CN105440091A - Method for removing stevioside RB by anion exchange resin - Google Patents
Method for removing stevioside RB by anion exchange resin Download PDFInfo
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- CN105440091A CN105440091A CN201510989883.8A CN201510989883A CN105440091A CN 105440091 A CN105440091 A CN 105440091A CN 201510989883 A CN201510989883 A CN 201510989883A CN 105440091 A CN105440091 A CN 105440091A
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- exchange resin
- anionite
- steviol glycoside
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- stevioside
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to the field of natural high-potency sweetener extraction in the field of food additives, and provides a method for removing stevioside RB by anion exchange resin. The method comprises the following steps: adsorbing a stevioside solution containing RB by treated exchange resin; and reducing the content of RB in the solution to be lower than 1 percent and maintaining the content of other ingredients by means of selective adsorption of the anion exchange resin on RB. The method can be used for improving the product taste and removing unpleasant aftertaste on the one hand, and removing the RB ingredient in the high RB feed liquid on the other hand to facilitate subsequent treatment.
Description
Technical field
The present invention relates to natural high potency sweetener in foodstuff additive field and extract field, particularly remove the method for steviol glycoside RB.
Background technology
Steviol glycoside, also known as stevioside glycosides, it is a kind of mixture of the diterpene glucoside containing Multiple components extracted from the leaf of catananche's sweet Stevia, according to the division of natural phant chemistry, belong to the glucoside of tetracyclic diterpene, it is subject to the favor of people gradually with features such as high sugariness, low in calories, safety non-toxics, is widely used in the industries such as food, medicine, daily chemical industry at present.The sugariness of stevioside and mouthfeel depend on its glucosides component and content, in known 9 kinds of components, comprise Lay bud enlightening glycosides A (RebaudiosideA is called for short RA), stevioside (Stevioside is called for short ST), Lay bud enlightening glycosides B (RebaudiosideB is called for short RB), stevia rebaudianum bioside (Steviolbioside is called for short SB) etc., wherein the relative content of RA and ST in total glucosides is higher, sugariness is the highest, be equivalent to 200 ~ 350 times of sucrose, sweet taste characteristic is also close with sucrose, that one has high sugariness, low in calories, soluble, heat-resisting, the new type natural sweeting agent of the feature such as stable.RB sugariness is only 10 ~ 15 times of sucrose, and rear pained highly seasoned, containing bad pleasant impression.Therefore, utilize resin that the RB component in steviol glycoside is had very important meaning for improving products taste; On the other hand, remove the RB component in high RB feed liquid, facilitate follow-up process.
All contain RB in general Stevioside products, because RB sugariness is low, rear bitterness is highly seasoned, containing bad pleasant impression.Mostly utilize the purifying such as recrystallization method, enzyme process stevioside at present, and there is the bringing into of organic solvent in recrystallization technology, energy consumption is high, clearance is low shortcoming.
Summary of the invention
The object of the invention is to overcome enzyme process to enzyme purity with Active pharmaceutical is high, operation controls difficult problem, a kind of anionite-exchange resin is provided to remove the method for steviol glycoside RB, overcome the bringing into of organic solvent in recrystallization technology, energy consumption is high, clearance is low shortcoming, there is reaction conditions simply controlled, pollution-free, cost is low, clearance advantages of higher.
Technical problem of the present invention is solved mainly through following technical proposals:
A kind of anionite-exchange resin removes the method for steviol glycoside RB, it is characterized in that: under 10 ~ 40 DEG C of temperature condition, getting anionite-exchange resin loads in chromatography column, by the steviol glycoside feed liquid containing RB, adsorbed by anion-exchange column, collect effluent liquid, stop charging when RB content is increased to more than 1% in effluent liquid, by effluent liquid concentrate drying, obtain the Stevioside products of RB content≤1%.
Concrete, described anionite-exchange resin is macroporous type or gel-type anion exchange resin.
Concrete, described steviol glycoside feed liquid is take steviol glycoside as solute, and water is the mixing solutions of solvent, and this steviol glycoside feed concentration is 10 ~ 300g/L, PH is 4 ~ 6.
Concrete, described steviol glycoside feed liquid passes through anion-exchange column with the speed of 0.2 ~ 2BV/h.
Concrete, described anionite-exchange resin needs to do pre-treatment before loading chromatography column, adopts the aqueous sodium hydroxide solution of 3BV5% by anionite-exchange resin, is washed to PH < 9; Pass through anionite-exchange resin with the hydrochloric acid of 3BV5% again, be washed to PH > 5; Finally pass through anionite-exchange resin with the aqueous sodium hydroxide solution of 3BV5%, be washed to PH < 9.
