CN1754883A - Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent - Google Patents
Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent Download PDFInfo
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Abstract
The preparation method to extract tea saponin from oil meal, which comprises smashing, removing enzyme, leaching with hot mixing to boost infiltration capacity, centrifugal solid-liquid separating to add flocculant, deposition separating, disc centrifugal separating for cleaning solution, prefiltration separating for flocculation deposition, nano-membrane concentrating, and spray drying. Wherein, using chemical treatment to inhibit and eliminate hydrolase activity before leaching. This invention is simple and low cost with yield more than 70% and 80% purity.
Description
Technical field
The present invention relates to a kind of production method of from cake of camellia oleifera seeds, extracting tea saponin, particularly a kind ofly use water as solvent extracts tea saponin from cake of camellia oleifera seeds production method.
Background technology
Oil tea is the distinctive woody oleiferous plants of China, also is the oil crops that China greatly develops, and the comprehensive utilization value of oil tea is very high, and the tea seed grouts behind the process system oil contain the sasanguasaponin of about 10-15%, i.e. tea saponin.Tea saponin is a kind of nonionic surface active agent, has the performance of emulsification, dispersion, moistening, foaming, and pharmacological actions such as impervious, anti-inflammatory, analgesia are arranged, and sterilizing pesticide is arranged and stimulate the function of certain plants growth.Therefore, can be used for producing emulsifying agent, washing composition, whipping agent, sanitas, sterilant and other pharmaceuticals.China has the maximum country of resources of tea saponin in the world.
The general employing with water-containing solvents such as methyl alcohol or ethanol of suitability for industrialized production tea saponin extracted at present, but extraction time increases, the product yield is not high, and solvent has certain toxicity, reasons such as equipment requirements and tooling cost height.One ton of powdery tea saponin that contains about 70% of every aborning production consumes the about 0.8-1.5 ton of alcohol amount, the production cost height.
In fact sasanguasaponin is a kind of water-soluble fabulous material, it is easier to dissolving in water than in pure equal solvent, and show according to secular application experiment, only depend on and change solvent to improve the limitation of aspect performance index such as product yield, purity very big, therefore only manage to solve with water and to be the re-refine defective of process of solvent extraction sasanguasaponin, it is more feasible just to seem in actual production.
The extraction of tea saponin and be applied in existing years of researches of China and practice is to be solvent extraction oil tea saponin (abbreviation water extraction) with water the earliest.In leaching process, because there are a large amount of starch pasting that make in the tea seed in water, the protein colloidization causes the solid-liquid separation difficulty, and the product water-absorbent is very strong, and toughness requires the drying temperature height, tends to make the rotten decomposition of saponin, color burn.Not only difficulty is big for water extract evaporation concentration, and the energy consumption height.Present water extraction method gained tea saponin, purity is low, and color and luster is pitch black, and viscosity is big, and content is not high, thereby has limited the application of tea saponin.
In recent years, some had also once been carried out in this area is the research work of re-refining behind the solvent extraction sasanguasaponin with water, for example adopt the oil tea cake heating will put into encloses container to boost to pre-treatment such as 0.2-1.2Mpa after, use flooding; Water is carried after evaporation concentration is the adsorbents adsorb tea saponin with silica gel again, and then comes refined theasapogenin with the eluting solvent desorb; Come refined theasapogenin with absorption with macroporous adsorbent resin, desorb in addition, but these methods are all existing defectives such as the product yield is low, tooling cost is high, facility investment is big in varying degrees, be difficult to do large-scale industrialization and promote.Also the someone imagines and earlier removes macromolecular substance (as protein, glucide etc.) with prefilter, and small-molecule substance (as water, solvent etc.) is removed with ultra-filtration membrane in the back, obtains the tea saponin slurry.Ultra-filtration membrane is fit to separation, purifying and concentrated macromolecular substance.But the vat liquor that does not solve water as solvent is easy to stop up the problem of filter membrane, and it is higher to contain tea saponin during ultrafiltration process concentrates and discards mutually, causes waste.
From present disclosed document, also be not concerned about the problem of tea saponin hydrolysis in the water extraction production process.Tea saponin has glucoside and is easily generated the general character sugared and glucoside unit by diluted acid or enzymic hydrolysis.After glucoside was hydrolyzed into glucoside unit, solubleness in water and curative effect often greatly reduced, and must be noted that when therefore adopting water extraction to prevent hydrolysis.
