CN105175462A - Process for extracting stevioside by percolation method - Google Patents
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Abstract
The invention provides a process for extracting stevioside by a percolation method. The process comprises the following steps of (1) carrying out extraction; (2) regulating extract with an alkaline solution; (3) filtering clear liquid; (4) passing filtrate through columns for adsorbing; (5) washing the columns with alkali; (6) washing the columns with water; (7) washing the columns with acid; (8) washing the columns with water; (9) resolving the columns with alcohol; (10) concentrating the collected alcohol; (11) carrying out desalination and decolorization treatment; (12) passing the substance obtained in the step (11) through refined resin; and (13) decolorizing the substance obtained in the step (12) with activated carbon. According to the method, the processes of alkali regulation, alkalization, impurity removal with acid, alcohol elution, solvent reclamation, serial passing through of desalination, decolorization and refined resin and activated carbon decolorization are conducted to directly obtain raw sugar which has a total sugar of over 95 percent and RA of over 60 percent.
Description
Technical field
The present invention relates to a kind of technique extracting stevioside, especially relate to the technique that a kind of percolation extracts stevioside.
Background technology
Sweet Stevia (SteviarebaudinanBetroni) belongs to composite family Stevia per nnial herb, originates in Amambay and the Mbaxacayu mountain range of Paraguay.Sweet Stevia, as novel sugared source plant, just once caused attention when World War II.Within 1970, Japan tames, cultivates, refines sugar from Brazil introduces a fine variety, carries out the experiment such as toxicity, food inspection simultaneously.China is in 1976 from Japanese successful introduction, and also there are Extend culture in various degree in current Korea S, Thailand, Philippines etc.Sweet Stevia happiness temperature, be feverfew, having widely should kind property.
Steviosides, it is a kind of new type natural green food additive, it is the natural sweeteners closest to sucrose sweet taste that the world today has found, it has the four characteristicses such as sugariness high (more than 300 times for sucrose), heat low (being only 1/300 of sucrose), safe and reliable and medicinal health value be high, and is widely used in the industries such as domestic and international food, medicine and light industry.Within 1984, stevioside is listed among " national development of food industry outline in 2000 " by former national Economic and Trade Commission, and as giving priority to and promotion project.Within 1985, health ministry official approval Steviosides uses as foodstuff additive.Steviol glycoside comprises Lay bud enlightening glycosides A(and RA), RA refers to RebaudiosideA, namely A3; RA component is sweet taste component the most excellent in stevioside, and form by recrystallization technology is refining from common stevioside, mouthfeel is pure and fresh in bitter taste, sugariness be 300-400 times of sucrose and taste matter closer to sucrose.But the method for current extraction of steviosides RA, be that Folium Chrysanthemi is refined through operations such as lixiviate, absorption, decolouring, drying and formed.In the method gained Steviosides RA product, Steviosides RA content is lower, and obtained stevioside specification is total reducing sugar 85%, Lay bud enlightening glycosides A(RA) 50%, can not meet the demands.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of percolation to extract the technique of stevioside, can obtain total reducing sugar more than 95% without refining, Lay bud enlightening glycosides A(RA) stevioside of more than 60% specification.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of percolation extracts the technique of stevioside, comprises the following steps:
(1) extract: by the series connection of more than 3 (preferred 4-6) extractors, each extractor is provided with charging opening, Stevia rebaudiana starting material is added respectively in each tank, add again and be equivalent to Stevia rebaudiana starting material weight 10-12 water doubly, extracting water temperature controls at 40-45 DEG C, lixiviate 6-12 hour, obtains extracting solution;
