CN105175462B - A kind of technique of percolation extraction stevioside - Google Patents
A kind of technique of percolation extraction stevioside Download PDFInfo
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Abstract
A kind of technique of percolation extraction stevioside, comprises the following steps:(1)Extraction;(2)Alkali tune;(3)Cleaner liquid;(4)Upper prop adsorbs;(5)Alkali cleaning;(6)Washing;(7)Pickling;(8)Washing;(9)Alcohol parses;(10)Concentration;(11)Desalination, decolorization;(12)Cross refined resin;(13)Activated carbon decolorizing.The present invention uses alkali tune, crosses alkali, acid removal of impurities, and alcohol elutes afterwards, and desalination of connecting again after recycling design, decoloration refine resin, and total reducing sugar more than 95%, the raw sugar of more than RA60% are directly obtained after activated carbon decolorizing.
Description
Technical field
The present invention relates to a kind of technique for extracting stevioside, more particularly, to a kind of technique of percolation extraction stevioside.
Background technology
STEVIA REBAUDIANA (Stevia rebaudinan Betroni) belongs to composite family Stevia herbaceos perennial, originates in bar
Draw Amambay the and Mbaxacayu mountain ranges of Gui.STEVIA REBAUDIANA was just once drawn as new sugar source plant in World War II
Played attention.Japan tames since introducing a fine variety Brazil, cultivates, refining sugar within 1970, is carried out at the same time the experiments such as toxicity, food inspection.
China is in 1976 from Japanese successful introduction, and also there are different degrees of Extend culture in South Korea, Thailand, Philippine etc. at present.Sweetleaf
Chrysanthemum happiness temperature, is feverfew, has extensive preferably kind property.
Stevioside is a kind of new type natural green food additive, is had found in the world today closest to sucrose
The natural sweetener of sweet taste, it has sugariness height(For 300 times or more of sucrose), heat it is low(Only the 1/300 of sucrose), safety
The four characteristics such as reliable and medicinal health value height, and it is widely used in the industries such as domestic and international food, medicine and light industry.1984
Among stevioside is included in " national development of food industry outline in 2000 " by Economic and Trade Commission of former country, and as giving priority to and promote item
Mesh.Health ministry official approval stevioside is used as food additives within 1985.Steviol glycoside includes Lay bud enlightening glycosides A
(That is RA), RA refers to Rebaudioside A, that is, A3;RA components are sweet taste components most excellent in stevioside, are passed through
Recrystallization technology is refined from common stevioside and formed, the pure and fresh no bitter taste of mouthfeel, sugariness for 300-400 times of sucrose and taste matter more
Close to sucrose.However the method for extraction of steviosides RA at present, it is stevia rebaudian leaf through extracting, adsorbing, decolourizing, the processes essence such as drying
It makes.Stevioside RA contents are relatively low in stevioside RA products obtained by this method, and obtained stevioside specification is total reducing sugar
85%, Lay bud enlightening glycosides A(RA)50%, it is impossible to meet the requirements.
The content of the invention
The technical problems to be solved by the invention are to overcome the deficiencies of the prior art and provide a kind of percolation extraction stevia rebaudianum
The technique of sugar can obtain total reducing sugar more than 95%, Lay bud enlightening glycosides A without refined(RA)The stevioside of more than 60% specification.