Realize that water extraction suitability for industrialized production tea saponin must solve following key issue: (1) effectively suppresses even eliminates the hydrolysis of tea saponin; (2) effectively remove impurity such as carbohydrate in the vat liquor, protein, starch, pectin; (3) efficiently concentrate vat liquor, improve productive rate.Up to the present, these three key issues still do not solve, and also do not realize water extraction suitability for industrialized production tea saponin.
Summary of the invention
The objective of the invention is to solve above-mentioned key issue, so provide a kind of improve the quality of products and be suitable for industrial applications, use water as solvent extracts tea saponin from tea oilseedsand cake method.Adopt that this method facility investment is little, production cost is low, tea saponin extraction yield height, product purity height.
In order to realize the foregoing invention purpose, the technical solution adopted in the present invention is: a kind of use water as solvent from cake of camellia oleifera seeds, extract tea saponin production method, may further comprise the steps:
1, pulverize: the tea oilseedsand cake that will remove behind the grease is crushed to 40～100 orders;
2, dezymotize: in tea dregs of rice powder, add tea dregs of rice grain weight amount 0.3-0.5% and dezymotize agent and 0.3-0.5% slight alkalinity material, to eliminate, to suppress the activity of lytic enzyme in the tea dregs of rice powder;
3, hot dipping is carried: tea dregs of rice powder is put into the container of taking advantage of hot water, and the hot water amount is 2-3 a times of tea oilseedsand cake amount, and temperature is 30～50 ℃; The back insulation that stirs was soaked after 1.5～2.0 hours; Separate while hot through soaking the back material, obtain filtrate and filter residue; The gained filter residue repeats 1～2 time by immersion, the separation method of above-mentioned steps, and each gained filtrate exchange becomes parting liquid, and the filter residue oven dry obtains byproduct;
4, settlement separate: as, after stirring, to leave standstill more than 1 hour with adding separating filtrate weight 1-2% flocculation agent in the 3rd step gained parting liquid;
5, separate:, must contain the light phase of clarifying extracting solution and the heavy phase that contains carbohydrate, protein, starch with the filtrate of disk centrifuge separation through the 4th step gained;
6, pre-filtering:, must contain the light phase and the heavy phase that contains macromolecular substance such as carbohydrate, protein of tea saponin solution with the light phase of prefilter filtration through the 5th step gained;
7, press filtration: with the heavy phase of the 5th step of pressure filter press filtration and the 6th step gained, the light phase of the 6th step gained is gone in the filtrate exchange, obtain clarifying extracting solution, filter residue is dried and is obtained byproduct;
8, concentrate: use the extracting solution of the nanofiltration device of nanofiltration membrane material making, remove small-molecule substance in 0.3-1.0Mpa pressure range inner filtration the 7th step; When tea saponin concentration surpasses 10%, add the discoloring agent of concentrated solution weight 1-2%, continue to concentrate, must contain the concentrated solution of 1 5-30% tea saponin, filtrate can be used as solvent and is used for third step;
9, drying: will promptly get refined theasapogenin through the concentrated solution spraying drying powder-forming after the 8th step.
The agent of dezymotizing that the present invention adopts is stupid sodium formiate, and the slight alkalinity material is ammonia or soda or sodium bicarbonate.
The present invention compared with prior art has following advantage:
1, dezymotizes agent, slight alkalinity material with adding,, prevent the tea saponin hydrolysis effectively to reach the activity of elimination, inhibition tea saponin lytic enzyme.
2, adopt disc separator and filter process filtrate, removed macromole foreign material such as carbohydrate, starch, protein effectively,, improved product purity, realized the suitability for industrialized production of tea saponin water extraction for the nanofiltration concentrated filtrate provides condition.
3, with pressure filter press filtration heavy phase, the filtrate that obtains can exchange be gone into the isolating light phase of disc separator, has improved the rate of recovery of tea saponin, filter residue and drying get final product protein fodder, fully utilized tea oilseedsand cake.