Its principle of work is: under 10 ~ 40 DEG C of conditions, getting processed good exchange resin loads in chromatography column, blade diameter length ratio is 1:2 ~ 1:8, it is 10 ~ 300g/L that high RB content steviol glycoside mother liquor sugar is mixed with concentration, PH is the feed liquid of 4 ~ 6, feed liquid is adsorbed to out by chromatography column sweet with the speed of 0.2 ~ 2BV/h, when RB content is increased to more than 1% in effluent liquid, namely stops charging.By effluent liquid concentrate drying, the Stevioside products of RB content below 1% can be obtained.Adopt concentration be 0.5 ~ 10% sodium hydroxide solution wash-out is carried out to pillar, consumption is 1 ~ 5 times of resin volume, collect elutriant, elutriant, through subsequent disposal, can obtain the steviol glycoside byproduct of high RB content.
Utilize anionite-exchange resin to the selective adsorption of steviol glycoside component RB, the concentration of feed liquid and the adsorptive power of pH value to anionite-exchange resin have certain influence, excessive or too small adsorptive power and the efficiency that all can reduce resin of concentration.
Beneficial effect of the present invention: the Stevioside products RB content obtained by aforesaid method is below 1%.With not through removing compared with RB steviol glycoside, this product sweetness is higher, and mouthfeel is purer, without bad pleasant impression, has wide market outlook.Meanwhile, present method can be avoided using a large amount of organic solvents needed for recrystallization method, and can overcome enzyme process to enzyme purity with Active pharmaceutical is high, operation controls difficult problem.Have reaction conditions simply controlled, pollution-free, cost is low, clearance advantages of higher.
Accompanying drawing explanation
Fig. 1 is the efficient liquid phase chromatographic analysis collection of illustrative plates of feed liquid former state in the embodiment of the present invention 1;
Fig. 2 is the efficient liquid phase chromatographic analysis collection of illustrative plates of effluent liquid 1 in the embodiment of the present invention 1.
Embodiment
Below technical scheme of the present invention is described in further detail.
Embodiment 1
Feed concentration: 40g/L
Under 25 DEG C of conditions, get 04D macroporous type anionite-exchange resin 150mL and load in chromatography column, blade diameter length ratio is 1:4, carries out pre-treatment according to the following steps to resin: pass through resin with the sodium hydroxide of 3BV5%, be washed to PH < 9; Pass through resin with the hydrochloric acid of 3BV5% again, be washed to PH > 5; Finally pass through resin with the sodium hydroxide of 3BV5%, be washed to PH < 9.By high RB content steviol glycoside solution, (detecting total glucosides amount through efficient liquid phase chromatographic analysis is 90.05%, wherein RB content is 11.03%) add water that to be mixed with concentration be 40g/L, PH is the feed liquid of 5, feed liquid is adsorbed to out sweet with the speed of 0.3BV/h by chromatography column, Fractional Collections effluent liquid, when RB content is increased to more than 1% in effluent liquid, namely stop charging.
Mixed by effluent liquid 1 to effluent liquid 4, i.e. comprehensive sample 1, obtain the Stevioside products that RB content is 0.04%, treatment capacity reaches 654g/L.
Also can collect different effluent liquid according to the specification of product, as mixed by effluent liquid 1 to effluent liquid 5, i.e. comprehensive sample 2, obtain the Stevioside products that RB content is 0.26%, treatment capacity reaches 960g/L.
Adopt the sodium hydroxide solution of 300mL5% to carry out wash-out to pillar, collect elutriant, elutriant is through subsequent disposal, and obtaining RB content is 65.87%, and total glucosides amount is the steviol glycoside byproduct of 82.27%.
Embodiment 2
Feed concentration: 100g/L
Under 25 DEG C of conditions, get 07D gel-type anion exchange resin 100mL and load in chromatography column, blade diameter length ratio is 1:8, carries out pre-treatment according to the following steps to resin: pass through resin with the sodium hydroxide of 3BV5%, be washed to PH < 9; Pass through resin with the hydrochloric acid of 3BV5% again, be washed to PH > 5; Finally pass through resin with the sodium hydroxide of 3BV5%, be washed to PH < 9.By high RB content steviol glycoside solution, (detecting total glucosides amount through efficient liquid phase chromatographic analysis is 88.15%, wherein RB content is 10.98%) add water that to be mixed with concentration be 100g/L, PH is the feed liquid of 5, feed liquid is adsorbed to out sweet with the speed of 0.3BV/h by chromatography column, Fractional Collections effluent liquid, when RB content is increased to more than 1% in effluent liquid, namely stop charging.
Mixed by effluent liquid 1 to effluent liquid 2, i.e. comprehensive sample 1, obtain the Stevioside products that RB content is 0.01%, treatment capacity reaches 320g/L.