The present invention solve its technical problem the technical solution adopted is that, a kind of technique of percolation extraction stevioside, including
Following steps:
(1)Extraction:By 3 or more(It is preferred that 4-6)Extractor is connected, and each extractor is equipped with charge door, respectively toward every
Stevia rebaudiana starting material is added in a tank, adds the water for being equivalent to 10-12 times of Stevia rebaudiana starting material weight, extraction water temperature control is in 40-
45 DEG C, when extraction 6-12 is small, obtain extracting solution;
During extraction, continuous flow upstream seepage pressure effects of preferably connecting:Water passes sequentially through the extractor of series connection, and water is introduced into first
Extractor, after first extractor is full the extracting solution of i.e. first tank out after overflow into second tank as fresh solvent,
The extracting solution of second tank enters back into the 3rd tank after coming out, and so on, the extracting solution of the last one tank is out just final to be made
For extracting solution;The method extracts more complete, product yield higher;And solvent used is few, more water-saving, sewage quantity reduces 20%;
(2)Alkali tune:By step(1)Gained extracting solution is 10-11 with alkaline solution tune pH;
The preferred NaOH solution of alkaline solution;
The present invention exempt flocculation step, and after alkali tune extracting solution store in alkaline conditions do not allow it is perishable;
(3)Cleaner liquid:It will be through step(2)The extracting solution filtering of processing, obtains filtrate;
(4)Upper prop adsorbs:Using three Splite LX-T28 resin columns series connection absorption, by step(3)Gained filtrate is to flow
Speed≤2BV/hr(Column volume is per hour)3 adsorption resin columns are passed sequentially through, when extracting solution crosses column to the 3rd pillar efflux
Stop first after pleasantly sweet, and increase an adsorption column to after the 3rd, and so on;After the completion of upper prop, by the every of upper prop
Root Splite LX-T28 resin columns cross 1-1.2 times of BV purified waters removal of impurities;
(5)Alkali cleaning:By step(4)Gained resin column crosses the lye of 0.3-0.7wt%, flow velocity 1-1.5BVL/hr, every
Resin column elution amount is 3-4BV, removes impurity;
The preferred NaOH solution of lye;
(6)Washing:It will be through step(5)Every resin column of processing crosses water 2-3BVL, flow control 1.8-2.0BVL/
hr;Lye is removed on top;
(7)Pickling:It will be through step(6)The resin column of processing crosses the acid solution of 0.3-0.7wt%, flow velocity 1-1.5BVL/hr,
Every resin column elution amount is 2-3BV;Neutralize lye;
The preferred HCl solution of acid solution;
(8)Washing:It will be through step(7)Every resin column of processing crosses water 2-3BVL to efflux to be neutral, flow control
For 1.8-2BVL/hr;Acid solution is gone on top;
(9)Alcohol parses:It will be through step(8)The volumetric concentration that every resin column of processing crosses 4 ± 0.2 times of BV is 70-75%
Ethanol solution;After ethanol solution drains, after washing every resin column with 70-80 DEG C of pure water of 5-6 times of column volume, tree is kept
Liquid level is higher than resin column surface 4-5 cm in fat column, stops washing, spare;
(10)Concentration:By step(9)In the ethanol solution that is collected into, concentrated using heating in vacuum, vacuum degree for-
0.070MPa to -0.095MPa, heating and temperature control recycle ethyl alcohol, until no alcohol taste, obtain treating destainer at 50~60 DEG C;
(11)Desalination, decolorization:By step(10)Gained treat destainer successively continuously through Seplite LX-T5 resins,
D941 resins, D285 resin decolorizations, flow velocity are 2 ± 0.1BV/h, collect and start pleasantly sweet omission timber;Again with 3-3.5BV's
60-70 DEG C of purifying three resins of washing are to efflux without sweet taste;Omission timber, water lotion are merged, concentrated using heating in vacuum, very
Reciprocal of duty cycle is -0.070MPa to -0.095MPa, and heating and temperature control is at 60~80 DEG C, when drying 8-12 is small;Baking oven is placed into do
It is dry, 75-85 DEG C of oven temperature is kept, drying time 4-5 h obtains raw sugar;
(12)Cross refined resin:By step(11)Gained raw sugar is configured to aqueous solution, and sugar content is in every 100ml aqueous solutions
15-20g crosses LX-69B to fat column afterwards, and the resin column volume is equivalent to the 1/4~1/3 of raw sugar aqueous solution volume, collects tree
Fat raw sugar efflux;
Remaining feed liquid can be parsed directly with ethyl alcohol on resin, be recycled;
(13)Activated carbon decolorizing:By step(12)Gained resin raw sugar efflux is configured to the water of mass concentration 10-12%
Solution, adds in the decoloration active carbon for being equivalent to raw sugar quality 5%-10%, and 70-80 DEG C of stirring in water bath 30-35min treats that destainer is cold
When but to room temperature, with the membrane filtration of 0.4 micron pore size, filtrate is collected;Filtrate using heating in vacuum concentrate, vacuum degree for-
0.070MPa to -0.095MPa, heating and temperature control is at 60~80 DEG C, when drying 8-12 is small;Oven drying is placed into, keeps drying
75-85 DEG C of box temperature degree, drying time 4-5 h is to get more than total reducing sugar 95wt%, Lay bud enlightening glycosides A(RA)More than 60% raw sugar.
