CN101194707B - High purity stevioside glycoside refining process - Google Patents
High purity stevioside glycoside refining process Download PDFInfo
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- CN101194707B CN101194707B CN2008100137117A CN200810013711A CN101194707B CN 101194707 B CN101194707 B CN 101194707B CN 2008100137117 A CN2008100137117 A CN 2008100137117A CN 200810013711 A CN200810013711 A CN 200810013711A CN 101194707 B CN101194707 B CN 101194707B
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- Prior art keywords
- steviosides
- ethanol
- liquid
- solid
- high purity
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- 235000019202 steviosides Nutrition 0.000 title claims abstract description 94
- 238000007670 refining Methods 0.000 title claims abstract description 25
- 229940013618 stevioside Drugs 0.000 title claims abstract description 23
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229930182470 glycoside Natural products 0.000 title 1
- -1 stevioside glycoside Chemical class 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000007788 liquid Substances 0.000 claims abstract description 34
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract 4
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 230000002093 peripheral effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 241000544066 Stevia Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
Landscapes
- Seasonings (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to a refining process of high-purity stevioside, which comprises heating up ethyl alcohol with weight percentage concentration of 88+-2% to 55-65 DEG C by peripheral vapor under the condition of stirring, and then putting stevioside powder into ethyl alcohol as stirring up under the temperature. The weight percentage of ethyl alcohol and stevioside powder is 2.2-2.7:1, the temperature of mixed liquid of ethyl alcohol and the stevioside rapidly decreased to a normal temperature in five minutes in cool water, and the mixed liquid is placed quietly and is stirred per several minutes, the dissolved mixture is separated from solid and liquid after placing quietly for 48-72 hours, and the obtained solid and liquid are dried to obtain refining stevioside. The stevioside whose A monomer content can exceed 95% is prepared in large scale through the process, and the purity is much higher compared with the current product, which can meet the user' requests for extremely top products with RA.
Description
Technical field:
The present invention relates to a kind of separation method of liquid mixture, specifically is the process for purification of Steviosides.
Background technology:
Stevioside can be widely used in industries such as varieties of food items, beverage, medicine, day chemical industry as a kind of novel sweetener.About the general production method of stevioside comparative maturity, the product RA content of just producing is difference to some extent, and the difference of RA content will cause application target obviously different with result of use.Therefore, a lot of scholars and research unit all are being devoted to study the method that improves product RA content.For example, a kind of process for purification of Steviosides is disclosed in Chinese patent ZL01127569.3, this method is to use Steviosides to be dissolved in edible ethanol at 25-70 ℃, in 1.4-1.7: 1 ratio, placed 12-32 hour complete molten back, stirred 10-15 minute in 2-4 hour at interval, filter crystal, crystal is water-soluble, spray after being condensed into 45% dried, product.Because this technological temperature parameter span of control is big, particularly complete molten back cooling control is reasonable inadequately, causes the product RA content of producing according to this kind method to be limited to for 88% (belonging to RA80), further improves product RA content and can't realize.The product of this RA content can not satisfy the demand of client to high end RA content product when using as foodstuff additive.
Summary of the invention
The object of the present invention is to provide a kind of process for purification of high purity stevioside; but utilize this method mass-producing to make Steviosides A monomer content (RA content) at the Steviosides more than 95%; and higher than currently available products purity, reach customer requirement, satisfy its expection expectation.
The present invention solves the concrete technical scheme that its technical problem takes:
To be mixed with weight percent concentration and be 88 ± 2% ethanol, under stirring state, be heated to 55-65 ℃ with the steam periphery, under this temperature, while stirring the Steviosides powder is put into ethanol, ethanol is 2.2-2.7 with Steviosides powder weight ratio: 1, after the Steviosides powder is molten entirely, in 5 minutes, the mixeding liquid temperature of described ethanol and Steviosides is reduced to normal temperature rapidly with cold water, leave standstill then, mix liquid during leaving standstill at set intervals, after placing 48-72 hour, to carry out solid-liquid separation through the dissolved mixture, the solid that obtains and liquid are carried out drying respectively after, obtain refining Steviosides.
Usually will carry out solid that solid-liquid separation obtains and add no salt solution and dissolve fully,, obtain refining Steviosides the solution drying; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, it is 45 ± 2% that gained Steviosides concentration of aqueous solution transfers to weight percent concentration, obtains refining Steviosides after the drying.
