antibiotic Additive in feed.Therefore, the animal food safety problem becomes one of focus of national governments and common people's concern day by day.Seeking natural alternative feeding antibiotic as feed addictive, is long-term striving direction in the feed industry research field.
In recent years, antibiotic substitute products both domestic and external mainly contain enzyme preparation, Chinese herbal medicine, probiotic, oligosaccharides, betaine and antibacterial peptide etc.And saccharicter-penin (Saccharicterpenin) is as a kind of new green feed additive, saccharicter-penin is the plant extracts of pure natural, by carbohydrate (〉=30%), the pure-natural biological active additive of triterpenoid saponin (〉=30%) and organic acid composition, being the triterpenoid saponin that extracts from Camellia Plants seed grouts and the mixture of carbohydrate, is a kind of brown color, ashless fine shape crystallization.It is insoluble to ether, chloroform, acetone, benzene, benzinum equal solvent, dissolves in warm water, carbon disulfide, ethyl acetate, is soluble in aqueous methanol, hydrous ethanol, n-butanol and glacial acetic acid.Saccharicter-penin can substitute the feeding antibiotic medicine, and noresidue, and is pollution-free, is national unique AA level fully natural green additive, has good market prospects, just is being subject to paying close attention to more and more widely.No. 1126 bulletins of the Ministry of Agriculture " feed addictive kind catalogue " have been listed at present in.
The mechanism of action of saccharicter-penin obviously is different from antibiotic.Antibiotic mainly is the harmful microorganism that suppresses in the digestive organs such as animal small intestine, caecum, thereby is conducive to infiltration and the absorption of nutrient, promotes the appetite of animal, increases feed intake, promotes body growth to grow.And saccharicter-penin is whole immune performance and internal system function by the raising animal, improves the general level of the health of animal, thereby improves the production performance of animal.
Saccharicter-penin has obvious adjusting animal body neuroendocrine-immune network, improves body's immunity, eliminates free radical, promotes the effect that protein is synthetic and improve digestive enzyme activity as feed addictive, can obviously regulate cAMP/ cGMP system, and have certain anti-stress and antioxidation.Saccharicter-penin can also obviously improve survival rate, growth performance and the product quality of livestock and poultry and aquatic livestock; can the substitute antibiotics feed addictive in aquaculture; be a kind of novel, safety and non-harmful green feed additive, animal foodstuff and the to protect mankind health of production safety high-quality is had great importance.
But the systematization production of saccharicter-penin is demanded urgently further perfect.The one, provide the Extracted From Oil-tea-cake cake of a large amount of cheapnesss as the raw material that extract saccharicter-penin.The 2nd, develop a technology of overlapping efficient deep processing Extracted From Oil-tea-cake cake.Along with the deep development of camellia oleiferaindustry, extracting saccharicter-penin will provide the Extracted From Oil-tea-cake cake of a large amount of cheapnesss to make raw material problems will to be resolved very soon, and rational exploitation and utilization Extracted From Oil-tea-cake cake how, is the difficult problem that the industrial chain of oil tea will face and need to be resolved hurrily.
At present, saccharicter-penin has two kinds of preparation methods: the one, obtain a kind of pentacyclic triterpene compound and a kind of oligosaccharides with pure Tea Saponin hydrolysis (acidolysis or enzymolysis all can), and the mixture of the two is exactly " saccharicter-penin ", and its shortcoming is at first to need to extract Tea Saponin; The 2nd, use first acid or suitable enzyme hydrolysis CHAKUBING, from hydrolyzate, extract again triterpenoid and oligosaccharides, mix according to a certain percentage being " saccharicter-penin ", its shortcoming is that extract yield is lower.
Chinese patent CN101756023A has announced a kind of extracting method of novel feed additive saccharicter-penin, gets the seed of oil tea section plant, and dry rear peeling is pulverized, and is solvent with ethanol, extracting through microwave heating three times.Merge extract, with its reduced pressure concentration, use extracting n-butyl alcohol, extract is dry through reduced pressure concentration, obtains extract powder.Its shortcoming is to utilize the seed of oil tea directly to extract, and has wasted oil tea oil wherein.But it adopts extraction process, complicated operation, and clearly record in its specification, and yield only has about 15%.