During extraction, preferred series connection continuous countercurrent seepage pressure effects: water is successively by the extractor of series connection, water is introduced into first extractor, first extractor completely afterwards namely the extracting solution of first tank out after overflow enter second tank as fresh solvent, the extracting solution of second tank out after enter the 3rd tank again, the rest may be inferred, and the extracting solution of last tank is out just final as extracting solution; This method is extracted more complete, and product yield is higher; And solvent used is few, more economizes on water, sewage quantity reduces 20%;
(2) alkali tune: adjust pH to be 10-11 step (1) gained extracting solution basic solution;
The preferred NaOH solution of described basic solution;
The present invention exempts flocculation step, and after alkali tune, extracting solution is stored in the basic conditions and is not easy to go bad;
(3) cleaner liquid: the extracting liquid filtering that will process through step (2), obtains filtrate;
(4) upper prop absorption: adopt three SpliteLX-T28 resin column series connection absorption, step (3) gained filtrate is per hour with flow velocity≤2BV/hr(column volume) successively by 3 adsorption resin columns, when extracting solution cross post pleasantly sweet to the 3rd pillar effluent liquid after stopped first, increase again adsorption column to after the 3rd, the rest may be inferred; After upper prop completes, every root SpliteLX-T28 resin column of upper prop is crossed the removal of impurities of 1-1.2 times of BV purified water;
(5) alkali cleaning: alkali lye step (4) gained resin column being crossed 0.3-0.7wt%, flow velocity is 1-1.5BVL/hr, and every root resin column elution amount is 3-4BV, removing impurity;
The preferred NaOH solution of described alkali lye;
(6) wash: the every root resin column processed through step (5) is crossed water 2-3BVL, and flow rate control is 1.8-2.0BVL/hr; Top lixiviating liquid;
(7) pickling: the acid solution resin column processed through step (6) being crossed 0.3-0.7wt%, flow velocity is 1-1.5BVL/hr, and every root resin column elution amount is 2-3BV; In and alkali lye;
The preferred HCl solution of described acid solution;
(8) wash: the every root resin column processed through step (7) is crossed water 2-3BVL to effluent liquid for neutral, flow rate control is 1.8-2BVL/hr; Top disacidify liquid;
(9) alcohol is resolved: be the ethanolic soln of 70-75% by the volumetric concentration that the every root resin column processed through step (8) crosses 4 ± 0.2 times of BV; After ethanolic soln drains, after washing every root resin column with the pure water of 70-80 DEG C of 5-6 times of column volume, liquid level in resin column is kept higher than resin column surface 4-5cm, to stop washing, for subsequent use;
(10) concentrated: by the ethanolic soln collected in step (9), adopt heating under vacuum to concentrate, vacuum tightness is-0.070MPa to-0.095MPa, and heating and temperature control, at 50 ~ 60 DEG C, reclaims ethanol, until without alcohol taste, obtains treating destainer;
(11) desalination, desolventing technology: step (10) gained is treated destainer is continuous in SepliteLX-T5 resin, D941 resin, D285 resin decolorization successively, flow velocity is 2 ± 0.1BV/h, collect and start pleasantly sweet omission timber; Three resins are washed to effluent liquid without sweet taste again with the 60-70 DEG C of purifying of 3-3.5BV; Omission timber, water lotion are merged, adopt heating under vacuum to concentrate, vacuum tightness be-0.070MPa extremely-0.095MPa, heating and temperature control at 60 ~ 80 DEG C, dry 8-12 hour; Put into oven drying again, keep oven temperature 75-85 DEG C, time of drying, 4-5h, obtained raw sugar;
(12) refining resin is crossed: step (11) gained raw sugar is mixed with the aqueous solution, in every 100ml aqueous solution, sugar degree is 15-20g, cross LX-69B afterwards to fat post, described resin column volume is equivalent to 1/4 ~ 1/3 of raw sugar aqueous solution volume, collects resin raw sugar effluent liquid;
Feed liquid residual on resin can directly be resolved with ethanol, recycles;
(13) activated carbon decolorizing: aqueous solution step (12) gained resin raw sugar effluent liquid being mixed with mass concentration 10-12%, add the decoloration active carbon being equivalent to raw sugar quality 5%-10%, 70-80 DEG C of stirring in water bath 30-35min, when destainer is cooled to room temperature, with the membrane filtration of 0.4 micron pore size, collect filtrate; Filtrate adopts heating under vacuum to concentrate, and vacuum tightness be-0.070MPa extremely-0.095MPa, heating and temperature control at 60 ~ 80 DEG C, dry 8-12 hour; Put into oven drying again, keep oven temperature 75-85 DEG C, time of drying, 4-5h, obtained more than total reducing sugar 95wt%, Lay bud enlightening glycosides A(RA) raw sugar of more than 60%.