The present invention avoids having an impact the purity of product using high temperature using vacuum drying concentration.
The present invention uses alkali tune, crosses alkali, acid removal of impurities, and alcohol elutes afterwards, connected again after recycling design desalination, decoloration, essence
Resin processed directly obtains total reducing sugar more than 95%, the raw sugar of more than RA60% after activated carbon decolorizing.Compared to traditional handicraft, extracting solution tune
After alkali, the growth of microorganism had both been can inhibit, has extended the feed liquid resting period, while can also have been accomplished without using flocculant, has avoided making
The residue problem caused by flocculant;Impurity is washed away using soda acid by adsorbing resin, improves the content of product, not by refined
Technique, can directly be made total reducing sugar more than 95%, the raw sugar of more than RA60%, this specification is higher by the rule of GB8270-2014 total reducing sugars 85%
Lattice reach JECFA international standards.
Specific embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
The present embodiment comprises the following steps:
(1)Extraction:3 extractors are connected, each extractor is equipped with charge door, adds STEVIA REBAUDIANA into each tank respectively
Raw material, adds the water for being equivalent to 10 times of Stevia rebaudiana starting material weight, and extraction water temperature control when extraction 6 is small, must be extracted at 45 DEG C
Liquid;
(2)Alkali tune:By step(1)Gained extracting solution NaOH solution tune pH is 10.1;
(3)Cleaner liquid:It will be through step(2)The extracting solution filtering of processing, obtains filtrate;
(4)Upper prop adsorbs:Using three Splite LX-T28 resin columns series connection absorption, by step(3)Gained filtrate is to flow
Fast 1BV/hr(Column volume is per hour)3 adsorption resin columns are passed sequentially through, crossing column to the 3rd pillar efflux when extracting solution has
Stop first after sweet taste, and increase an adsorption column to after the 3rd;After the completion of upper prop, by every Splite LX- of upper prop
T28 resin columns cross 1.2 times of BV purified waters removal of impurities;
(5)Alkali cleaning:By step(4)Gained resin column crosses the NaOH solution of 0.7wt%, flow velocity 1.5BVL/hr, every tree
Fat column elution amount is 4BV, removes impurity;
(6)Washing:It will be through step(5)Every resin column of processing crosses water 3BVL, flow control 1.8BVL/hr;Top is gone
Lye;
(7)Pickling:It will be through step(6)The resin column of processing crosses the HCl solution of 0.3wt%, flow velocity 1BVL/hr, every tree
Fat column elution amount is 3BV;Neutralize lye;
(8)Washing:It will be through step(7)It is neutrality that every resin column of processing, which crosses water 3BVL to efflux, and flow control is
1.8BVL/hr;Acid solution is gone on top;
(9)Alcohol parses:It will be through step(8)The ethyl alcohol that the volumetric concentration that every resin column of processing crosses 4 times of BV is 75% is molten
Liquid;After ethanol solution drains, after washing every resin column with 80 DEG C of pure water of 5 times of column volumes, keep liquid level in resin column high
In resin column surface 4-5 cm, stop washing, it is spare;
(10)Concentration:By step(9)In the ethanol solution that is collected into, concentrated using heating in vacuum, vacuum degree for-
0.070MPa, heating and temperature control recycle ethyl alcohol, until no alcohol taste, obtain treating destainer at 60 DEG C;
(11)Desalination, decolorization:By step(10)Gained treat destainer successively continuously through Seplite LX-T5 resins,
D941 resins, D285 resin decolorizations, flow velocity 2BV/h are collected and are started pleasantly sweet omission timber;Again with 70 DEG C of purifying of 3.5BV
Three resins are washed to efflux without sweet taste;By omission timber, water lotion merge, concentrated using heating in vacuum, vacuum degree for-
0.070MPa MPa, heating and temperature control is at 80 DEG C, when drying 8 is small;Oven drying is placed into, keeps 85 DEG C of oven temperature, is done