Chinese patent CN101695336A has announced tea seed episperm bioactive extracts and has used and the preparation method, and application and the preparation method of tea seed episperm bioactive extracts is provided, and relates to agricultural wastes comprehensive utilization of resources technical field.This extract is the bioactivator that comprises saccharicter-penin and Tea Polyphenols etc. that extracts from the shell of camellia oleifera fruit and tealeaves fruit.Its shortcoming is to utilize organic solvent to extract, and organic solvent is residual easily.
The ultrasonic wave extraction itself has two implications: the extraction of ingredient in the application of ultrasonic technique and the material.Namely be exactly utilize that ultrasonic wave produces the special roles such as cavitation, come for material chemical composition extraction process, with the new extractive technique of ingredient to extract quickly and efficiently.Pair other plant is also arranged in the prior art such as ginseng, rhodiola root etc., adopt the hot water ultrasonic extraction process to extract polysaccharide and triterpenoid saponin, but the purpose of its extraction is to extract also less than 15% of single item grouping and recovery rate, and the raw material that adopts is expensive.
Oil tea seed grouts are residues of Theaceae seed oil expression, and present present situation is that most of grouts are taken as fuel and burn, or cheapness exports to the countries and regions such as Japan, Southeast Asia, and this situation should get a new look.
Summary of the invention
The invention provides a kind of technology of efficient extraction saccharicter-penin.
For obtaining above-mentioned effect, the invention provides a kind of extracting method of antivirus somatotropic agent saccharicter-penin, comprise following steps,
S1. get the Extracted From Oil-tea-cake cake, pulverize;
S2. add water, heating, ultrasonic wave extracts, and gets extract,
S3. concentrated extracting solution gets concentrate,
S4. dry concentrate, and get final product.
Be heated to 60 ~ 80 ℃ among the described step S2, be preferably 75 ℃.The preferred temperature of institute can better be dissolved saccharicter-penin thoroughly, and can not decompose saccharicter-penin.
Hyperacoustic power among the described step S2 is 400W ~ 6000W, and the time is 5 ~ 15 minutes, is preferably under 4500W ultrasonic 10 minutes.
The number of times of the extraction among the described step S2 is 2 ~ 5 times, and preferred 3 times, 3 extractions can be extracted the saccharicter-penin more than 97%, and are most effective; The time of extracting is 1 ~ 4 hour, preferred 2 hours, basically all saccharicter-penin extractions can be finished, and can because of the prolongation of time, not cause saccharicter-penin to decompose in 2 hours.
Be ground into 30 ~ 40 orders among the described step S1.
Simmer down to reduced pressure concentration among the described step S3, described decompression for reduce to-0.080MPa ~-0.099MPa, preferred-0.095MPa, the most energy-efficient decompression pressure.
Drying among the described step S4 is the fluidization and spray-drying method.Described sulfuration spray drying process adopts fluidization and spray-drying machine (model is ZDG3 * 0.3) to realize.The fluidization and spray-drying method can be enhanced productivity greatly, saves the production cycle, thereby reduces cost, saves the energy.
Ultrasonic wave extracts the superiority of Chinese medicine, is based on hyperacoustic specific physical character.Mainly be thereby that the active force that the main Quick mechanical vibration wave that produces by PZT (piezoelectric transducer) reduces between target extract and the sample matrices is realized solid--the liquid extract and separate.
1) accelerating medium particle movement.When being higher than middle propagation of hyperacoustic continuous media (for example water) of 20 KHz frequency of sound wave, according to Huygens's wave principle, on the wave surface of its propagation, will cause the motion of medium particle (particle that comprises the important active ingredient of medicinal material), and make the medium particle movement obtain huge acceleration and kinetic energy.The acceleration of particle generally can reach more than 2,000 times of acceleration of gravity as calculated.Make it to obtain huge acceleration and kinetic energy in the medicinal material on the effective component particle owing to the medium particle acts on ultrasonic energy, overflow rapidly the medicinal material matrix and be free in the water.
2) cavitation.Ultrasonic wave is propagated in liquid medium and is produced special " cavitation effect ", " cavitation effect " constantly produce countless internal pressures reach thousands of atmospheric little air pockets and constantly " explosion " produce powerful shock wave on the microcosmic on Chinese medicine, make wherein medicinal ingredient material quilt " bombardment " effusion, and so that the medicinal material matrix is constantly degraded, the effective component that does not wherein belong to plant structure constantly is separated.Accelerating the leaching of active ingredients of plants extracts.
