CN107936066A - A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside - Google Patents
A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside Download PDFInfo
- Publication number
- CN107936066A CN107936066A CN201711221887.7A CN201711221887A CN107936066A CN 107936066 A CN107936066 A CN 107936066A CN 201711221887 A CN201711221887 A CN 201711221887A CN 107936066 A CN107936066 A CN 107936066A
- Authority
- CN
- China
- Prior art keywords
- column
- steviol glycoside
- liquid glucose
- chromatographic
- chromatographic column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C07H1/08—Separation; Purification from natural products
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside, it is related to STEVIA REBAUDIANA extractive technique field, includes the following steps：(1) single stage desalting decolourizes, (2) two level desalination bleaching.The present invention uses two stage desalting decolorization to liquid glucose, and the single stage desalting for realizing liquid glucose first with sequential simulated mobile chromatography decolourizes, and removes most salt and pigment contained in liquid glucose；Decolorising agent and ion exchange resin is recycled to realize two level desalination bleaching, further remaining salt and pigment effectively in removing liquid glucose, make the removal efficiency of salt and pigment in liquid glucose reach more than 99%, so as to improve the content of steviol glycoside in product.
Description
Technical field：
The present invention relates to STEVIA REBAUDIANA extractive technique field, and in particular to a kind of liquid glucose using STEVIA REBAUDIANA extraction steviol glycoside
Desalination bleaching technique.
Background technology：
STEVIA REBAUDIANA, composite family, sweetleaf Chrysanthemum herbaceos perennial.Stem is upright, and base portion tip lignifying, top is tender, dense
Short down, corolla base portion light violet magenta or white, top white.Achene is linear, slightly flat, brown, has pappus.STEVIA REBAUDIANA is liked in temperature
Grown in the environment of warm moistening, it is light sensitive.Steviol glycoside, also known as stevioside, are one extracted from Stevia leaves
Kind glucosides.Steviol glycoside is a kind of natural sweetener of sugariness low in calories, high, is one of raw material of food and pharmaceutical industries.
At present, the general extraction methods of steviol glycoside be by by STEVIA REBAUDIANA cured leaf immersion in water, filter by liquid with
Leaf, stem separation, are further purified using water or food-grade alcohol etc..The technique has the following disadvantages：(1) production time
It is long, a large amount of virose preservatives are added in production, otherwise material will go bad, and part steviol glycoside can lose；(2) add
Flocculant, flocculates the suspended impurity to get off and activated carbon decolorizing absorbs the product of part, and steviol glycoside yield reduces.
The content of the invention：
The technical problems to be solved by the invention are to provide a kind of the degree of automation height and desalination bleaching effect is good with profit
In the liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside for improving steviol glycoside purity in product.
The technical problems to be solved by the invention are realized using following technical solution：
A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside, includes the following steps：
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
The sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 colors
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns are composed, each cycle is divided into three steps, and first walks out of salt component and colour component,
Colour component, No. 5 chromatographic column inlet feeds, outlet connection 6 are collected in time 350-400s, No. 2 chromatographic column import water inlets, outlet
Chromatographic column import, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns stop transporting at this time
OK；Second walks out of steviol glycoside component, time 450-500s, and No. 2 chromatographic column import water inlets, outlets connect No. 3 chromatographic column imports,
No. 3 column outlets connect No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect
No. 6 chromatographic column imports are connect, No. 6 column outlets collect steviol glycoside component；3rd step is circulates, time 600-650s, No. 1 color
Compose column outlet and connect No. 2 chromatographic column imports, No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4
Chromatographic column import, No. 4 column outlets No. 5 chromatographic column imports of connection, No. 5 column outlets No. 6 chromatographic column imports of connection, No. 6
Column outlet connects No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
During the double salt precipitation 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide.
Release agent used in the sequential simulated mobile chromatography is the Ca of granularity 0.25-0.35mm2+Type cation exchange tree
Fat.
The separation temperature of the sequential simulated mobile chromatography is controlled at 50-60 DEG C.
The ion exchange resin includes cation exchange resin and anion exchange resin, and anion exchange resin is weak
Alkalescence anion-exchange resin.
The decolorising agent selects activated carbon.
