CN105061527A - Process for refined production of stevioside - Google Patents
Process for refined production of stevioside Download PDFInfo
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- CN105061527A CN105061527A CN201510541394.6A CN201510541394A CN105061527A CN 105061527 A CN105061527 A CN 105061527A CN 201510541394 A CN201510541394 A CN 201510541394A CN 105061527 A CN105061527 A CN 105061527A
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Abstract
A process for refined production of stevioside comprises the following steps: (1) mixing stevioside raw sugar and edible ethanol solution and performing stirring backflow until the stevioside raw sugar is fully dissolved; (2) performing immediate filtration of the obtained solution and crystallizing filtrate obtained after the filtration; performing refiltration after the crystallization and obtaining crystal I and filtrate I; (3) after the obtained crystal I is dried, mixing the obtained crystal I and the edible ethanol solution, and performing stirring backflow until the crystal I is fully dissolved; (4) performing immediate filtration of the obtained solution and crystallizing the filtrate obtained after the filtration; performing refiltration after the crystallization and obtaining crystal II and filtrate II; (5) performing concentration and drying of the obtained filtrate II; (6) drying the crystal II obtained through the step (4), and obtaining the product. By utilizing the fact that components of stevioside are different in solubility in the edible ethanol solution, rebaudioside A is separated and extracted, stevioside with the purity of rebaudioside A over 97% is obtained, and the use of solvents class 2 such as methanol and isopropanol is avoided.
Description
Technical field
The present invention relates to a kind of stevioside refined raw production art.
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.Sweet Stevia happiness temperature is feverfew, and having widely should kind property.China is in 1976 from Japanese successful introduction.Also there are Extend culture in various degree in current Korea S, Thailand, Philippines etc.Cultivate the plant husbandry of sweetleaf Chrysanthemum, produce Steviosides and then belong to processing of agriculture product, this is the industry that country advocates energetically and develops.
Steviol glycoside is a kind of new type natural green food additive, 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.RA refers to Lay bud enlightening glycosides A(RebaudiosideA), namely A3, RA component is sweet taste component the most excellent in stevioside, and generally form by recrystallization technology is refining from common stevioside, mouthfeel is pure and fresh in bitter taste.
The sugariness of steviol glycoside is 300 times of sucrose, but it is with certain bad pleasant impression.Steviol glycoside comprises Lay bud enlightening glycosides A and Lay bud enlightening glycosides C; The sugariness of Lay bud enlightening glycosides C less than 50 times of sucrose, and has stronger rear bitter taste and bad pleasant impression; The sugariness of Lay bud enlightening glycosides A is 250-450 times of sucrose, and outward appearance is white powder or crystal, soluble in water, is the best substitute of sucrose.General steviol glycoside purity is 80%-95%, and wherein Lay bud enlightening glycosides A purity is 20%-90%, and therefore general steviol glycoside is with certain peculiar smell, is difficult to directly directly use as independent composition.But the high purity Lay bud enlightening glycosides A that purity reaches more than 95% directly as foodstuff additive use, can be able to apply in the sugared fields of nearly all use such as the huge beverage of sugared demand, wine brewing, food, medicine.Therefore, how to improve the purity of Lay bud enlightening glycosides A product, develop the Technology of low-cost industrial production high purity Lay bud enlightening glycosides A product, the focus of Shi Ge Steviosides manufacturing enterprise and related researcher's concern always.Have common structural motif stevia rebaudianum alcohol radical between different steviol glucoside, structure is very similar each other, is separated more difficult.Through effort for many years and practice, people have have researched and developed the Technology of various production high purity Lay bud enlightening glycosides A product, but have all used two kind solvents such as methyl alcohol in current treating process, and in remaining processing sequences, the general methods such as baking that adopt remove.Methyl alcohol etc. two kind solvent lowest limit requirement in the standard of European Union's product is 10ppm, depends baking alone and is difficult to reach this requirement, even if pulverize the situation that rebake also has solvent to exceed standard often again after baking.
