CN101979400A - Method for comprehensively extracting tea saponin and tea polysaccharide from camellia oil seed cake or tea seed cake - Google Patents
Method for comprehensively extracting tea saponin and tea polysaccharide from camellia oil seed cake or tea seed cake Download PDFInfo
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Abstract
The invention discloses a method for comprehensively extracting tea saponin and tea polysaccharide from a camellia oil seed cake or tea seed cake. In the method, a comprehensive extraction process for the tea saponin and the tea polysaccharide is researched by taking the degreased camellia oil seed cake or tea seed cake as raw materials. The method for extracting the tea saponin and tea polysaccharide comprises the following steps of: crushing the camellia oil seed cake or tea seed cake and performing water extraction and alcohol precipitation or alcohol extraction and water extraction to obtain rough tea saponin and tea polysaccharide; purifying the supernatant subjected to water extraction or alcohol extraction by using a macroporous adsorption resin chromatography column; eluting resin adsorbate with alkali and ethanol with gradually increasing volumetric concentration in turn; and collecting the ethanol eluent to obtain high-purity tea saponin. The method has a simple process and low production cost, and by the method, the high-purity tea saponin can be prepared and also another active product, namely the tea polysaccharide can be obtained.
Description
Technical field
The present invention relates to the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice.Belong to food, makeup and medical technical field.
Background technology
Oil tea is one of the world four big woody oleiferous plants plants, is that China originates in indigenous tree, and more than 2000 year cultivation history arranged.China is world's oil tea cultivated area maximum, output is the highest, the country that kind is the abundantest, according to statistics, about 5,000 ten thousand mu of the existing camellia oleifera lams of China, mainly be distributed in the low mountains and hills area of 14 provinces (district, city) in Huaihe River such as Zhejiang, Anhui, Fujian, Jiangxi, river, Hubei, Hunan, Guangdong, Guangxi, Chongqing, Sichuan, Yunnan, Guizhou, Shaanxi, south, the Changjiang river, wherein Hunan, Jiangxi provinces distribute at most, account for 2/3 of the national camellia oleifera lam total area.National annual about 1,060,000 tons of the tea seeds of producing, about 27.7 ten thousand tons of process for processing oil tea oil, the camellia seed meal after pre-press for extracting juice is leached is about 700,000 tons.Another and the equal generic raw material of tea seed are tea-seed.Tea-seed is the fruit of tea tree, is the by product of Tea Production.About 2,700 ten thousand mu of China's tealeaves cultivated area is produced more than 80 ten thousand tons of tea-seed per year, contains more than 10 ten thousand tons of greases, about 50,000 tons of tea saponin.
For a long time, people pay close attention to more for the exploitation of camellia seed oil and tea-seed oil, but not too pay attention to for the development and use of tea seed grouts and tea waste.Tea seed and tea-seed remaining residue behind the squeezing extracting edible oil is rich in multiple useful matter, as tea saponin, soluble polysaccharide, starch and protein etc.Containing 10%～16% saponin in the camellia seed meal or the tea-seed dregs of rice, is an important source of tea saponin, contains more rich polysaccharide and protein in addition, is a kind of good feed.Yet because the tea saponin bitter, to the toxic effect of cold blooded animal, present most of camellia seed meal is directly made pool-cleaning agent or fertilizer and is used, or cheapness exports to countries such as Japan, South East Asia, has caused the very big wasting of resources.Therefore, carry out the further investigation of the camellia seed meal or the tea-seed dregs of rice, from the camellia seed meal or the tea-seed dregs of rice, extract tea saponin and tea seed polysaccharide, forestry plantation, minor forest products comprehensive utilization and new product development etc. are all had crucial meaning.
Tea saponin is a kind of pure natural nonionic surface active agent, have functions such as emulsification, dispersion, wetting, decontamination, foaming and steady bubble, and not influenced by water hardness, be widely used in fields such as daily-use chemical industry, agricultural chemicals, medicine, food, building materials, gold metallurgy and metal material processing.Only with regard to this industry of shampoo, about 100 kilotons of China's shampoo gross annual output value, wherein half need add amendments such as tea saponin, needs amendment 1.0 kilotons altogether, and share of market is in 10%, year can sell 100 tons of amendments, 4,500,000 yuan of the output values.The tea saponin shade deviation of present most of plant produced, purity is low, can not satisfy the requirement of all trades and professions, has especially limited the application of tea saponin on medical technical field.