The present invention adopts vacuum-drying to concentrate, and avoids using the purity of high temperature to product to have an impact.
The present invention adopts alkali tune, crosses alkali, sour removal of impurities, afterwards alcohol wash-out, and desalination of connecting again after recycling design, decolouring, refining resin, directly obtain the raw sugar of total reducing sugar more than 95%, more than RA60% after activated carbon decolorizing.Compare traditional technology, after extracting solution alkali tune, both can suppress microbial growth, extend the feed liquid shelf-time, also can accomplish not use flocculation agent simultaneously, avoid the residue problem using flocculation agent to cause; Adopt soda acid to wash away impurity by polymeric adsorbent, improve the content of product, not by process for refining, directly can obtain the raw sugar of total reducing sugar more than 95%, more than RA60%, this specification exceeds the specification of GB8270-2014 total reducing sugar 85%, reaches JECFA international standard.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) extract: by 3 extractor series connection, each extractor is provided with charging opening, adds Stevia rebaudiana starting material respectively in each tank, then adds the water being equivalent to Stevia rebaudiana starting material weight 10 times, and extract water temperature and control at 45 DEG C, lixiviate 6 hours, obtains extracting solution;
(2) alkali tune: adjust pH to be 10.1 step (1) gained extracting solution NaOH solution;
(3) cleaner liquid: the extracting liquid filtering that will process through step (2), obtains filtrate;
(4) upper prop absorption: adopt three SpliteLX-T28 resin column series connection absorption, step (3) gained filtrate is per hour with flow velocity 1BV/hr(column volume) successively by 3 adsorption resin columns, when extracting solution cross post pleasantly sweet to the 3rd pillar effluent liquid after stopped first, increase again adsorption column to after the 3rd; After upper prop completes, every root SpliteLX-T28 resin column of upper prop is crossed the removal of impurities of 1.2 times of BV purified water;
(5) alkali cleaning: NaOH solution step (4) gained resin column being crossed 0.7wt%, flow velocity is 1.5BVL/hr, and every root resin column elution amount is 4BV, removing impurity;
(6) wash: the every root resin column processed through step (5) is crossed water 3BVL, and flow rate control is 1.8BVL/hr; Top lixiviating liquid;
(7) pickling: the HCl solution resin column processed through step (6) being crossed 0.3wt%, flow velocity is 1BVL/hr, and every root resin column elution amount is 3BV; In and alkali lye;
(8) wash: the every root resin column processed through step (7) is crossed water 3BVL to effluent liquid for neutral, flow rate control is 1.8BVL/hr; Top disacidify liquid;
(9) alcohol is resolved: be the ethanolic soln of 75% by the volumetric concentration that the every root resin column processed through step (8) crosses 4 times of BV; After ethanolic soln drains, after washing every root resin column with the pure water of 80 DEG C of 5 times of column volumes, liquid level in resin column is kept higher than resin column surface 4-5cm, to stop washing, for subsequent use;
(10) concentrated: by the ethanolic soln collected in step (9), adopt heating under vacuum to concentrate, vacuum tightness is-0.070MPa, and heating and temperature control, at 60 DEG C, reclaims ethanol, until without alcohol taste, obtains treating destainer;
(11) desalination, desolventing technology: step (10) gained is treated destainer is continuous in SepliteLX-T5 resin, D941 resin, D285 resin decolorization successively, flow velocity is 2BV/h, collect and start pleasantly sweet omission timber; Three resins are washed to effluent liquid without sweet taste again with 70 DEG C of purifying of 3.5BV; By omission timber, water lotion merge, adopt heating under vacuum concentrate, vacuum tightness be-0.070MPaMPa, heating and temperature control at 80 DEG C, drying 8 hours; Put into oven drying again, keep oven temperature 85 DEG C, time of drying, 4h, obtained raw sugar;
(12) cross refining resin: step (11) gained raw sugar is mixed with the aqueous solution, and in every 100ml aqueous solution, sugar degree is 20g, cross LX-69B afterwards to fat post, described resin column volume is equivalent to 1/4 of raw sugar aqueous solution volume, collects resin raw sugar effluent liquid;
Feed liquid residual on resin can directly be resolved with ethanol, recycles;
(13) activated carbon decolorizing: aqueous solution step (12) gained resin raw sugar effluent liquid being mixed with mass concentration 12%, add the decoloration active carbon being equivalent to raw sugar quality 10%, 70 DEG C of stirring in water bath 30min, when destainer is cooled to room temperature, with the membrane filtration of 0.4 micron pore size, collect filtrate; Filtrate adopt heating under vacuum concentrate, vacuum tightness be-0.070MPaMPa, heating and temperature control at 80 DEG C, drying 8 hours; Put into oven drying again, keep oven temperature 85 DEG C, time of drying, 4h, obtained total reducing sugar 95.1wt%, Lay bud enlightening glycosides A(RA) raw sugar of 60.2%.