In the market, RA content is the price of the stevioside of 95wt% and 97wt% is 620 yuan/kilogram and 720 yuan/kilogram respectively, and the main flow specification of market circulation is now 97%.In prior art, obtain the stevioside that RA content is 97wt%, generally need to use two kind solvent such as methyl alcohol, Virahol, there is the problem of product dissolvent residual on the one hand, that the problems such as employee's operational safety highlight on the other hand, enterprise certainly will need to drop into and improves security measures more, also just will certainly increase cost.But in prior art, if only carry out refined stevioside with ethanol as solvent, generally can only obtain the product that purity is 95%, be difficult to be refined to 97%.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, provides a kind of to use edible ethanol, operates safer stevioside refined raw production art, refined by stevioside, obtains Lay bud enlightening glycosides A(RA) mass percentage is the product of 97%.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of stevioside refined raw production art, comprises the following steps:
(1) be that the edible ethanol solution of 84%-87% mixes by mass volume ratio 1g: 3-3.5ml by the stevioside raw sugar of total reducing sugar mass content > 85% and volumetric concentration, be heated to 70-80 DEG C, stirring and refluxing is dissolved completely to stevioside raw sugar;
If described volumes of aqueous ethanol concentration is lower than 84%, be then difficult to crystallization in subsequent process, if volumes of aqueous ethanol concentration is higher than 87%, then the RA content of products obtained therefrom does not reach requirement;
(2) by step (1) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, add the crystal seed being equivalent to stevioside sugar materials weight more than 1/1000 during crystallization and (can crystallization velocity be accelerated, improve yield) simultaneously, the Tc of filtrate be 0-5 DEG C (if carry out crystallization at normal temperatures, then almost do not have crystallization to produce, crystallization temperature controls very important), crystallization time 8h-12h; Refilter after crystallization, obtain crystallization I (stevioside raw sugar I) and filtrate I;
(3) after step (2) gained crystallization I being dried, the edible ethanol being 84%-87% by gained crystallization I and volumetric concentration (is difficult to crystallization lower than this scope, RA content higher than this scope products obtained therefrom does not reach) solution according to mass volume ratio be 1g: 4-4.5ml ratio mixing, be heated to 70-80 DEG C, stirring and refluxing to crystallization I is dissolved completely;
(4) by step (3) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, and the Tc of filtrate is 0-5 DEG C, crystallization time 8h-12h; Refilter after crystallization, obtain crystallization II (stevioside raw sugar II) and filtrate II;
(5) by step (4) gained filtrate II (mother liquor) concentrate drying, mother liquor sugar II is obtained; It is refining that mother liquid obtained sugared II (its RA content is higher) can replace the stevioside raw sugar of total sugar content > 85% to continue in step (1), also dry again after mother liquor sugar II can being pulverized, bake out temperature is 70-80 DEG C, and the time is 45-60min, uses after oven dry as raw sugar;
(6) step (4) gained crystallization II dried, bake out temperature is 70-80 DEG C, and the time is 45-60min, obtains the stevioside of Lay bud enlightening glycosides A mass content >=97%.
Further, step (2) can be filtered gained filtrate I (mother liquor) concentrate drying, obtain mother liquor sugar I; Mother liquor sugar I is dried after pulverizing again, and bake out temperature is 70-80 DEG C, and the time is 45-60min; Mother liquid obtained sugared I is separately used as him.
The present invention's edible ethanol solution refining stevioside raw sugar twice, utilizes the different solubility of each component of stevioside in edible ethanol solution, and separating-purifying Lay bud enlightening glycosides A(is called for short RA), obtain the stevioside of Lay bud enlightening glycosides A purity more than 97%.Avoid using two kind solvent such as methyl alcohol, Virahol simultaneously.This technological operation safely, simply, does not have traditional technology strict to the requirement of environment, and employee's security when plant operations improves, and avoids using methyl alcohol to cause larger infringement to employee's health.
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) (the RA content of raw material stevioside raw sugar is 55.4wt% to take 400kg stevioside raw sugar, total sugar content is 87.6wt%), add the edible ethanol solution that 1300L volumetric concentration is 84.1%, be heated to 70-80 DEG C, stirring and refluxing to stevioside raw sugar dissolves completely;
(2) by step (1) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, adds the crystal seed (0.4kg) being equivalent to sugar materials weight 1/1000 during crystallization, filtrate is cooled to 5 DEG C with refrigerated water, stirred crystallization 8h; Centrifuging again after crystallization, obtains 283Kg crystallization I (stevioside raw sugar I) and filtrate I (mother liquor);
(3), after step (2) gained crystallization I being dried, obtain 226Kg crystallization I, take 200kg crystallization I, add the edible ethanol solution that 900L volumetric concentration is 86.3%, be heated to 70-80 DEG C, stirring and refluxing to crystallization I is dissolved completely;
(4) by step (3) gained solution filtered while hot, after filtering, gained filtrate carries out crystallization, and the Tc of filtrate is 5 DEG C, crystallization time 12h; Refilter after crystallization, obtain crystallization II (stevioside raw sugar II) and filtrate II;
(5) by step (4) gained filtrate II (mother liquor) concentrate drying, obtain mother liquor sugar II, mother liquid obtained sugared II (its RA content is higher) returns and replaces the stevioside raw sugar of total sugar content > 85% to continue to refine in step (1);
(6) step (4) gained crystallization II dried, bake out temperature is 80 DEG C, and the time is 45min; Obtain the stevioside 134Kg that Lay bud enlightening glycosides A mass content is 97.6%.