Steviosides and the mixed solvent temperature of ethanol are preferred 58-62 ℃ in the above-mentioned Steviosides treating process;
Preferably stirred the mixture 3-7 minute every 4-6 hour;
The equipment that mixture behind ethanol and the stevioside mixed dissolution is carried out solid-liquid separation is plate-and-frame filter press.
The invention has the beneficial effects as follows: because the solvent temperature of Steviosides is rationally controlled, cause Steviosides better to be separated being dissolved under the alcoholic acid situation each component, cooling can make other component and impurity be stranded in the ethanol rapidly, and Steviosides A separates out fast with crystalline form, and resulting crystal can obtain Steviosides A monomer content at the Steviosides more than 95% after purifying; The liquid that separation obtains after mixing obtains refining Steviosides after purifying; The overall yield of refining back Steviosides reaches 85%, the productive rate height; Steviosides taste fundamental sum sucrose after refining is suitable, and powder or lenticular are white in color.The present invention has thoroughly solved the problem of large-scale production high purity stevioside.Therefore, its creativeness of prior art is tangible relatively.
Test shows that the solvent temperature scope of controlling Steviosides and the rate of temperature fall of mixed solution are keys of the present invention.
But utilize present method mass-producing to make products such as Steviosides RA95, RA97.
Embodiment
Embodiment one
Choosing Steviosides A content and be 10 kilograms in 50% Steviosides powder and 22 kilograms of concentration and be 86% ethanol mixes, dissolving finishes and reduces to normal temperature rapidly in back 5 minutes in the time of 55 ℃, stirred the mixture 3 minutes every 4 hours, place after 48 hours, to carry out solid-liquid separation through plate-and-frame filter press through the dissolved mixture, the solid that leaches is added no salt solution concentration is transferred to 25%, be concentrated into 45%, the solution drying, obtain 4 kilograms of refining Steviosidess, Steviosides A content is 95.75% in this refining stevioside; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, the Steviosides concentration of aqueous solution will be transferred to 45%, obtain 4.5 kilograms of refining Steviosidess after the drying, the total yield 85% of Steviosides.
Embodiment two
Choosing Steviosides A content and be 10 kilograms in 55% Steviosides powder and concentration and be 25 kilograms of ethanol of 88% mixes, dissolving finishes and reduces to normal temperature rapidly in back 5 minutes in the time of 58 ℃, stirred the mixture 5 minutes every 5 hours, place after 60 hours, to carry out solid-liquid separation through plate-and-frame filter press through the dissolved mixture, the solid that leaches is added no salt solution concentration is transferred to 25%, be concentrated into 45%, the solution drying, obtain 5 kilograms of refining Steviosidess, Steviosides A content is 97.25% in this refining stevioside; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, the Steviosides concentration of aqueous solution will be transferred to 45%, obtain 3.6 kilograms of refining Steviosidess after the drying, the total yield 86% of Steviosides.
Embodiment three
Choosing Steviosides A content and be 10 kilograms in 57% Steviosides powder and concentration and be 27 kilograms of ethanol of 90% mixes, dissolving finishes and reduces to normal temperature rapidly in back 5 minutes in the time of 62 ℃, stirred the mixture 7 minutes every 6 hours, place after 72 hours, to carry out solid-liquid separation through plate-and-frame filter press through the dissolved mixture, the solid that leaches is added no salt solution concentration is transferred to 25%, be concentrated into 47%, the solution drying, obtain 5.4 kilograms of refining Steviosidess, Steviosides A content is 98.46% in this refining stevioside; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, the Steviosides concentration of aqueous solution will be transferred to 45%, obtain 3.5 kilograms of refining Steviosidess after the drying, the total yield 89% of Steviosides.
Embodiment four
Choosing Steviosides A content and be 10 kilograms in 53% Steviosides powder and concentration and be 25 kilograms of ethanol of 88% mixes, dissolving finishes and reduces to normal temperature rapidly in back 5 minutes in the time of 65 ℃, stirred the mixture 6 minutes every 5 hours, place after 60 hours, to carry out solid-liquid separation through plate-and-frame filter press through the dissolved mixture, the solid that leaches is added no salt solution concentration is transferred to 25%, be concentrated into 45%, the solution drying, obtain 4.8 kilograms of refining Steviosidess, Steviosides A content is 96.01% in this refining stevioside; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, the Steviosides concentration of aqueous solution will be transferred to 45%, obtain 3.75 kilograms of refining Steviosidess after the drying, the total yield 85.5% of Steviosides.