The test method standard of raw sugar content of the present invention: National Standard Method: " GB8270-2014 national food safety standard foodstuff additive steviol glycoside "; Jus gentium: " stevioside JECFA standard-American-European international standard ".
Embodiment 2
The present embodiment comprises the following steps:
(1) extract: by 6 extractor series connection, each extractor is provided with charging opening, adds Stevia rebaudiana starting material respectively in each tank, then adds the water being equivalent to Stevia rebaudiana starting material weight 12 times, and extract water temperature and control at 40 DEG C, each tank lixiviate 12 hours, obtains extracting solution;
During extraction, select series connection continuous countercurrent seepage pressure effects: water is successively by the extractor of series connection, water is introduced into first extractor, first extractor completely afterwards namely the extracting solution of first tank out after overflow enter second tank as fresh solvent, the extracting solution of second tank out after enter the 3rd tank again, the rest may be inferred, and the extracting solution of last tank is out just final as extracting solution; This method is extracted more complete, and product yield is higher; And solvent used is few, more economizes on water, sewage quantity reduces 20%;
(2) alkali tune: adjust pH to be 11 step (1) gained extracting solution NaOH solution;
(3) cleaner liquid: the extracting liquid filtering that will process through step (2), obtains filtrate;
(4) upper prop absorption: adopt three SpliteLX-T28 resin column series connection absorption, step (3) gained filtrate is per hour with flow velocity 1.5BV/hr(column volume) successively by 3 adsorption resin columns, when extracting solution cross post pleasantly sweet to the 3rd pillar effluent liquid after stopped first, increase again adsorption column to after the 3rd; After upper prop completes, every root SpliteLX-T28 resin column of upper prop is crossed the removal of impurities of 1.2 times of BV purified water;
(5) alkali cleaning: NaOH solution step (4) gained resin column being crossed 0.7wt%, flow velocity is 1.5BVL/hr, and every root resin column elution amount is 4BV, removing impurity;
(6) wash: the every root resin column processed through step (5) is crossed water 3BVL, and flow rate control is 2.0BVL/hr; Top lixiviating liquid;
(7) pickling: the HCl solution resin column processed through step (6) being crossed 0.7wt%, flow velocity is 1.5BVL/hr, and every root resin column elution amount is 3BV; In and alkali lye;
(8) wash: the every root resin column processed through step (7) is crossed water 3BVL to effluent liquid for neutral, flow rate control is 2BVL/hr; Top disacidify liquid;
(9) alcohol is resolved: be the ethanolic soln of 75% by the volumetric concentration that the every root resin column processed through step (8) crosses 4 times of BV; After ethanolic soln drains, after washing every root resin column with the pure water of 80 DEG C of 6 times of column volumes, liquid level in resin column is kept higher than resin column surface 4-5cm, to stop washing, for subsequent use;
(10) concentrated: by the ethanolic soln collected in step (9), adopt heating under vacuum to concentrate, vacuum tightness is-0.095MPa, and heating and temperature control, at 60 DEG C, reclaims ethanol, until without alcohol taste, obtains treating destainer;
(11) desalination, desolventing technology: step (10) gained is treated destainer is continuous in SepliteLX-T5 resin, D941 resin, D285 resin decolorization successively, flow velocity is 2BV/h, collect and start pleasantly sweet omission timber; Three resins are washed to effluent liquid without sweet taste again with 70 DEG C of purifying of 3.5BV; By omission timber, water lotion merge, adopt heating under vacuum concentrate, vacuum tightness be-0.095MPa, heating and temperature control at 60 DEG C, drying 12 hours; Put into oven drying again, keep oven temperature 85 DEG C, time of drying, 4h, obtained raw sugar;