3) it is consistent that hyperacoustic vibration homogenize (Sonication) makes the effect that each point is subject in the sample media, makes whole sample extraction more even.
In sum, the effective substance in the Chinese medicine not only obtains huge acceleration and the kinetic energy of self as the medium particle under the ultrasound field effect, and obtains powerful external impacts by " cavitation effect ", so can high efficiency also fully separate.
In order to explain the present invention, still can not be interpreted as limitation of the present invention, comprehensive extracting method is as follows:
S1. take by weighing a certain amount of Extracted From Oil-tea-cake cake, pulverize, sieve with the 30-40 order;
S2. add a certain proportion of water, heating-up temperature 60-80 ℃, then use the ultrasonic wave assisted extraction, extract three times.
S3. extract complete rear merging extract, its nanofiltration is condensed into suspension, suspension is further through reduced pressure concentration;
S4. last concentrate gets product by the fluidization and spray-drying legal system again, weighs.
The present invention has advantage:
1. the present invention is developed to the novel purely natural green additive with discarded oil tea seed grouts, has solved the harm that present fowl poultry uses antibiotic to bring, and health is beneficial to man.
2. the present invention adopts a kind of novel process for extracting, combines with membrane separation and purification technology by the hot water ultrasound assisted extraction technique, and then cryogenic vacuum is concentrated, and last concentrate gets product by the fluidization and spray-drying legal system again.This technological operation is simple, is a kind of production technology of cleaning, yield up to more than 50%, good product quality, obviously be better than existing extractive technique.
3. improved the recovery rate of saccharicter-penin, bring up to from original 15% and to surpass 50%, and the saccharicter-penin that has provided a kind of cheapness extracts raw material, namely extracts efficiently saccharicter-penin in the residue after the Seed of Camellia oleifera oil expression, the further like this comprehensive benefit that has promoted the oil tea plantation.
Provided by the invention in the Extracted From Oil-tea-cake cake method of high efficiency extraction saccharicter-penin, all high more a lot of than the recovery rate of the method for the extraction saccharicter-penin of putting down in writing in the background technology, and polysaccharide wherein and triterpene content all are higher than average level.
The specific embodiment
Embodiment 1
S1. get Extracted From Oil-tea-cake cake 100g, pulverize, cross 30 orders;
S2. adding distil water 1L is heated to 60 ℃, is under the ultrasonic wave of 400W at power, extracts 5 minutes, removes the supernatant extract, and residue is extracted twice more repeatedly.
S3. merge the supernatant extract, concentration extraction under the condition of 0.5PA,
S4. the concentrate that step S3 is obtained is dry by the fluidization and spray-drying method, and get final product.
The weighing products obtained therefrom gets the 56.2g saccharicter-penin.
Embodiment 2
S1. get Extracted From Oil-tea-cake cake 100g, pulverize, cross 40 orders;
S2. adding distil water 1L is heated to 75 ℃, is under the ultrasonic wave of 300W at power, extracts 10 minutes, removes the supernatant extract, and residue is extracted twice more repeatedly.
S3. merge the supernatant extract, concentration extraction under the condition of 0.25PA,
S4. the concentrate that step S3 is obtained is dry by the fluidization and spray-drying method, and get final product.
The weighing products obtained therefrom gets the 58.0g saccharicter-penin.
Embodiment 3
S1. get Extracted From Oil-tea-cake cake 100g, pulverize, cross 30 orders;
S2. adding distil water 1L is heated to 80 ℃, is under the ultrasonic wave of 500W at power, extracts 10 minutes, removes the supernatant extract, and residue is extracted twice more repeatedly.
S3. merge the supernatant extract, concentration extraction under the condition of 0.5PA,
S4. the concentrate that step S3 is obtained is dry by the fluidization and spray-drying method, and get final product.
The weighing products obtained therefrom gets the 58.6g saccharicter-penin.
The determination of polysaccharide that embodiment 4 measures in the saccharicter-penin
With glucose as a standard product adopt the phenolsulfuric acid colorimetric method for determining.
