CN101830947A - Method for making high-content rebaudioside-A stevioside - Google Patents

Method for making high-content rebaudioside-A stevioside Download PDF

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Publication number
CN101830947A
CN101830947A CN201010162911A CN201010162911A CN101830947A CN 101830947 A CN101830947 A CN 101830947A CN 201010162911 A CN201010162911 A CN 201010162911A CN 201010162911 A CN201010162911 A CN 201010162911A CN 101830947 A CN101830947 A CN 101830947A
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powder
steviosides
stevioside
content
rebaudioside
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CN201010162911A
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宋英海
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Individual
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Abstract

The invention discloses a method for making high-content rebaudioside-A stevioside, which comprises the steps of: firstly, injecting methyl alcohol into a material crystallizing tank, stirring and putting stevioside powder, reducing the temperature and crystallizing after fully dissolving the stevioside powder, filtering out crystals, spraying filtrate to be dried into powder after carrying out absorption, analysis, distillation and concentration; stirring and putting the powdered stevioside powder subjected to spraying dry into an alcohol solvent tank, reducing the temperature and crystallizing after the stevioside powder is fully dissolved, and filtering crystals; and mixing the crystals with soft water, entering a concentrating tower for concentration after stirred uniformly, when the concentration of a mixed solution reaches up to 46 percent, adding active carbon for decoloring, finely filtering once, then spraying to be dried into powder to obtain the stevioside with rebaudioside-A content of 90-98 percent. The invention has the advantage that butter and astringent ST aloin and partial RC aloin can be effectively separated out; the rebaudioside-A content of the produced stevioside is high, the product purity is high, the mouthfeel is pure and the processing time is saved.