(12) cross refining resin: step (11) gained raw sugar is mixed with the aqueous solution, and in every 100ml aqueous solution, sugar degree is 20g, cross LX-69B afterwards to fat post, described resin column volume is equivalent to 1/3 of raw sugar aqueous solution volume, collects resin raw sugar effluent liquid;
Feed liquid residual on resin can directly be resolved with ethanol, recycles;
(13) activated carbon decolorizing: aqueous solution step (12) gained resin raw sugar effluent liquid being mixed with mass concentration 10%, add the decoloration active carbon being equivalent to raw sugar quality 10%, 70 DEG C of stirring in water bath 30min, when destainer is cooled to room temperature, with the membrane filtration of 0.4 micron pore size, collect filtrate; Filtrate adopt heating under vacuum concentrate, vacuum tightness be-0.095MPa, heating and temperature control at 60 DEG C, drying 8 hours; Put into oven drying again, keep oven temperature 85 DEG C, time of drying, 5h, obtained total reducing sugar 95.2wt%, Lay bud enlightening glycosides A(RA) raw sugar of 60.1%.
Claims (6)
1. percolation extracts a technique for stevioside, it is characterized in that, comprises the following steps:
(1) extract: by more than 3 extractor series connection, each extractor is provided with charging opening, adds Stevia rebaudiana starting material respectively in each tank, add again and be equivalent to Stevia rebaudiana starting material weight 10-12 water doubly, extracting water temperature controls at 40-45 DEG C, and lixiviate 6-12 hour, obtains extracting solution;
(2) alkali tune: adjust pH to be 10-11 step (1) gained extracting solution basic solution;
(3) cleaner liquid: the extracting liquid filtering that will process through step (2), obtains filtrate;
(4) upper prop absorption: adopt three SpliteLX-T28 resin column series connection absorption, step (3) gained filtrate is passed through 3 adsorption resin columns successively with flow velocity≤2BV/hr, when extracting solution cross post pleasantly sweet to the 3rd pillar effluent liquid after stopped first, increase again adsorption column to after the 3rd, the rest may be inferred; After upper prop completes, every root SpliteLX-T28 resin column of upper prop is crossed the removal of impurities of 1-1.2 times of BV purified water;
(5) alkali cleaning: alkali lye step (4) gained resin column being crossed 0.3-0.7wt%, flow velocity is 1-1.5BVL/hr, and every root resin column elution amount is 3-4BV, removing impurity;
(6) wash: the every root resin column processed through step (5) is crossed water 2-3BVL, and flow rate control is 1.8-2.0BVL/hr; Top lixiviating liquid;
(7) pickling: the acid solution resin column processed through step (6) being crossed 0.3-0.7wt%, flow velocity is 1-1.5BVL/hr, and every root resin column elution amount is 2-3BV; In and alkali lye;
(8) wash: the every root resin column processed through step (7) is crossed water 2-3BVL to effluent liquid for neutral, flow rate control is 1.8-2BVL/hr; Top disacidify liquid;
(9) alcohol is resolved: be the ethanolic soln of 70-75% by the volumetric concentration that the every root resin column processed through step (8) crosses 4 ± 0.2 times of BV; After ethanolic soln drains, after washing every root resin column with the pure water of 70-80 DEG C of 5-6 times of column volume, liquid level in resin column is kept higher than resin column surface 4-5cm, to stop washing, for subsequent use;
(10) concentrated: by the ethanolic soln collected in step (9), adopt heating under vacuum to concentrate, vacuum tightness is-0.070MPa to-0.095MPa, and heating and temperature control, at 50 ~ 60 DEG C, reclaims ethanol, until without alcohol taste, obtains treating destainer;