Single operation yield calculates: yield=(134 × 97.6%)/(400 × 55.4%) * 100%=59.0%, suitable with the yield of use two kind solvent process.
In the present embodiment, step (2) is filtered gained filtrate I (mother liquor) concentrate drying, obtains mother liquor sugar I, mother liquor sugar is dried after pulverizing again, and bake out temperature is 80 DEG C, and the time is 45min; Mother liquid obtained sugared I is separately used as him.
In the present invention, in described raw material or product, RA detection method of content standard is GB GB8270-2014 or international standard jecfa.
Embodiment 2
The present embodiment comprises the following steps:
(1) (the RA content of raw material stevioside raw sugar is 55.6wt% to take 400kg stevioside raw sugar, total sugar content is 87.4wt%), add the edible ethanol solution that 1200L volumetric concentration is 86.7%, be heated to 70-80 DEG C, stirring and refluxing to stevioside raw sugar dissolves completely;
(2) by step (1) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, adds crystal seed 0.5kg during crystallization, filtrate is cooled to 0 DEG C with refrigerated water, stirred crystallization 10h; Centrifuging again after crystallization, obtains 304Kg crystallization I (stevioside raw sugar I) and filtrate I (mother liquor);
(3), after step (2) gained crystallization I being dried, obtain 217Kg crystallization I, take 200kg crystallization I, add the edible ethanol solution that 800L volumetric concentration is 86.9%, be heated to 70-80 DEG C, stirring and refluxing to crystallization I is dissolved completely;
(4) by step (3) gained solution filtered while hot, after filtering, gained filtrate carries out crystallization, and the Tc of filtrate is 0 DEG C, crystallization time 8h; Refilter after crystallization, obtain crystallization II (stevioside raw sugar II) and filtrate II;
(5) by step (4) gained filtrate II (mother liquor) concentrate drying, obtain mother liquor sugar II, mother liquid obtained sugared II (its RA content is higher) returns and replaces the stevioside raw sugar of total sugar content > 85% to continue to refine in step (1);
(6) step (4) gained crystallization II dried, bake out temperature is 70 DEG C, and the time is 60min; Obtain the stevioside 115Kg of Lay bud enlightening glycosides A mass content 97.4%.
In the present embodiment, step (2) is filtered gained filtrate I (mother liquor) concentrate drying, obtains mother liquor sugar I, mother liquor sugar is dried after pulverizing again, and bake out temperature is 70 DEG C, and the time is 60min; Mother liquid obtained sugared I is separately used as him.
Reference examples 1
Take 200kg stevioside raw sugar (the RA content of raw material stevioside raw sugar is 55.4wt%, and total sugar content is 87.6wt%), add the edible ethanol solution that 600L volumetric concentration is 85.1%, be heated to 70-80 DEG C, stirring and refluxing makes it to dissolve completely; Filtered while hot, when filtrate is cooled to 5 DEG C with refrigerated water, does not add crystal seed, stirred crystallization 12h; Can't see crystallization or crystallization content is little.Description of step does not add crystal seed in (2), and crystallization effect is bad.
Reference examples 2
Take 200kg stevioside raw sugar (the RA content of raw material stevioside raw sugar is 55.4wt%, and total sugar content is 87.6wt%), add the ethanolic soln that 700L volumetric concentration is 80%, be heated to 70-80 DEG C, stirring and refluxing makes it to dissolve completely.Filtered while hot, when filtrate is cooled to 5 DEG C with refrigerated water, adds the crystal seed of 1/1000 weight being equivalent to stevioside sugar materials weight, and it is 5 DEG C that Tc controls, stirred crystallization 12h.Result can't see crystallization or crystallization content is little.Illustrate that use ethanol solution concentration is too low, can not get crystallization.
Reference examples 3
(1) take 400kg stevioside raw sugar (the RA content of raw material stevioside raw sugar is 55.4wt%, and total sugar content is 87.6wt%), add the ethanolic soln that 1200L volumetric concentration is 90%, be heated to 70-80 DEG C, stirring and refluxing makes it to dissolve completely;
(2) by step (1) gained solution filtered while hot, when filtrate is cooled to 5 DEG C with refrigerated water, add the crystal seed of 1/1000 weight being equivalent to raw material raw sugar weight, it is 0 DEG C that Tc controls, stirred crystallization 12h; Centrifuging afterwards, obtains crystallization I and filtrate I (mother liquor) after centrifugal;
(3), after step (2) gained crystallization I being dried, take 200kg crystallization I, add the edible ethanol solution that 900L volumetric concentration is 86.3%, be heated to 70-80 DEG C, stirring and refluxing to crystallization I is dissolved completely;
(4) by step (3) gained solution filtered while hot, after filtering, gained filtrate carries out crystallization, and the Tc of filtrate is 5 DEG C, crystallization time 12h; Refilter after crystallization, obtain crystallization II (stevioside raw sugar II) and filtrate II;
(5) by step (4) gained filtrate II (mother liquor) concentrate drying, obtain mother liquor sugar II, mother liquid obtained sugared II (its RA content is higher) returns and replaces the stevioside raw sugar of total sugar content > 85% to continue to refine in step (1);
(6) step (4) gained crystallization II dried, bake out temperature is 80 DEG C, and the time is 45min; Obtain the stevioside 101Kg that Lay bud enlightening glycosides A mass content is 93%.