At present existing a lot of articles and patent disclosure be the method that raw material extracts tea saponin with the tea seed grouts, though these technologies have obtained bigger progress, the tea saponin quality product that obtains still can not satisfy the requirement in market.In addition, except that being rich in tea saponin, also contain a large amount of tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice, yet most people just study the extraction of tea saponin in the camellia seed meal or the tea-seed dregs of rice, have ignored the extraction of tea polysaccharide.Make the camellia seed meal or the tea-seed dregs of rice to be fully utilized, uselessly accomplish real change Fei Weibao.Tea polysaccharide is a kind of vegetable active polysaccharide, a kind of macromolecular compound of similar ganoderan and panaxan.Tea polysaccharide is except hypoglycemic, blood fat reducing function, also have other multiple efficacies such as anticoagulation and antithrombotic,, hypotensive, raise immunity, hypoxia tolerance and coronary blood flow increasing effect, radiation protection or the like, be a kind of very promising natural radioactivity product.
Summary of the invention
The objective of the invention is for the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice is provided,, improve the tea saponin color and luster simultaneously and improve tea saponin purity to remedy the above-mentioned deficiency of prior art.
Purpose of the present invention can be achieved through the following technical solutions.
The combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice, its concrete steps are as follows:
1) extraction of thick tea saponin and tea seed polysaccharide: get a certain amount of degreasing camellia seed meal or the tea-seed dregs of rice and pulverize, extracting in water twice, slagging-off after filtration gets water layer, use the 30-90% ethanol sedimentation, the precipitation supernatant liquor obtains tea saponin through recovery, concentrated and dry, and purity can reach 45-60%, resolution of precipitate is in water, drying obtains the tea seed polysaccharide, purity about 20%.
2) the thick tea seed polysaccharide of high-purity tea saponin and byproduct extracts: the clear liquid that step 1) gained water layer is contained tea saponin is in 45 ℃ of decompression recycling ethanols, be 3-5% back containing with consolidating of Abbe refractometer regulator solution, solution passes through macroporous adsorbent resin, effluent liquid is through concentrating, use the 30-90% ethanol sedimentation, resolution of precipitate is in water, drying, get the tea seed polysaccharide, purity is 25-30%.The resin absorption thing earlier with alkali, the ethanol elution that increases gradually with concentration again, reclaims solvent, concentrates, and drying must tea saponin, and purity reaches more than 80%.
Improvement technology as the said extracted method is:
1) extraction of thick tea saponin and tea seed polysaccharide: get a certain amount of degreasing camellia seed meal or the tea-seed dregs of rice and pulverize, add organic solvent or aqueous solutions of organic solvent and extract twice, after the extraction, after filtration, centrifugal, get supernatant and concentrate, drying promptly gets tea saponin, and purity has reached more than 60%; Precipitation is then used water extraction, and is centrifugal after filtration after the extraction, gets supernatant and concentrates, and ethanol sedimentation, resolution of precipitate are in water, and drying gets the tea seed polysaccharide, and purity is about 20%.
2) with in the step 1) with the clear liquid that contains tea saponin of the extraction with aqueous solution of organic solvent or organic solvent in 45 ℃ of decompression recycling ethanols, be 3-5% back containing with consolidating of Abbe refractometer regulator solution, solution stream is crossed macroporous adsorbent resin, the resin absorption thing earlier with alkali, the ethanol elution that increases gradually with volumetric concentration again, is collected ethanol eluate, the recovery solvent, concentrate, drying gets tea saponin, and purity reaches more than 85%.
The described camellia seed meal or the tea-seed dregs of rice are crushed to the 20-40 order.
The solid-liquid ratio that organic solvent or aqueous solutions of organic solvent extract is carried twice or added to described water is 1: 3-10, and temperature is 40-90 ℃, the time is 1.0-4.0h.
The organic solvent that described organic solvent or aqueous solutions of organic solvent extract is a kind of in methyl alcohol, ethanol, the propyl carbinol etc., aqueous solutions of organic solvent be by the volume ratio of organic solvent and water mixed, its concentration range is 50-90%.