Also can collect different effluent liquid according to the specification of product, as mixed by effluent liquid 1 to effluent liquid 3, i.e. comprehensive sample 2, obtain the Stevioside products that RB content is 0.41%, treatment capacity reaches 557g/L.
Adopt the sodium hydroxide solution of 300mL2% to carry out wash-out to pillar, collect elutriant, elutriant is through subsequent disposal, and obtaining RB content is 68.13%, and total glucosides amount is the steviol glycoside byproduct of 83.47%.
The present embodiment is the embodiment of example of the present invention; for those skilled in the art; on the basis that the invention discloses application method and principle; be easy to make various types of improvement or distortion; and the structure be not limited only to described by the above-mentioned embodiment of the present invention, therefore previously described mode is preferred version, and does not have restrictive meaning; every equivalence done according to the present invention changes and amendment, all in the scope protection domain of claims of the present invention.
Claims (5)
1. the method for an anionite-exchange resin removal steviol glycoside RB, it is characterized in that: under 10 ~ 40 DEG C of temperature condition, getting anionite-exchange resin loads in chromatography column, by the steviol glycoside feed liquid containing RB, adsorbed by anion-exchange column, collect effluent liquid, stop charging when RB content is increased to more than 1% in effluent liquid, by effluent liquid concentrate drying, obtain the Stevioside products of RB content≤1%.
2. a kind of anionite-exchange resin according to claim 1 removes the method for steviol glycoside RB, it is characterized in that: described anionite-exchange resin is macroporous type or gel-type anion exchange resin.
3. a kind of anionite-exchange resin according to claim 1 removes the method for steviol glycoside RB, it is characterized in that: described steviol glycoside feed liquid is for being solute with steviol glycoside, water is the mixing solutions of solvent, and this steviol glycoside feed concentration is 10 ~ 300g/L, PH is 4 ~ 6.
4. a kind of anionite-exchange resin according to claim 1 removes the method for steviol glycoside RB, it is characterized in that: described steviol glycoside feed liquid passes through anion-exchange column with the speed of 0.2 ~ 2BV/h.
5. a kind of anionite-exchange resin according to claim 1 removes the method for steviol glycoside RB, it is characterized in that: described anionite-exchange resin needs to do pre-treatment before loading chromatography column, adopt the aqueous sodium hydroxide solution of 3BV5% by anionite-exchange resin, be washed to PH < 9; Pass through anionite-exchange resin with the hydrochloric acid of 3BV5% again, be washed to PH > 5; Finally pass through anionite-exchange resin with the aqueous sodium hydroxide solution of 3BV5%, be washed to PH < 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510989883.8A CN105440091A (en) | 2015-12-24 | 2015-12-24 | Method for removing stevioside RB by anion exchange resin |
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| CN201510989883.8A CN105440091A (en) | 2015-12-24 | 2015-12-24 | Method for removing stevioside RB by anion exchange resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2022524217A (en) * | 2019-04-06 | 2022-04-28 | カーギル インコーポレイテッド | Methods for Producing Plant Extraction Compositions |
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| CN1192447A (en) * | 1998-02-18 | 1998-09-09 | 南开大学 | Adsorption resin method for conectrating and separating vegetable baudy glucoside from stevioside |
| CN101270138A (en) * | 2007-03-23 | 2008-09-24 | 宁波绿之健药业有限公司 | Extracting method for high-content sweet inulin A3 |
| CN101366496A (en) * | 2008-09-17 | 2009-02-18 | 无锡绿色分离应用技术研究所有限公司 | Method for separating and purifying Stevioside RA and SS from Stevia rebaudiana Bertoni concentrated liquor |
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| WO2015126876A1 (en) * | 2014-02-18 | 2015-08-27 | Mcneil Nutritionals, Llc. | Process for separation, isolation and characterization of steviol glycosides |
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2015
- 2015-12-24 CN CN201510989883.8A patent/CN105440091A/en active Pending
Patent Citations (8)
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| CN1192447A (en) * | 1998-02-18 | 1998-09-09 | 南开大学 | Adsorption resin method for conectrating and separating vegetable baudy glucoside from stevioside |
| CN101270138A (en) * | 2007-03-23 | 2008-09-24 | 宁波绿之健药业有限公司 | Extracting method for high-content sweet inulin A3 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2022524217A (en) * | 2019-04-06 | 2022-04-28 | カーギル インコーポレイテッド | Methods for Producing Plant Extraction Compositions |
| JP7391993B2 (en) | 2019-04-06 | 2023-12-05 | カーギル インコーポレイテッド | Method for making plant extract compositions |
| US11931391B2 (en) | 2019-04-06 | 2024-03-19 | Cargill, Incorporated | Methods for making botanical extract composition |
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Application publication date: 20160330 |