4, use the nanofiltration membrane concentrated filtrate, saved energy consumption, improved the rate of recovery of tea saponin.To be concentrated by the saponin solution that flooding obtains by the sodium filter membrane method, technological process is short, effective, and saponin liquid cycles of concentration greatly reduces aspect the power consumption than the mode of past by evaporation concentration more than 10 times.The tea saponin rate of recovery of sodium filter method is than the height of ultrafiltration process, and energy consumption and flux are but very approaching.
4, no longer with an organic solvent, thereby need not anti-flamingly in each side such as technology, equipment, electrical equipment, civil engineerings, explosion-proof design does not have any pollution to environment, so just greatly reduces investment and running cost and helps improving the security of production.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
Take by weighing the tea seed grouts 6kg of degreasing, after pulverizer is pulverized, with the activity of lytic enzyme in the method for chemical treatment inhibition elimination tea dregs of rice powder, promptly in tea dregs of rice powder, add the stupid sodium formiate of tea dregs of rice grain weight amount 0.3% and 0.5% yellow soda ash, soaked 1.5 hours with 45 ℃ of tap water 12kg of temperature again; Link-suspended basket centrifuge soaks residue 1 time after separating vat liquor more as stated above, gets filtrate 23.2kg altogether; Filtrate is introduced settlement separate groove, adds 90g flocculation agent (50% alum, 40% poly-chitose, 10% iron(ic) chloride), after stirring, leaves standstill 1 hour; Clear liquor 23.0Kg got gently phase and heavy phase by disc separator after 10 minutes; Heavy phase through pressure filter, and is gone into light phase with the filtrate exchange, altogether clarifying extracting solution (tea saponin solution) 22.2kg, slag 0.8kg carefully.The nanofiltration membrane area is 2m
2, molecular weight cut-off is according to being designated as 1000, and intake pressure is 0.5Mpa, and nanofiltration concentrated after 0.5 hour, added concentrated solution weight 0.3%H
2O
2Obtained enriched material 2.7kg after the nanofiltration separation, nanofiltration water 19.5kg through 1 hour.Dry-matter is 21.8% in the enriched material, and the tea salidroside content is 85.3% in dry-matter.
Obtain content behind the said process and be 85.3% tea saponin 0.59kg, the tea saponin yield is 24.7%.The nanofiltration method of enrichment can make extracting solution be concentrated to by 22.2kg to be 2.7kg, concentrates 8.2 times, and the concentrated solution that obtains can directly carry out spraying drying at last.
Embodiment 2:
Take by weighing tea seed grouts 10kg, after pulverizer is pulverized,, promptly in tea dregs of rice powder, add the stupid sodium formiate of tea dregs of rice powder 0.3% and 0.5% yellow soda ash with the activity of lytic enzyme in the method for chemical treatment inhibition elimination tea dregs of rice powder; 40 ℃ of tap water 20kg soaked 2.0 hours with temperature; Link-suspended basket centrifuge soaks residue 1 time after separating vat liquor more as stated above, gets filtrate 38.7kg altogether; Filtrate is introduced settlement separate groove, adds 150g flocculation agent (50% alum, 40% poly-chitose, 10% iron(ic) chloride), leaves standstill 1 hour; 38.3Kg clear liquor by disc separator, got gently phase and heavy phase after 17 minutes; Will be gently pass through prefilter mutually, heavy phase is gone into light phase through pressure filter with the filtrate exchange, altogether clarifying extracting solution (tea saponin solution) 36.9kg, slag 1.4kg carefully.The nanofiltration membrane area is 2m
2, molecular weight cut-off is according to being designated as 1000, and intake pressure is 0.4Mpa, and nanofiltration concentrated after 1 hour, added concentrated solution weight 0.3%H
2O
2Obtained enriched material 4.2kg after the nanofiltration separation, nanofiltration water 32.7kg through 2 hours.Dry-matter is 23.1% in the enriched material, and saponin content is 86.4% in dry-matter.
Obtain content behind the said process and be 86.4% tea saponin 0.97kg, the tea saponin yield is 74.8%.The nanofiltration method of enrichment to 4.2Kg, has concentrated 8.8 times with 36.9Kg tea saponin solution concentration, and the concentrated solution that obtains can directly carry out spraying drying at last.