The decolorising agent is made of the raw material of following parts by weight：10-15 parts of water process level polyglutamic acid, 4A molecular sieves
10-15 parts of powder, 5-10 parts of N hydroxymethyl acrylamide, 1-5 parts of PEG-60 rilanit specials, trimethylolpropane tris is activated to shrink
0.5-2 parts of glycerin ether, 0.05-0.5 parts of potassium peroxydisulfate, 0.05-0.5 parts of sodium sulfite；
Its preparation method comprises the following steps：
(1) 45-50 DEG C of water is added dropwise until being completely dissolved into N hydroxymethyl acrylamide under stirring, adds potassium peroxydisulfate
And sodium sulfite, the reaction of reflux state insulated and stirred is heated to, mixed liquor is concentrated under reduced pressure after cross-linking reaction is complete, white to be had
Solid separate out when stop concentration, residue is transferred to sealing and standing 8-12h in 5-10 DEG C of environment, filter, gained white solid in
Dried in 55-60 DEG C of baking oven to constant weight, up to self-crosslinking acrylic resin；
(2) 45-50 DEG C of water is added dropwise until being completely dissolved into water process level polyglutamic acid under stirring, and utilizes dilute sulfuric acid
Solution ph is adjusted to 4-5, made self-crosslinking acrylic resin is added, adds 45-50 DEG C of water until self-crosslinking acrylic tree
Fat is completely dissolved, and is heated to the reaction of reflux state insulated and stirred, is sent into gained mixed liquor after esterification and is spray-dried
In machine, micro mist is made through micronizer in dry gained particle, up to polyglutamic acid/acrylic resin carboxylate；
(3) 4A molecular sieve activations powder, PEG-60 hydrogen are added into above-mentioned made polyglutamic acid/acrylic resin carboxylate
Change castor oil and trihydroxymethylpropanyltri diglycidyl ether, be sufficiently mixed, by gained mixture in 50-55 DEG C of hot pressing temperature, heat
The particle of granularity 0.25-0.35mm is made through pulverizer for hot pressing 2-3min under pressure pressure 0.5-1MPa, obtained solid, up to decolourizing
Agent.
The beneficial effects of the invention are as follows：
(1) present invention uses two stage desalting decolorization to liquid glucose, and liquid glucose is realized first with sequential simulated mobile chromatography
Single stage desalting decoloration, remove most salt and pigment contained in liquid glucose；Recycle decolorising agent and ion exchange resin real
Existing two level desalination bleaching, further remaining salt and pigment effectively in removing liquid glucose, make the removal efficiency of salt and pigment in liquid glucose equal
Reach more than 99%, so as to improve the content of steviol glycoside in products made thereby；
(2) decolorising agent of the present invention has two kinds of selections, and one kind is activated carbon, and another kind is self-control decolorising agent, although activated carbon
Institute's saliferous and pigment in liquid glucose can be effectively removed, but can also adsorb a certain amount of steviol glycoside at the same time, so as to cause stevioside
The loss of glycosides；And contained salt and pigment can effectively be removed in liquid glucose by making decolorising agent by oneself, and relative to activated carbon its to stevia rebaudianum
The adsorbance very little of glucosides, so as to reduce the loss late of liquid glucose steviol glycoside after desalination bleaching is handled.
Embodiment：
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
Sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
Wherein, 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide during double salt precipitation；Sequential mould
The Ca that release agent used in intending mobile chromatography is granularity 0.25-0.3mm2+Type cation exchange resin；Sequential simulated mobile chromatography
Separation temperature control at 50-55 DEG C；Ion exchange resin includes cation exchange resin and anion exchange resin, anion
Exchanger resin is weak-base anion-exchange resin；Decolorising agent selects activated carbon.
Embodiment 2
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
Sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
Wherein, 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide during double salt precipitation；Sequential mould
The Ca that release agent used in intending mobile chromatography is granularity 0.25-0.3mm2+Type cation exchange resin；Sequential simulated mobile chromatography
Separation temperature control at 50-55 DEG C；Ion exchange resin includes cation exchange resin and anion exchange resin, anion
Exchanger resin is weak-base anion-exchange resin；Decolorising agent selects activated carbon.
The preparation of decolorising agent：
(1) 45-50 DEG C of water is added dropwise until being completely dissolved into 8g N hydroxymethyl acrylamides under stirring, adds 0.2g
Potassium peroxydisulfate and 0.1g sodium sulfites, are heated to the reaction of reflux state insulated and stirred, depressurize mixed liquor after cross-linking reaction is complete
Concentration, stops concentration when having white solid precipitation, residue is transferred to sealing and standing 12h in 5-10 DEG C of environment, filters, gained
White solid is dried to constant weight in 55-60 DEG C of baking oven, up to self-crosslinking acrylic resin；
(2) 45-50 DEG C of water is added dropwise until being completely dissolved into 10g water process level polyglutamic acids under stirring, and utilizes dilute
Sulfuric acid regulation solution pH value adds made self-crosslinking acrylic resin, adds 45-50 DEG C of water until selfing bipropenyl to 4-5
Acid resin is completely dissolved, and is heated to the reaction of reflux state insulated and stirred, is sent into gained mixed liquor after esterification and sprays
In drying machine, micro mist is made through micronizer in dry gained particle, up to polyglutamic acid/acrylic resin carboxylate；
(3) 10g 4A molecular sieve activations powder, 2g are added into above-mentioned made polyglutamic acid/acrylic resin carboxylate
PEG-60 rilanit specials and 0.5g trihydroxymethylpropanyltri diglycidyl ethers, are sufficiently mixed, by gained mixture in hot pressing temperature
The particle of granularity 0.25-0.3mm is made through pulverizer for hot pressing 3min under 50-55 DEG C of degree, hot pressing pressure 0.5MPa, obtained solid,
Up to decolorising agent.