Dry time 4h, obtains raw sugar;
(12)Cross refined resin:By step(11)Gained raw sugar is configured to aqueous solution, and sugar content is in every 100ml aqueous solutions
20g crosses LX-69B to fat column afterwards, and the resin column volume is equivalent to the 1/4 of raw sugar aqueous solution volume, collects resin raw sugar stream
Go out liquid;
Remaining feed liquid can be parsed directly with ethyl alcohol on resin, be recycled;
(13)Activated carbon decolorizing:By step(12)Gained resin raw sugar efflux is configured to the aqueous solution of mass concentration 12%,
The decoloration active carbon for being equivalent to raw sugar quality 10% is added in, 70 DEG C of stirring in water bath 30min when destainer is cooled to room temperature, are used
The membrane filtration of 0.4 micron pore size collects filtrate;Filtrate is concentrated using heating in vacuum, and vacuum degree is -0.070MPa MPa, is added
Hot temperature control is at 80 DEG C, when drying 8 is small;Oven drying is placed into, keeps 85 DEG C of oven temperature, drying time, 4 h was to get total
Sugared 95.1wt%, Lay bud enlightening glycosides A(RA)60.2% raw sugar.
The test method standard of raw sugar content of the present invention:National Standard Method:《GB 8270-2014 food securities country mark
Quasi- food additives steviol glycoside》;International law:《Stevioside JECFA standards-America and Europe's international standard》.
Embodiment 2
The present embodiment comprises the following steps:
(1)Extraction:6 extractors are connected, each extractor is equipped with charge door, adds STEVIA REBAUDIANA into each tank respectively
Raw material, adds the water for being equivalent to 12 times of Stevia rebaudiana starting material weight, and extraction water temperature control is at 40 DEG C, when each tank extraction 12 is small,
Obtain extracting solution;
During extraction, series connection continuous flow upstream seepage pressure effects are selected:Water passes sequentially through the extractor of series connection, and water is introduced into first
Extractor, after first extractor is full the extracting solution of i.e. first tank out after overflow into second tank as fresh solvent,
The extracting solution of second tank enters back into the 3rd tank after coming out, and so on, the extracting solution of the last one tank is out just final to be made
For extracting solution;The method extracts more complete, product yield higher;And solvent used is few, more water-saving, sewage quantity reduces 20%;
(2)Alkali tune:By step(1)Gained extracting solution NaOH solution tune pH is 11;
(3)Cleaner liquid:It will be through step(2)The extracting solution filtering of processing, obtains filtrate;
(4)Upper prop adsorbs:Using three Splite LX-T28 resin columns series connection absorption, by step(3)Gained filtrate is to flow
Fast 1.5BV/hr(Column volume is per hour)3 adsorption resin columns are passed sequentially through, when extracting solution crosses column to the 3rd pillar efflux
Stop first after pleasantly sweet, and increase an adsorption column to after the 3rd;After the completion of upper prop, by every Splite of upper prop
LX-T28 resin columns cross 1.2 times of BV purified waters removal of impurities;
(5)Alkali cleaning:By step(4)Gained resin column crosses the NaOH solution of 0.7wt%, flow velocity 1.5BVL/hr, every tree
Fat column elution amount is 4BV, removes impurity;
(6)Washing:It will be through step(5)Every resin column of processing crosses water 3BVL, flow control 2.0BVL/hr;Top is gone
Lye;
(7)Pickling:It will be through step(6)The resin column of processing crosses the HCl solution of 0.7wt%, flow velocity 1.5BVL/hr, every
Resin column elution amount is 3BV;Neutralize lye;
(8)Washing:It will be through step(7)It is neutrality that every resin column of processing, which crosses water 3BVL to efflux, and flow control is
2BVL/hr;Acid solution is gone on top;
(9)Alcohol parses:It will be through step(8)The ethyl alcohol that the volumetric concentration that every resin column of processing crosses 4 times of BV is 75% is molten
Liquid;After ethanol solution drains, after washing every resin column with 80 DEG C of pure water of 6 times of column volumes, keep liquid level in resin column high