Claims (5)
1, a kind ofly use water as solvent extracts tea saponin from cake of camellia oleifera seeds production method, may further comprise the steps:
(1), pulverize: the tea oilseedsand cake that will remove behind the grease is crushed to 40～100 orders;
(2), dezymotize: in tea dregs of rice powder, add tea dregs of rice grain weight amount 0.3-0.5% and dezymotize agent and 0.3-0.5% slight alkalinity material;
(3), hot dipping is carried: tea dregs of rice powder is put into the container of taking advantage of hot water, and the hot water amount is 2-3 a times of tea oilseedsand cake amount, and temperature is 30～50 ℃; The back insulation that stirs was soaked after 1.5～2.0 hours; Separate while hot through soaking the back material, obtain filtrate and filter residue; The gained filter residue repeats 1～2 time by immersion, the separation method of above-mentioned steps, and each gained filtrate exchange becomes parting liquid, and the filter residue oven dry obtains byproduct;
(4), settlement separate: as, after stirring, to leave standstill more than 1 hour with adding separating filtrate weight 1-2% flocculation agent in the 3rd step gained parting liquid;
(5), separate:, must contain the light phase of clarifying extracting solution and the heavy phase that contains carbohydrate, protein, starch with the filtrate of disk centrifuge separation through the 4th step gained;
(6), pre-filtering:, must contain the light phase and the heavy phase that contains macromolecular substance such as carbohydrate, protein of tea saponin solution with the light phase of prefilter filtration through the 5th step gained;
(7), press filtration: with the heavy phase of the 5th step of pressure filter press filtration and the 6th step gained, the light phase of the 6th step gained is gone in the filtrate exchange, obtain clarifying extracting solution, filter residue is dried and is obtained byproduct;
(8), concentrate: use the extracting solution of the nanofiltration device of nanofiltration membrane material making, remove small-molecule substance in 0.3-1.0Mpa pressure range inner filtration the 7th step; When tea saponin concentration surpasses 10%, add the discoloring agent of concentrated solution weight 1-2%, continue to concentrate, must contain the concentrated solution of 15-30% tea saponin, filtrate can be used as solvent and is used for third step;
(9), drying: will promptly get refined theasapogenin through the concentrated solution spraying drying powder-forming after the 8th step.
2, a kind of solvent extracts tea saponin from cake of camellia oleifera seeds production method that uses water as according to claim 1 is characterized in that: described to dezymotize agent be stupid sodium formiate, and the slight alkalinity material is ammonia or soda or sodium bicarbonate.
3, a kind of solvent extracts tea saponin from cake of camellia oleifera seeds production method that uses water as according to claim 1, it is characterized in that: described flocculation agent is made up of the alum of 50% weight part, the glycan shell and 10% iron(ic) chloride of 40% weight part.
4, according to claim 1 or 2 or 3 described a kind of solvent extracts tea saponin from cake of camellia oleifera seeds production methods that use water as, it is characterized in that: employed nanofiltration membrane area is 2m
2, molecular weight cut-off is according to being designated as 1000, and intake pressure is 0.4Mpa.
5, according to claim 1 or 2 or 3 described a kind of solvent extracts tea saponin from cake of camellia oleifera seeds production methods that use water as, it is characterized in that: in enrichment step, nanofiltration concentrated after 0.5-1 hour, added the H of concentrated solution weight 0.3%
2O
2
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Cited By (18)
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| CN100431424C (en) * | 2006-12-06 | 2008-11-12 | 福州大学 | Preparation method and use of a fish toxic made of tea saponin |
| 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 |
| CN101070334B (en) * | 2007-06-21 | 2010-12-29 | 复旦大学 | Process for separating tea sapogenin and tea polysaccharide from tea-oil cake |
| CN102028042A (en) * | 2010-10-28 | 2011-04-27 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN101531690B (en) * | 2009-04-28 | 2011-09-14 | 浙江神茗山茶业科技有限公司 | New technology for extracting tea saponin and tea seed oil from tea seeds by using water as solvent |