Description

Produce the method for high-content rebaudioside-A stevioside
Technical field
The present invention relates to a kind of separation method of liquid mixture, specifically a kind of method of producing high-content rebaudioside-A stevioside.
Background technology
Stevioside is as natural sweeteners, its sugariness is 200~400 times of sucrose, heat only is 1/300 of a sucrose, pure taste, edible safety, is well received in industries such as food, beverage, medicine, cosmetics in many countries use, being described as " natural asccharin ", the world " trisaccharide source ", is the best substitute of sucrose and other synthetic sweeteners.About the production method of Steviosides comparative maturity, the product content rebaudioside-A of just producing (being called for short RA) content and extraction yield be difference to some extent, and the difference of content rebaudioside-A content and extraction yield not only causes as same application target the time effect obviously different, and had a strong impact on economic benefit of enterprises.Therefore, a lot of scholars and research unit all are being devoted to study the method that improves product content rebaudioside-A content.For example, disclose a kind of content rebaudioside-A extracting method in Chinese patent ZL98114220.6, this method is to use Steviosides to be dissolved in methyl alcohol at normal temperatures, the ratio in 1: 2~2.5, under atmospheric pressure state, carry out primary crystallization after, filter crystal; Filtrate is carried out secondary crystal more at normal temperatures and pressures with resins exchange, after isolating methyl alcohol, and filtering gained filtrate is desired product.Because this technology only uses a kind of solvent of methyl alcohol to carry out periodic crystallisation, and solvent strength and solvent temperature are not rationally controlled, cause the product content rebaudioside-A content of producing according to this kind method to be limited to for 85~91% (belonging to RA80 substantially), further improve product content rebaudioside-A content and the content rebaudioside-A extraction yield can't be realized.The product of this content rebaudioside-A content can not satisfy the demand of client to high end content rebaudioside-A content product when using as foodstuff additive.
Summary of the invention
Technical assignment of the present invention provides a kind of method of producing high-content rebaudioside-A stevioside.
Technical assignment of the present invention is realized in the following manner, the step of this method is as follows: elder generation's implantation quality percentage concentration in the substance crystallization jar is 90~99% methyl alcohol, be warming up to 50~60 ℃, under this temperature, drop into content rebaudioside-A content while stirring and be 50~55% Steviosides powder, after the Steviosides powder is molten entirely, constant temperature kept 0.5~1 hour, reduce to normal temperature then, after the crystallization 12~16 hours, filter out crystal, filtrate through absorption, resolve, distillation, concentrate the back and spray the dried powder that becomes; The dried Steviosides powder that becomes powder of spray put into while stirring be warming up to 50~55 ℃, mass percent concentration is in 97~99% the alcohol solvent jar, the Steviosides powder complete molten after, crystallization was filtered crystal after 16~24 hours; The gained crystal is mixed with soft water, after stirring, advance upgrading tower and concentrate, when mixed liquid concentration reaches 46% when above, the adding activated carbon decolorizing, fine filtering once sprays the dried powder that becomes then again, can get content rebaudioside-A content at 90~98% Steviosides.
Described methyl alcohol and Steviosides mass ratio are: methyl alcohol: Steviosides=2.5~3: 1.
Described ethanol and Steviosides mass ratio are: ethanol: Steviosides=2~2.5: 1.
Described crystal and soft water quality ratio are: crystal: soft water=1: 1.5~2.
The invention has the beneficial effects as follows: owing to made full use of the characteristics of each component of Steviosides different solubility in methyl alcohol, thereby ST glucoside and part RC glucoside have effectively been isolated with bitter taste, simultaneously again because concentration of ethanol and solvent temperature have been carried out reasonable control, cause the Steviosides content rebaudioside-A content of producing 90~98%, content rebaudioside-A extraction yield height, the product purity height, mouthfeel is pure, fundamental sum sucrose is suitable, and has saved process period.
Embodiment
Embodiment 1:
Choosing content rebaudioside-A content and be 50% Steviosides powder double centner and 250 kilogram-mass percentage concentrations and be 90% methyl alcohol mixes in the substance crystallization jar, after dissolving finishes when being warming up to 50 ℃, constant temperature kept 0.5 hour, reduce to normal temperature then, crystallization is after 12 hours under whipped state, filter out crystal, filtrate through absorption, resolve, distillation, concentrate the back and spray the dried powder that becomes; With dried 82.65 kilograms of Steviosides powder that become powder of spray and 165.3 kilogram-mass percentage concentrations is that 97% ethanol mixes, and is being warming up to after 50 ℃ of dissolvings finish, and crystallization is 16 hours under whipped state, filter 45.8 kg of crystalline; The gained crystal is mixed with 68.4 kilograms of soft water, after stirring, advancing upgrading tower concentrates, when mixed liquid concentration reaches 46%, add activated carbon decolorizing, fine filtering once sprays the dried powder that becomes then again, can get content rebaudioside-A content 44.72 kilograms of 95.58% Steviosidess, the content rebaudioside-A extraction yield is 89.44%.
Embodiment 2:
Choosing content rebaudioside-A content and be 54% Steviosides powder double centner and 280 kilogram-mass percentage concentrations and be 95% methyl alcohol mixes in the substance crystallization jar, after dissolving finishes when being warming up to 55 ℃, constant temperature kept 0.8 hour, reduce to normal temperature then, crystallization is after 14 hours under whipped state, filter out crystal, filtrate through absorption, resolve, distillation, concentrate the back and spray the dried powder that becomes; With dried 87.28 kilograms of Steviosides powder that become powder of spray and 192 kilogram-mass percentage concentrations is that 98% ethanol mixes, and is being warming up to after 53 ℃ of dissolvings finish, and crystallization is 20 hours under whipped state, filter 49.8 kg of crystalline; The gained crystal is mixed with 89.64 kilograms of soft water, after stirring, advancing upgrading tower concentrates, when mixed liquid concentration reaches 47%, add activated carbon decolorizing, fine filtering once sprays the dried powder that becomes then again, can get content rebaudioside-A content 48.95 kilograms of 96.27% Steviosidess, the content rebaudioside-A extraction yield is 90.65%.
Embodiment 3:
Choosing content rebaudioside-A content and be 55% Steviosides powder double centner and 300 kilogram-mass percentage concentrations and be 99% methyl alcohol mixes in the substance crystallization jar, after dissolving finishes when being warming up to 60 ℃, constant temperature kept 1 hour, reduce to normal temperature then, crystallization is after 16 hours under whipped state, filter out crystal, filtrate through absorption, resolve, distillation, concentrate the back and spray the dried powder that becomes; With dried 90.32 kilograms of Steviosides powder that become powder of spray and 225.8 kilogram-mass percentage concentrations is that 99% ethanol mixes, and finishes being warming up to 55 ℃ of dissolvings, and crystallization is 24 hours under whipped state, filter 51.25 kg of crystalline; The gained crystal is mixed with 102.5 kilograms of soft water, after stirring, advancing upgrading tower concentrates, when mixed liquid concentration reaches 46.5%, add activated carbon decolorizing, fine filtering once sprays the dried powder that becomes then again, can get content rebaudioside-A content 50.84 kilograms of 98.45% Steviosidess, the content rebaudioside-A extraction yield is 92.44%.
Among the present invention, the adjusting of the concentration of the Steviosides aqueous solution can Steviosides solid content obtains in the aqueous solution by measuring, and the drying of Steviosides can be passed through variety of way, wherein does to obtain white powder by the vacuum spray, or the lenticular Steviosides.
Employed Steviosides powder stock was commercially available common product before the present invention purified.
Content rebaudioside-A content can detect by high performance liquid phase and obtain among the present invention.