In resin column surface 4-5cm, stop washing, it is spare;
(10)Concentration:By step(9)In the ethanol solution that is collected into, concentrated using heating in vacuum, vacuum degree for-
0.095MPa, heating and temperature control recycle ethyl alcohol, until no alcohol taste, obtain treating destainer at 60 DEG C;
(11)Desalination, decolorization:By step(10)Gained treat destainer successively continuously through Seplite LX-T5 resins,
D941 resins, D285 resin decolorizations, flow velocity 2BV/h are collected and are started pleasantly sweet omission timber;Again with 70 DEG C of purifying of 3.5BV
Three resins are washed to efflux without sweet taste;By omission timber, water lotion merge, concentrated using heating in vacuum, vacuum degree for-
0.095MPa, heating and temperature control is at 60 DEG C, when drying 12 is small;Oven drying is placed into, 85 DEG C of oven temperature is kept, when dry
Between 4h, obtain raw sugar;
(12)Cross refined resin:By step(11)Gained raw sugar is configured to aqueous solution, and sugar content is in every 100ml aqueous solutions
20g crosses LX-69B to fat column afterwards, and the resin column volume is equivalent to the 1/3 of raw sugar aqueous solution volume, collects resin raw sugar stream
Go out liquid;
Remaining feed liquid can be parsed directly with ethyl alcohol on resin, be recycled;
(13)Activated carbon decolorizing:By step(12)Gained resin raw sugar efflux is configured to the aqueous solution of mass concentration 10%,
The decoloration active carbon for being equivalent to raw sugar quality 10% is added in, 70 DEG C of stirring in water bath 30min when destainer is cooled to room temperature, are used
The membrane filtration of 0.4 micron pore size collects filtrate;Filtrate is concentrated using heating in vacuum, and vacuum degree is -0.095MPa, and heating is warm
Degree control is at 60 DEG C, when drying 8 is small;Oven drying is placed into, keeps 85 DEG C of oven temperature, drying time, 5 h was to get total reducing sugar
95.2wt%, Lay bud enlightening glycosides A(RA)60.1% raw sugar.
Claims (6)
1. a kind of technique of percolation extraction stevioside, which is characterized in that comprise the following steps:
(1)Extraction:3 or more extractors are connected, each extractor is equipped with charge door, adds STEVIA REBAUDIANA into each tank respectively
Raw material adds the water for being equivalent to 10-12 times of Stevia rebaudiana starting material weight, and at 40-45 DEG C, extraction 6-12 is small for extraction water temperature control
When, obtain extracting solution;
(2)Alkali tune:By step(1)Gained extracting solution is 10-11 with alkaline solution tune pH;
(3)Cleaner liquid:It will be through step(2)The extracting solution filtering of processing, obtains filtrate;
(4)Upper prop adsorbs:Using three Splite LX-T28 resin columns series connection absorption, by step(3)Gained filtrate with flow velocity≤
2BV/h passes sequentially through 3 adsorption resin columns, when extracting solution cross column to the 3rd pillar efflux it is pleasantly sweet after stopped first,
Increase an adsorption column again to after the 3rd, and so on;After the completion of upper prop, by every Splite LX-T28 resin of upper prop
Column crosses 1-1.2 times of BV purified waters removal of impurities;
(5)Alkali cleaning:By step(4)Gained resin column crosses the lye of 0.3-0.7wt%, flow velocity 1-1.5BV/h, every resin column
Elution amount is 3-4BV, removes impurity;
(6)Washing:It will be through step(5)Every resin column of processing crosses water 2-3BV, flow control 1.8-2.0BV/h;Push up lixiviating
Liquid;
(7)Pickling:It will be through step(6)The resin column of processing crosses the acid solution of 0.3-0.7wt%, flow velocity 1-1.5BV/h, every tree
Fat column elution amount is 2-3BV;Neutralize lye;
(8)Washing:It will be through step(7)Every resin column of processing crosses water 2-3BV to efflux to be neutral, flow control 1.8-
2BV/h;Acid solution is gone on top;
(9)Alcohol parses:It will be through step(8)The second that the volumetric concentration that every resin column of processing crosses 4 ± 0.2 times of BV is 70-75%