At first carry out determining of calibration curve: correctly take by weighing the dextrose standard sample of 100mg, water is settled to 100ml, and then the glucose concentration of standard solution is 1.0mg/mL.Draw glucose titer 10mL, 10 times of dilute with waters, glucose final concentration are 0.1mg/mL.Accurate draw glucose Standard Applying Solution 0.10,0.20,0.40,0.60,0.80,1.00mL(is equivalent to respectively glucose 0.01,0.02,0.04,0.06,0.08,0.10mg) moisturizing is to 2.0mL, add phenol solution (50g/L) 1.0mL, concentrated sulfuric acid solution 10mL, mixing, boiling water bath 2min, sentencing reagent blank with spectrophotometer at the 485nm wavelength after the cooling is reference, measure light absorption value, take concentration of glucose as abscissa, light absorption value is ordinate drawing standard curve.Obtaining regression equation by calibration curve is: y=8.9221x-0.0035, y are light absorption value, and x is concentration of glucose, mg/mL.
Polyoses content in the saccharicter-penin that mensuration embodiment 1 to 3 obtains, the saccharicter-penin that takes by weighing respectively 100mg embodiment 1 to 3 acquisition adds in the 80mg distilled water, add phenol solution (50g/L) 1.0mL, concentrated sulfuric acid 10mL is settled to 100mL again, saccharicter-penin content be the solution of 1mg/mL, boiling water bath 2 minutes, sentencing reagent blank with spectrophotometer at the 485nm wavelength after the cooling is reference, measures light absorption value, calculate polysaccharide concentration in the again substitution regression equation, measurement result is as shown in table 1.
The assay result of polysaccharide in the saccharicter-penin that table 1 embodiment 1 to 3 obtains
| Embodiment | Light absorption value | Polysaccharide concentration (mg/mL) | Contain polysaccharide percentage amounts (%) |
| Embodiment 1 | 3.280 | 0.368 | 36.8 |
| Embodiment 2 | 3.110 | 0.349 | 34.9 |
| Embodiment 3 | 3.164 | 0.355 | 35.5 |
The triterpene assay that embodiment 5 measures in the saccharicter-penin
Take betulin as standard items, take vanillic aldehyde-ice acetic acid method to measure triterpene content.
The preparation of calibration curve: accurately take by weighing the standard items 10.0mg of betulin of dry constant weight in the volumetric bottle of 50mL, add the methyl alcohol dissolving, be diluted to scale and shake up, be the standard solution of concentration 0.2mg/mL.Accurately draw white birch alcohol ester standard items methanol solution 0.00,0.10,0.20,0.30,0.40,0.50,0.60,0.70mL, add respectively in the tool plug test tube of 10mL, the water-bath volatilization is solvent to the greatest extent, water bath method adds the perchloric acid of 5% vanillic aldehyde of the fresh configuration of 0.3mL-glacial acetic acid solution and 1mL, 60 ℃ of reflections 20 minutes, the frozen water cooling, add glacial acetic acid to 10mL, shake up, under the 551nm wavelength, measure absorbance.And take betulin concentration as abscissa, absorbance is ordinate, is depicted as calibration curve.Obtaining regression equation by calibration curve is y=0.0086x+0.0133, R
2=0.9998, y is absorbance, and x is betulin concentration, μ g/mL.
Measure the triterpene content of embodiment 1 to 3, what take by weighing respectively 10mg is that the saccharicter-penin of embodiment 1 to 3 is dissolved in the methyl alcohol of 10mL, make the saccharicter-penin ethanolic solution of 1mg/mL, precision is measured the saccharicter-penin ethanolic solution of 1mL, behind the drying with water bath, the perchloric acid that adds freshly prepared 5% vanillic aldehyde of 0.3mL-glacial acetic acid solution and 1mL, 60 ℃ were reacted 20 minutes, and the frozen water cooling adds glacial acetic acid to 10mL, shake up, under the 551nm wavelength, measure absorbance.Obtain light absorption value substitution regression equation, obtain as calculated the triterpene content results, measurement result is as shown in table 2.