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 can be and directly takes from extract in the sweet Stevia blade before the present invention purified, and also can be the Steviosides that obtains after other method is refining.
The solvent temperature of Steviosides powder of the present invention in ethanol is to realize with steam periphery (periphery refers to that the annulus that larger storage tank overlaps between the little storage tank is a steam) heating under stirring state.
Claims (6)
1. the process for purification of high purity stevioside, it is characterized in that, to be mixed with weight percent concentration and be 88 ± 2% ethanol, under stirring state, be heated to 55-65 ℃ with the steam periphery, under this temperature, while stirring the Steviosides powder is put into ethanol, ethanol is 2.2-2.7 with Steviosides powder weight ratio: 1, after the Steviosides powder is molten entirely, in 5 minutes, the mixeding liquid temperature of described ethanol and Steviosides is reduced to normal temperature rapidly with cold water, leave standstill then, mix liquid during leaving standstill at set intervals, after placing 48-72 hour, to carry out solid-liquid separation through the dissolved mixture, the solid that obtains and liquid are carried out drying respectively after, obtain refining Steviosides.
2. the process for purification of high purity stevioside according to claim 1 is characterized in that, will carry out solid that solid-liquid separation obtains and add no salt solution and dissolve fully, with the solution drying, obtains refining Steviosides; To carry out the liquid that solid-liquid separation obtains and boil off ethanol and unnecessary water, it is 45 ± 2% that gained Steviosides concentration of aqueous solution transfers to weight percent concentration, obtains refining Steviosides after the drying.
3. the process for purification of high purity stevioside according to claim 1 and 2 is characterized in that, the mixed solvent temperature of Steviosides and ethanol is 58-62 ℃ in the Steviosides treating process.
4. the process for purification of high purity stevioside according to claim 1 and 2 is characterized in that, stirs the mixture 3-7 minute every 4-6 hour.
5. the process for purification of high purity stevioside according to claim 3 is characterized in that, stirs the mixture 3-7 minute every 4-6 hour.
6. the process for purification of high purity stevioside according to claim 1 is characterized in that, the equipment that the mixture behind ethanol and the Steviosides mixed dissolution is carried out solid-liquid separation is plate-and-frame filter press.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100137117A CN101194707B (en) | 2008-01-07 | 2008-01-07 | High purity stevioside glycoside refining process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100137117A CN101194707B (en) | 2008-01-07 | 2008-01-07 | High purity stevioside glycoside refining process |
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| CN101194707A CN101194707A (en) | 2008-06-11 |
| CN101194707B true CN101194707B (en) | 2010-10-20 |
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| CN2008100137117A Expired - Fee Related CN101194707B (en) | 2008-01-07 | 2008-01-07 | High purity stevioside glycoside refining process |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812096A (en) * | 2010-04-21 | 2010-08-25 | 赣州菊隆高科技实业有限公司 | Method for ultrasonically crystallizing rebaudiosideA |
| CN102286040A (en) * | 2011-08-09 | 2011-12-21 | 山东千千药业有限公司 | Refining method of high-purity steviosin |
| CN104151378A (en) * | 2014-08-12 | 2014-11-19 | 济南汉定生物工程有限公司 | Rebaudioside M purification method |
| 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 |
| CN114031655B (en) * | 2021-12-01 | 2024-02-20 | 江西海富生物工程有限公司 | Crystallization method of stevioside |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100727A (en) * | 1993-09-21 | 1995-03-29 | 袁斯鸣 | Method for purifying stevioside |
| CN1349997A (en) * | 2001-10-24 | 2002-05-22 | 青岛创升生物科技有限公司 | Stevioside glycoside refining process |
-
2008
- 2008-01-07 CN CN2008100137117A patent/CN101194707B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100727A (en) * | 1993-09-21 | 1995-03-29 | 袁斯鸣 | Method for purifying stevioside |
| CN1349997A (en) * | 2001-10-24 | 2002-05-22 | 青岛创升生物科技有限公司 | Stevioside glycoside refining process |
Non-Patent Citations (1)
| Title |
|---|
| 郭国瑞等.甜叶菊糖苷提取工艺的研究.《赣南师范学院学报》.1988,(第1期),42-46. * |
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| CN101194707A (en) | 2008-06-11 |
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