| CN101167507B (en) * | 2006-10-24 | 2011-11-02 | 株式会社伊藤园 | Method for preparing tea extraction liquor |
| CN103880914A (en) * | 2014-03-04 | 2014-06-25 | 陕西科技大学 | Flocculation extraction method of diosgenin |
| CN104151377A (en) * | 2014-08-07 | 2014-11-19 | 雷炳忠 | Technology and method for extraction of teasaponin from Camellia oleifera Abel seed meal |
| 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 |
| CN105558160A (en) * | 2015-12-28 | 2016-05-11 | 安徽农业大学 | Application of tea tree flower extract in improving foaming properties of tea leaves and tea products |
| CN106377458A (en) * | 2016-10-14 | 2017-02-08 | 佛山市梦莎美容化妆品有限公司 | Shampoo composition containing tea seed cake extracts and preparation method thereof |
| CN106420463A (en) * | 2016-10-14 | 2017-02-22 | 佛山市梦莎美容化妆品有限公司 | Preparation method of tea seed cake extract |
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| CN109336945A (en) * | 2018-11-23 | 2019-02-15 | 重庆理工大学 | Tea Saponin water mentions-foam separation method and foam separator in cake of camellia oleifera seeds |
| CN109679788A (en) * | 2019-01-30 | 2019-04-26 | 江苏安心养老服务股份有限公司 | The preparation method and applications of tea seed cake detergent |
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| CN111304662A (en) * | 2020-04-10 | 2020-06-19 | 湖南淳湘农林科技有限公司 | Preparation method of tea seed cake cleaning agent |
| CN113801172A (en) * | 2021-09-14 | 2021-12-17 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
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- 2004-10-01 CN CN 200410046824 patent/CN100522982C/en not_active Expired - Fee Related
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| CN101167507B (en) * | 2006-10-24 | 2011-11-02 | 株式会社伊藤园 | Method for preparing tea extraction liquor |
| CN100431424C (en) * | 2006-12-06 | 2008-11-12 | 福州大学 | Preparation method and use of a fish toxic made of tea saponin |
| CN101070334B (en) * | 2007-06-21 | 2010-12-29 | 复旦大学 | Process for separating tea sapogenin and tea polysaccharide from tea-oil cake |
| CN101531690B (en) * | 2009-04-28 | 2011-09-14 | 浙江神茗山茶业科技有限公司 | New technology for extracting tea saponin and tea seed oil from tea seeds by using water as solvent |
| 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 |
| CN101830948B (en) * | 2010-05-11 | 2013-01-23 | 武汉工业学院 | Method for preparing tea saponin by using tea seed degreased dreg |
| CN102028042A (en) * | 2010-10-28 | 2011-04-27 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN102028042B (en) * | 2010-10-28 | 2013-01-02 | 福建省尤溪县沈郎食用油有限公司 | Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake |
| CN103880914B (en) * | 2014-03-04 | 2016-05-18 | 陕西科技大学 | A kind of flocculation extracting method of Chinese yam saponin |
| CN103880914A (en) * | 2014-03-04 | 2014-06-25 | 陕西科技大学 | Flocculation extraction method of diosgenin |
| CN104151377A (en) * | 2014-08-07 | 2014-11-19 | 雷炳忠 | Technology and method for extraction of teasaponin from Camellia oleifera Abel seed meal |
| 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 |
| CN105558160A (en) * | 2015-12-28 | 2016-05-11 | 安徽农业大学 | Application of tea tree flower extract in improving foaming properties of tea leaves and tea products |
| CN106377458A (en) * | 2016-10-14 | 2017-02-08 | 佛山市梦莎美容化妆品有限公司 | Shampoo composition containing tea seed cake extracts and preparation method thereof |
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| CN109336945A (en) * | 2018-11-23 | 2019-02-15 | 重庆理工大学 | Tea Saponin water mentions-foam separation method and foam separator in cake of camellia oleifera seeds |
| CN109336945B (en) * | 2018-11-23 | 2021-06-01 | 重庆理工大学 | Water extraction-foam separation method and foam separation device for tea saponin in oil-tea-cake meal |
| CN109679788A (en) * | 2019-01-30 | 2019-04-26 | 江苏安心养老服务股份有限公司 | The preparation method and applications of tea seed cake detergent |
| CN110305227A (en) * | 2019-07-26 | 2019-10-08 | 江西农业大学 | A kind of taro mucus and taro starch and its co-production |
| CN111304662A (en) * | 2020-04-10 | 2020-06-19 | 湖南淳湘农林科技有限公司 | Preparation method of tea seed cake cleaning agent |
| CN113801172A (en) * | 2021-09-14 | 2021-12-17 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
| CN113801172B (en) * | 2021-09-14 | 2022-09-06 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
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