The assay result of triterpene in the saccharicter-penin that table 2 embodiment 1 to 3 obtains
| Embodiment | Absorbance | Triterpene concentration (μ g/mL) | Contain triterpene percentage amounts (%) |
| Embodiment 1 | 0.2756 | 30.5 | 30.5 |
| Embodiment 2 | 0.2816 | 31.2 | 31.2 |
| Embodiment 3 | 0.2696 | 29.8 | 29.8 |
Claims (7)
1. the extracting method of an antivirus somatotropic agent saccharicter-penin is characterized in that, comprises following steps,
S1. get the Extracted From Oil-tea-cake cake, pulverize;
S2. add water, heating, ultrasonic wave extracts, and gets extract,
S3. concentrated extracting solution gets concentrate,
S4. dry concentrate, and get final product.
2. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, is heated to 60 ~ 80 ℃ among the described step S2.
3. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, the hyperacoustic power among the described step S2 is 400W ~ 6000W, and the time is 5 ~ 15 minutes.
4. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, the number of times of the extraction among the described step S2 is 2 ~ 5 times, and the time of extraction is 1 ~ 4 hour.
5. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, is ground into 30 ~ 40 orders among the described step S1.
6. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, the simmer down to reduced pressure concentration among the described step S3, described decompression for reduce to-0.080MPa ~-0.099MPa.
7. the extracting method of antivirus somatotropic agent saccharicter-penin according to claim 1 is characterized in that, the drying among the described step S4 is the fluidization and spray-drying method.
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Cited By (8)
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| CN103859236A (en) * | 2014-04-02 | 2014-06-18 | 太仓市永发农场专业合作社 | Chicken feed with high nutrient ingredients |
| CN104431358A (en) * | 2014-11-28 | 2015-03-25 | 国家粮食局科学研究院 | System and method for treating liquid phase obtained in process course of extracting camellia oleosa seed oil by adopting aqueous enzymatic method |
| CN104585551A (en) * | 2015-02-02 | 2015-05-06 | 贵阳双胞胎饲料有限公司 | Pig feed additive for effectively improving intestinal health and enhancing immunity |
| CN106172124A (en) * | 2016-07-15 | 2016-12-07 | 杭州千岛湖鲟龙科技股份有限公司 | A kind of artificial breeding method of Europe, southern area huso sturgeon |
| CN109077185A (en) * | 2018-08-28 | 2018-12-25 | 湖南大三湘茶油股份有限公司 | The preparation method of natural saccharicter-penin |
| CN110946114A (en) * | 2019-12-06 | 2020-04-03 | 福建正大食品有限公司 | Camellia chicken feeding method |
| CN114130061A (en) * | 2021-11-29 | 2022-03-04 | 湖南省康多利油脂有限公司 | Device and method for efficiently extracting water-soluble saccharicterpenin |
| CN115521943A (en) * | 2022-10-10 | 2022-12-27 | 湖南文理学院 | Method for extracting saccharicterpenin from oil tea cake |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103859236A (en) * | 2014-04-02 | 2014-06-18 | 太仓市永发农场专业合作社 | Chicken feed with high nutrient ingredients |
| CN104431358A (en) * | 2014-11-28 | 2015-03-25 | 国家粮食局科学研究院 | System and method for treating liquid phase obtained in process course of extracting camellia oleosa seed oil by adopting aqueous enzymatic method |
| CN104585551A (en) * | 2015-02-02 | 2015-05-06 | 贵阳双胞胎饲料有限公司 | Pig feed additive for effectively improving intestinal health and enhancing immunity |
| CN106172124A (en) * | 2016-07-15 | 2016-12-07 | 杭州千岛湖鲟龙科技股份有限公司 | A kind of artificial breeding method of Europe, southern area huso sturgeon |
| CN109077185A (en) * | 2018-08-28 | 2018-12-25 | 湖南大三湘茶油股份有限公司 | The preparation method of natural saccharicter-penin |
| CN110946114A (en) * | 2019-12-06 | 2020-04-03 | 福建正大食品有限公司 | Camellia chicken feeding method |
| CN114130061A (en) * | 2021-11-29 | 2022-03-04 | 湖南省康多利油脂有限公司 | Device and method for efficiently extracting water-soluble saccharicterpenin |
| CN115521943A (en) * | 2022-10-10 | 2022-12-27 | 湖南文理学院 | Method for extracting saccharicterpenin from oil tea cake |
| CN115521943B (en) * | 2022-10-10 | 2024-05-14 | 湖南文理学院 | Method for extracting saccharicterpenin from oil tea cake |
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Application publication date: 20130403 |