Claims (4)

1. produce the method for high-content rebaudioside-A stevioside, the step that it is characterized in that this method is as follows: elder generation's implantation quality percentage concentration in the substance crystallization jar is 90~99% methyl alcohol, be warming up to 50~60 ℃, under this temperature, drop into content rebaudioside-A content while stirring and be 50~55% Steviosides powder, after the Steviosides powder is molten entirely, constant temperature kept 0.5~1 hour, reduce to normal temperature then, after the crystallization 12~16 hours, filter out crystal, filtrate through absorption, resolve, distillation, concentrate the back and spray the dried powder that becomes; The dried Steviosides powder that becomes powder of spray put into while stirring be warming up to 50~55 ℃, mass percent concentration is in 97~99% the alcohol solvent jar, the Steviosides powder complete molten after, crystallization was filtered crystal after 16~24 hours; The gained crystal is mixed with soft water, after stirring, advance upgrading tower and concentrate, when mixed liquid concentration reaches 46% when above, the adding activated carbon decolorizing, fine filtering once sprays the dried powder that becomes then again, can get content rebaudioside-A content at 90~98% Steviosides.
2. the method for producing high-content rebaudioside-A stevioside according to claim 1 is characterized in that described methyl alcohol and Steviosides mass ratio are: methyl alcohol: Steviosides=2.5~3: 1.
3. the method for producing high-content rebaudioside-A stevioside according to claim 1 is characterized in that described ethanol and Steviosides mass ratio are: ethanol: Steviosides=2~2.5: 1.
4. the method for producing high-content rebaudioside-A stevioside according to claim 1 is characterized in that described crystal and soft water quality ratio is: crystal: soft water=1: 1.5~2.
CN201010162911A 2010-05-05 2010-05-05 Method for making high-content rebaudioside-A stevioside Pending CN101830947A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250167A (en) * 2011-05-30 2011-11-23 周爱琴 Process for separating rebaudioside from stevioside
CN103570777A (en) * 2013-11-01 2014-02-12 湖南科源生物制品有限公司 Extraction and purification method of stevioside RA
CN105061527A (en) * 2015-08-31 2015-11-18 湖南威嘉生物科技有限公司 Process for refined production of stevioside

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250167A (en) * 2011-05-30 2011-11-23 周爱琴 Process for separating rebaudioside from stevioside
CN103570777A (en) * 2013-11-01 2014-02-12 湖南科源生物制品有限公司 Extraction and purification method of stevioside RA
CN105061527A (en) * 2015-08-31 2015-11-18 湖南威嘉生物科技有限公司 Process for refined production of stevioside

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Application publication date: 20100915