(11) desalination, desolventing technology: step (10) gained is treated destainer is continuous in SepliteLX-T5 resin, D941 resin, D285 resin decolorization successively, flow velocity is 2 ± 0.1BV/h, collect and start pleasantly sweet omission timber; Three resins are washed to effluent liquid without sweet taste again with the 60-70 DEG C of purifying of 3-3.5BV; Omission timber, water lotion are merged, adopt heating under vacuum to concentrate, vacuum tightness be-0.070MPa extremely-0.095MPa, heating and temperature control at 60 ~ 80 DEG C, dry 8-12 hour; Put into oven drying again, keep oven temperature 75-85 DEG C, time of drying, 4-5h, obtained raw sugar;
(12) refining resin is crossed: step (11) gained raw sugar is mixed with the aqueous solution, in every 100ml aqueous solution, sugar degree is 15-20g, cross LX-69B afterwards to fat post, described resin column volume is equivalent to 1/4 ~ 1/3 of raw sugar aqueous solution volume, collects resin raw sugar effluent liquid;
(13) activated carbon decolorizing: aqueous solution step (12) gained resin raw sugar effluent liquid being mixed with mass concentration 10-12%, add the decoloration active carbon being equivalent to raw sugar quality 5%-10%, 70-80 DEG C of stirring in water bath 30-35min, when destainer is cooled to room temperature, with the membrane filtration of 0.4 micron pore size, collect filtrate; Filtrate adopts heating under vacuum to concentrate, and vacuum tightness be-0.070MPa extremely-0.095MPa, heating and temperature control at 60 ~ 80 DEG C, dry 8-12 hour; Put into oven drying again, keep oven temperature 75-85 DEG C, time of drying, 4-5h, to obtain final product.
2. percolation according to claim 1 extracts the technique of stevioside, it is characterized in that, in step (1), the extractor of series connection is 4-6.
3. percolation according to claim 1 and 2 extracts the technique of stevioside, it is characterized in that, in step (1), during extraction, select series connection continuous countercurrent seepage pressure effects: water is successively by the extractor of series connection, water is introduced into first extractor, first extractor completely afterwards namely the extracting solution of first tank out after overflow enter second tank as fresh solvent, the extracting solution of second tank out after enter the 3rd tank again, the rest may be inferred, and the extracting solution of last tank is out just final as extracting solution.
4. percolation according to claim 1 and 2 extracts the technique of stevioside, and it is characterized in that, in step (2), described basic solution is NaOH solution.
5. percolation according to claim 1 and 2 extracts the technique of stevioside, and it is characterized in that, in step (5), described basic solution is NaOH solution.
6. percolation according to claim 1 and 2 extracts the technique of stevioside, and it is characterized in that, in step (7), described acid solution is HCl solution.
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CN107118243A (en) * | 2017-06-05 | 2017-09-01 | 江苏史蒂文生物科技有限公司 | A kind of industrial production process of stevioside |
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CN107325137A (en) * | 2017-08-21 | 2017-11-07 | 内蒙古昶辉生物科技股份有限公司 | A kind of extracting method of steviol glycoside |
CN109354596A (en) * | 2018-10-09 | 2019-02-19 | 山东奥晶生物科技有限公司 | A kind of preparation method of efficient steviol glycoside |
CN111187315A (en) * | 2019-05-10 | 2020-05-22 | 上海悦然生物科技有限公司 | Extraction system and extraction process of stevioside |
CN111187315B (en) * | 2019-05-10 | 2023-03-14 | 上海悦然生物科技有限公司 | Extraction system and extraction process of stevioside |
CN110437290A (en) * | 2019-06-14 | 2019-11-12 | 中国林业科学研究院林产化学工业研究所 | A kind of steviol glycoside extracting and developing and purification process |
CN111153951A (en) * | 2020-01-07 | 2020-05-15 | 西安蓝晓科技新材料股份有限公司 | Novel method for producing stevioside |
WO2021216553A1 (en) * | 2020-04-20 | 2021-10-28 | Cargill, Incorporated | Increasing yield of steviol glycosides |
CN115666269A (en) * | 2020-04-20 | 2023-01-31 | 嘉吉公司 | Increasing yield of steviol glycosides |
US11944112B2 (en) | 2020-04-20 | 2024-04-02 | Cargill, Incorporated | Stabilized steviol glycoside malonic acid esters |
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