Described ethanol sedimentation process is the vat liquor after merging to be concentrated into contain 15-30% admittedly, slowly adds the 30%-95% ethanol sedimentation, places 4-24h under the room temperature;
Described macroporous adsorbent resin is a kind of among HZ801, HZ816, HZ841, AB-8, D101, H103, D3520, NKA, X-5 and the ADS-7.
The step 2 of improvement technology) in the resin absorption thing is used the sodium hydroxide or the potassium hydroxide solution wash-out of 0.2% massfraction respectively, use the ethanol elution of 20%, 40%, 70% volume fraction more successively, the ethanol eluate of the volume fraction of collection 40% and 70% can get the high-purity tea saponin.
Described recovery solvent can adopt vacuum concentration method or distillation absorption method to reclaim.
Described spissated mode is vacuum rotating thin film method of enrichment, scraper plate method of enrichment or thin film concentration method.
The drying mode of described tea seed polysaccharide is vacuum lyophilization, vacuum-drying or air-dry.
The drying mode of described tea saponin is spraying drying, vacuum-drying or vacuum microwave drying.
The present invention has following advantage: 1) utilize alcohol collection, macroporous adsorption resin chromatography technology can prepare the high-purity tea saponin of purity more than 85%; 2) utilize water extraction and alcohol precipitation method or first alcohol extracting after water carry, can extract tea saponin and tea polysaccharide in the grouts simultaneously, make the comprehensive extraction of tea saponin, tea polysaccharide become possibility; 3) adopt filter operation behind the alcohol precipitation, can make tea polysaccharide purity improve about 5% with respect to centrifugally operated.And be easy to the alcoholic acid volatilization, reduced the concentrated recovery alcoholic acid time.
Embodiment
Further set forth technical characterstic of the present invention below in conjunction with specific embodiment.
Embodiment 1
Get the tea seed grouts 500g of pulverizing, 70 ℃ of water carry twice, and feed liquid when is respectively 1 heat-up time: 9/1.5h, 1: 5/1.5h, 300 orders filter, the centrifugal 15min of 4500rad/min.Merge the water extract, be evaporated to record in 60 ℃ and contain 15% admittedly, slowly add the industrial spirit of 1 times of volume, fully stir and place 4 ℃ of refrigerator alcohol precipitations to cross liquid with Abbe refractometer, 500 order filtering mixts obtain containing the clear liquid and the tea polysaccharide precipitation of tea saponin respectively.Behind the tea polysaccharide precipitation nature volatilization ethanol, lyophilize gets the tea polysaccharide crude product, and polysaccharide yield is 9.09%, and massfraction is 20.67%; The clear liquid that contains tea saponin is in 45 ℃ of decompression recycling ethanols, it is 3% that the back contains with consolidating of Abbe refractometer regulator solution, solution is after the AB-8 macropore is inhaled resin absorption, difference water, the sodium hydroxide, 20%, 40% of 0.2% mass concentration, the ethanol elution of 70% volumetric concentration, collect different elutriant freeze-drying respectively, 70% ethanol elution thing lyophilize gets the white crystal tea saponin of purity 83.5%, productive rate 4.76%.
Embodiment 2
Get the tea seed grouts 500g of pulverizing, 80 ℃ of extraction using alcohols twice, feed liquid when is respectively 1 heat-up time: 9/2.0h, 1: 5/1.0h, 300 orders filter, and contain under the alcohol extract reduced pressure of tea saponin, reclaim ethanol, vacuum-drying gets tea saponin, productive rate 18.29%, purity 68.79%; The slag that obtains after the filtration concentrates after twice water is carried carrying out under the same condition, merging water extract is evaporated in 60 ℃ and contains 30% admittedly, the industrial spirit that slowly adds 3 times of volumes, fully stir, alcohol precipitation is crossed liquid, 1000 order filter cloth filtering mixts, the throw out ethanol postlyophilization that volatilizees naturally, get the tea polysaccharide crude product, polysaccharide yield is 4.58%, and massfraction is 18.49%.