Alcoholic solution;After ethanol solution drains, after washing every resin column with 70-80 DEG C of pure water of 5-6 times of column volume, resin column is kept
Interior liquid level is higher than resin column surface 4-5 cm, stops washing, spare;
(10)Concentration:By step(9)In the ethanol solution that is collected into, concentrated using heating in vacuum, vacuum degree is -0.070MPa
To -0.095MPa, heating and temperature control recycles ethyl alcohol, until no alcohol taste, obtains treating destainer at 50~60 DEG C;
(11)Desalination, decolorization:By step(10)Gained treats destainer successively continuously through Seplite LX-T5 resins, D941
Resin, D285 resin decolorizations, flow velocity are 2 ± 0.1BV/h, collect and start pleasantly sweet omission timber;The 60-70 of 3-3.5BV is used again
DEG C purifying washing three resins to efflux without sweet taste;Omission timber, water lotion are merged, concentrated using heating in vacuum, vacuum degree
For -0.070MPa to -0.095MPa, heating and temperature control is at 60~80 DEG C, when drying 8-12 is small;Oven drying is placed into, is protected
75-85 DEG C of oven temperature is held, drying time 4-5 h obtains raw sugar;
(12)Cross refined resin:By step(11)Gained raw sugar is configured to aqueous solution, and sugar content is 15- in every 100mL aqueous solutions
20g crosses LX-69B resin columns afterwards, and the resin column volume is equivalent to the 1/4~1/3 of raw sugar aqueous solution volume, collects resin
Raw sugar efflux;
(13)Activated carbon decolorizing:By step(12)Gained resin raw sugar efflux is configured to the aqueous solution of mass concentration 10-12%,
The decoloration active carbon for being equivalent to raw sugar quality 5%-10% is added in, 70-80 DEG C of stirring in water bath 30-35min treats that destainer is cooled to
During room temperature, with the membrane filtration of 0.4 micron pore size, filtrate is collected;Filtrate using heating in vacuum concentrate, vacuum degree for-
0.070MPa to -0.095MPa, heating and temperature control is at 60~80 DEG C, when drying 8-12 is small;Oven drying is placed into, keeps drying
75-85 DEG C of box temperature degree, drying time 4-5 h to get.
2. the technique of percolation extraction stevioside according to claim 1, which is characterized in that step(1)In, series connection carries
Tank is taken as 4-6.
3. the technique of percolation extraction stevioside according to claim 1 or 2, which is characterized in that step(1)In, extraction
When, select series connection continuous flow upstream seepage pressure effects:Water passes sequentially through the extractor of series connection, and water is introduced into first extractor, and first
After a extractor is full i.e. the extracting solution of first tank out after overflow into second tank as fresh solvent, second tank carries
Liquid is taken to enter back into the 3rd tank after coming out, and so on, the extracting solution of the last one tank is out just eventually as extracting solution.
4. the technique of percolation extraction stevioside according to claim 1 or 2, which is characterized in that step(2)In, it is described
Alkaline solution is NaOH solution.
5. the technique of percolation extraction stevioside according to claim 1 or 2, which is characterized in that step(5)In, it is described
Alkaline solution is NaOH solution.
6. the technique of percolation extraction stevioside according to claim 1 or 2, which is characterized in that step(7)In, it is described
Acid solution is HCl solution.
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CN107474086A (en) * | 2016-06-07 | 2017-12-15 | 上海达盛食品有限公司 | The technique for extracting stevioside |
CN107118243B (en) * | 2017-06-05 | 2020-06-19 | 江苏史蒂文生物科技有限公司 | Industrial preparation method of stevioside |
CN107325137B (en) * | 2017-08-21 | 2020-08-04 | 内蒙古昶辉生物科技股份有限公司 | Extraction method of stevioside |
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 |
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 |
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WO2021216553A1 (en) * | 2020-04-20 | 2021-10-28 | Cargill, Incorporated | Increasing yield of steviol glycosides |
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