Visible, the excessive concentration of ethanolic soln, gained Lay bud enlightening glycosides A mass content is all below 95%, and products obtained therefrom does not reach U.S. FCC standard.
Claims (5)
1. a stevioside refined raw production art, is characterized in that, comprises the following steps:
(1) be that the edible ethanol solution of 84%-87% mixes by mass volume ratio 1g: 3-3.5ml by the stevioside raw sugar of total reducing sugar mass content > 85% and volumetric concentration, be heated to 70-80 DEG C, stirring and refluxing is dissolved completely to stevioside raw sugar;
(2) by step (1) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, and add the crystal seed being equivalent to stevioside sugar materials weight more than 1/1000 during crystallization, the Tc of filtrate is 0-5 DEG C, crystallization time 8h-12h; Refilter after crystallization, obtain crystallization I and filtrate I;
(3), after step (2) gained crystallization I being dried, be that the edible ethanol solution of 84%-87% mixes according to the ratio that mass volume ratio is 1g: 4-4.5ml by gained crystallization I and volumetric concentration, be heated to 70-80 DEG C, stirring and refluxing to crystallization I is dissolved completely;
(4) by step (3) gained solution filtered while hot, gained filtrate after filtration is carried out crystallization, and the Tc of filtrate is 0-5 DEG C, crystallization time 8h-12h; Refilter after crystallization, obtain crystallization II and filtrate II;
(5) by step (4) gained filtrate II concentrate drying, mother liquor sugar II is obtained;
(6) step (4) gained crystallization II dried, bake out temperature is 70-80 DEG C, and the time is 45-60min, obtains the stevioside of Lay bud enlightening glycosides A mass content >=97%.
2. stevioside refined raw production art according to claim 1, is characterized in that, in step (5), mother liquid obtained sugared II replaces the stevioside raw sugar of total sugar content > 85% to continue to refine in step (1).
3. stevioside refined raw production art according to claim 1, is characterized in that, in step (5), dry after being pulverized by mother liquor sugar II, bake out temperature is 70-80 DEG C, and the time is 45-60min again, uses after oven dry as raw sugar product.
4. stevioside refined raw production art according to claim 1 and 2, is characterized in that, step (2) is filtered gained filtrate I concentrate drying, obtains mother liquor sugar I; Mother liquor sugar I is dried after pulverizing again, and bake out temperature is 70-80 DEG C, and the time is 45-60min.
5. stevioside refined raw production art according to claim 3, is characterized in that, step (2) is filtered gained filtrate I concentrate drying, obtains mother liquor sugar I; Mother liquor sugar I is dried after pulverizing again, and bake out temperature is 70-80 DEG C, and the time is 45-60min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109645432A (en) * | 2019-02-20 | 2019-04-19 | 史迪威生物科技（苏州）有限公司 | A kind of crystallisation preparation stevia rebaudianum sugar-type dining table sugar method |
| CN111662344A (en) * | 2020-06-29 | 2020-09-15 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
| CN113201034A (en) * | 2021-04-25 | 2021-08-03 | 四川大学 | Obtaining high-purity stevioside from primary crystallization mother liquor of stevioside through secondary crystallization and enriching rebaudioside C |
| CN113527378A (en) * | 2021-08-27 | 2021-10-22 | 江南大学 | Method for recovering stevioside from industrial stevioside mother liquor sugar through crystallization |
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| CN109645432A (en) * | 2019-02-20 | 2019-04-19 | 史迪威生物科技（苏州）有限公司 | A kind of crystallisation preparation stevia rebaudianum sugar-type dining table sugar method |
| CN111662344A (en) * | 2020-06-29 | 2020-09-15 | 四川大学 | Method for recovering rebaudioside A from primary crystallization mother liquor of stevioside |
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| CN113201034A (en) * | 2021-04-25 | 2021-08-03 | 四川大学 | Obtaining high-purity stevioside from primary crystallization mother liquor of stevioside through secondary crystallization and enriching rebaudioside C |
| CN113527378A (en) * | 2021-08-27 | 2021-10-22 | 江南大学 | Method for recovering stevioside from industrial stevioside mother liquor sugar through crystallization |
| CN113527378B (en) * | 2021-08-27 | 2023-11-28 | 江南大学 | Method for recovering stevioside from industrial stevioside mother liquor sugar through crystallization |
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