Embodiment 3
Get the tea-seed grouts 500g of pulverizing, twice of 80 ℃ of extraction using alcohol, feed liquid when is respectively 1 heat-up time: 9/2.0h, 1: 5/1.0h, 300 orders filter, the alcohol extract that contains tea saponin, alcohol extract flows through the AB-8 macroporous adsorbent resin, the resin absorption thing is water, the sodium hydroxide, 20%, 40% of 0.2% mass concentration, the ethanol elution of 70% volumetric concentration respectively, collect different elutriant freeze-drying respectively, 70% ethanol elution thing lyophilize, get the white crystal tea saponin of purity 89.6%, productive rate 4.95%.The slag that obtains after the filtration concentrates after twice water is carried carrying out under the same condition, merge the water extract, under the reduced pressure, be concentrated in 60 ℃ and contain 30% admittedly, slowly add the industrial spirit of 3 times of volumes, fully stir, alcohol precipitation is crossed liquid, and 1000 order filter cloth filtering mixts, the throw out ethanol postlyophilization that volatilizees naturally gets the tea polysaccharide crude product, polysaccharide yield is 4.34%, and massfraction is 25.65%.
Claims (13)
1. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice is characterized in that concrete steps are as follows:
1) extraction of thick tea saponin and tea seed polysaccharide: get a certain amount of degreasing camellia seed meal or the tea-seed dregs of rice and pulverize, extracting in water twice, slagging-off after filtration, get water layer, use the 30-90% ethanol sedimentation, supernatant liquor is through recovery, concentrated and dry, obtain tea saponin, purity can reach 45-60%; Resolution of precipitate is in water, and drying obtains the tea seed polysaccharide, and purity reaches 20%.
2) the thick tea seed polysaccharide of high-purity tea saponin and byproduct extracts: the clear liquid that step 1) gained water layer is contained tea saponin is in 45 ℃ of decompression recycling ethanols, be 3-5% back containing with consolidating of Abbe refractometer regulator solution, solution passes through macroporous adsorbent resin, effluent liquid is through concentrating, use the 30-90% ethanol sedimentation, resolution of precipitate is in water, drying, get the tea seed polysaccharide, purity is 25-30%.The resin absorption thing earlier with alkali, the ethanol elution that increases gradually with concentration again, reclaims solvent, concentrates, and drying must tea saponin, and purity reaches more than 80%.
2. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal or the tea-seed dregs of rice is characterized in that concrete steps are as follows:
1) extraction of thick tea saponin and tea seed polysaccharide: get a certain amount of degreasing camellia seed meal or the tea-seed dregs of rice and pulverize, add organic solvent or aqueous solutions of organic solvent and extract twice, after the extraction, after filtration, centrifugal, supernatant concentration, drying promptly gets tea saponin, and purity has reached more than 60%; Precipitation is then used water extraction, and is centrifugal after filtration after the extraction, gets supernatant concentration, and ethanol sedimentation, resolution of precipitate are in water, and drying gets the tea seed polysaccharide, and purity reaches 20%.
2) the thick tea seed polysaccharide of high-purity tea saponin and byproduct extracts: with in the step 1) with the clear liquid that contains tea saponin of the extraction with aqueous solution of organic solvent or organic solvent in 45 ℃ of decompression recycling ethanols, be 3-5% back containing with consolidating of Abbe refractometer regulator solution, solution stream is crossed macroporous adsorbent resin, the resin absorption thing earlier with alkali, the ethanol elution that increases gradually with volumetric concentration again, is collected ethanol eluate, the recovery solvent, concentrate, drying gets tea saponin, and purity reaches more than 85%.
3. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: the described camellia seed meal or the tea-seed dregs of rice are crushed to the 20-40 order.
4. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 or the tea-seed dregs of rice is characterized in that: it is 1 that described water is carried twice solid-liquid ratio: 3-10, and temperature is 40-90 ℃, the time is 1.0-4.0h.
5. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 2 or the tea-seed dregs of rice, it is characterized in that: the solid-liquid ratio that adds the extraction of organic solvent or aqueous solutions of organic solvent is 1: 3-10, temperature is 40-90 ℃, and the time is 1.0-4.0h.
6. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 5 or the tea-seed dregs of rice, it is characterized in that: the organic solvent that described organic solvent or aqueous solutions of organic solvent extract is a kind of in methyl alcohol, ethanol and the propyl carbinol, aqueous solutions of organic solvent is to get by the volume ratio of organic solvent and water is mixed, and its concentration range is 50-90%.
7. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice, it is characterized in that: described ethanol sedimentation is the vat liquor after merging to be concentrated into contain 15-30% admittedly, slowly add the 30%-95% ethanol sedimentation, place 4-24h under the room temperature.
8. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: described macroporous adsorbent resin is a kind of among HZ801, HZ816, HZ841, AB-8, D101, H103, D3520, NKA, X-5 and the ADS-7.
9. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 2 or the tea-seed dregs of rice, it is characterized in that: step 2) in the resin absorption thing is used the sodium hydroxide or the potassium hydroxide solution wash-out of 0.2% massfraction respectively, use the ethanol elution of 20%, 40%, 70% volume fraction more successively; The ethanol eluate of the volume fraction of collection 40% and 70% can get the high-purity tea saponin.
10. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: described recovery solvent, adopt vacuum concentration method or distillation absorption method to reclaim.
11. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: described is vacuum rotating thin film method of enrichment, scraper plate method of enrichment or thin film concentration method to the spissated mode of solvent.
12. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: the drying mode of described tea seed polysaccharide is vacuum lyophilization, vacuum-drying or air-dry.
13. the combined extraction method of tea saponin, tea polysaccharide in the camellia seed meal according to claim 1 and 2 or the tea-seed dregs of rice is characterized in that: the drying mode of described tea saponin is spraying drying, vacuum-drying or vacuum microwave drying.
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| CN102796203A (en) * | 2011-05-27 | 2012-11-28 | 中南林业科技大学 | Method for preparing anti-oxidization active camellia olefera cake polysaccharide |
| CN102993329A (en) * | 2012-12-31 | 2013-03-27 | 广西师范大学 | Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes |
| CN102993322A (en) * | 2012-11-21 | 2013-03-27 | 南昌大学 | Method for synchronously extracting proteins and polysaccharides from cold-pressed tea cakes |
| CN102993328A (en) * | 2012-12-31 | 2013-03-27 | 广西师范大学 | Method for comprehensively extracting polysaccharides, polyphenol and saponin from camellia oleifera abel defatted cakes |
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| CN106967144A (en) * | 2017-03-28 | 2017-07-21 | 钦州市桂耘贸易有限公司 | A kind of method that Tea Saponin is extracted from tea bran |
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| CN102796203B (en) * | 2011-05-27 | 2014-08-20 | 中南林业科技大学 | Method for preparing anti-oxidization active camellia olefera cake polysaccharide |
| CN102796203A (en) * | 2011-05-27 | 2012-11-28 | 中南林业科技大学 | Method for preparing anti-oxidization active camellia olefera cake polysaccharide |
| CN103182004A (en) * | 2011-12-30 | 2013-07-03 | 株式会社爱茉莉太平洋 | Composition for preventing or improving metabolic syndrome comprising tea llant leaf, flower and seed extract |
| CN103182004B (en) * | 2011-12-30 | 2019-03-15 | 株式会社爱茉莉太平洋 | Containing tealeaves, camellia and tea seed extract, for preventing or improving the composition of metabolic syndrome |
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| CN102993322A (en) * | 2012-11-21 | 2013-03-27 | 南昌大学 | Method for synchronously extracting proteins and polysaccharides from cold-pressed tea cakes |
| CN102993329A (en) * | 2012-12-31 | 2013-03-27 | 广西师范大学 | Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes |
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| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
| CN113337347A (en) * | 2021-05-31 | 2021-09-03 | 湖南万象生物科技有限公司 | Washing liquid prepared from defatted tea seed meal and preparation method thereof |
| CN114213500A (en) * | 2021-12-21 | 2022-03-22 | 湖北人人爱油脂有限公司 | Tea saponin, tea polysaccharide and tea protein purification process based on comprehensive extraction of camellia oleifera |
| CN114686552A (en) * | 2022-04-02 | 2022-07-01 | 吉林农业大学 | Preparation method of camellia seed meal polypeptide zinc chelate |
| CN114686552B (en) * | 2022-04-02 | 2024-04-30 | 吉林农业大学 | Preparation method of camellia seed meal polypeptide zinc chelate |
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