Embodiment 3
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
Sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
Wherein, 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide during double salt precipitation；Sequential mould
The Ca that release agent used in intending mobile chromatography is granularity 0.25-0.3mm2+Type cation exchange resin；Sequential simulated mobile chromatography
Separation temperature control at 50-55 DEG C；Ion exchange resin includes cation exchange resin and anion exchange resin, anion
Exchanger resin is weak-base anion-exchange resin；Decolorising agent selects activated carbon.
The preparation of decolorising agent：
(1) 45-50 DEG C of water is added dropwise until being completely dissolved into 10g N hydroxymethyl acrylamides under stirring, adds 0.3g
Potassium peroxydisulfate and 0.1g sodium sulfites, are heated to the reaction of reflux state insulated and stirred, depressurize mixed liquor after cross-linking reaction is complete
Concentration, stops concentration when having white solid precipitation, residue is transferred to sealing and standing 12h in 5-10 DEG C of environment, filters, gained
White solid is dried to constant weight in 55-60 DEG C of baking oven, up to self-crosslinking acrylic resin；
(2) 45-50 DEG C of water is added dropwise until being completely dissolved into 15g water process level polyglutamic acids under stirring, and utilizes dilute
Sulfuric acid regulation solution pH value adds made self-crosslinking acrylic resin, adds 45-50 DEG C of water until selfing bipropenyl to 4-5
Acid resin is completely dissolved, and is heated to the reaction of reflux state insulated and stirred, is sent into gained mixed liquor after esterification and sprays
In drying machine, micro mist is made through micronizer in dry gained particle, up to polyglutamic acid/acrylic resin carboxylate；
(3) 15g 4A molecular sieve activations powder, 2g are added into above-mentioned made polyglutamic acid/acrylic resin carboxylate
PEG-60 rilanit specials and 1g trihydroxymethylpropanyltri diglycidyl ethers, are sufficiently mixed, by gained mixture in hot pressing temperature
The particle of granularity 0.25-0.3mm is made through pulverizer for 50-55 DEG C, hot pressing 3min under hot pressing pressure 0.5MPa, obtained solid, i.e.,
Obtain decolorising agent.
Reference examples 1
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
Sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
Wherein, 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide during double salt precipitation；Sequential mould
The Ca that release agent used in intending mobile chromatography is granularity 0.25-0.3mm2+Type cation exchange resin；Sequential simulated mobile chromatography
Separation temperature control at 50-55 DEG C；Ion exchange resin includes cation exchange resin and anion exchange resin, anion
Exchanger resin is weak-base anion-exchange resin；Decolorising agent selects activated carbon.
The preparation of decolorising agent：
(1) 45-50 DEG C of water is added dropwise until being completely dissolved into 10g N hydroxymethyl acrylamides under stirring, adds 0.3g
Potassium peroxydisulfate and 0.1g sodium sulfites, are heated to the reaction of reflux state insulated and stirred, depressurize mixed liquor after cross-linking reaction is complete
Concentration, stops concentration when having white solid precipitation, residue is transferred to sealing and standing 12h in 5-10 DEG C of environment, filters, gained
White solid is dried to constant weight in 55-60 DEG C of baking oven, up to self-crosslinking acrylic resin；
(2) made self-crosslinking acrylic resin, 15g 4A molecular sieve activations are added into 15g water process level polyglutamic acids
Powder, 2g PEG-60 rilanit specials and 1g trihydroxymethylpropanyltri diglycidyl ethers, are sufficiently mixed, by gained mixture in heat
Hot pressing 3min under 50-55 DEG C of temperature, hot pressing pressure 0.5MPa is pressed, of granularity 0.25-0.3mm is made through pulverizer for obtained solid
Grain, up to decolorising agent.
Reference examples 2
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose is using suitable obtained by press filtration
The mobile chromatography of sequence formula simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
Sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin
Desalination, up to steviol glycoside crude product.
Wherein, 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide during double salt precipitation；Sequential mould
The Ca that release agent used in intending mobile chromatography is granularity 0.25-0.3mm2+Type cation exchange resin；Sequential simulated mobile chromatography
Separation temperature control at 50-55 DEG C；Ion exchange resin includes cation exchange resin and anion exchange resin, anion
Exchanger resin is weak-base anion-exchange resin；Decolorising agent selects activated carbon.
The preparation of decolorising agent：
(1) 45-50 DEG C of water is added dropwise until being completely dissolved into 15g water process level polyglutamic acids under stirring, and utilizes dilute
Sulfuric acid regulation solution pH value adds 10g N hydroxymethyl acrylamides, adds 45-50 DEG C of water until selfing bipropenyl to 4-5
Acid resin is completely dissolved, and is heated to the reaction of reflux state insulated and stirred, is sent into gained mixed liquor after esterification and sprays
In drying machine, micro mist is made through micronizer in dry gained particle, up to polyglutamic acid/acrylic resin carboxylate；
(2) 15g 4A molecular sieve activations powder, 2g are added into above-mentioned made polyglutamic acid/acrylic resin carboxylate
PEG-60 rilanit specials and 1g trihydroxymethylpropanyltri diglycidyl ethers, are sufficiently mixed, by gained mixture in hot pressing temperature
The particle of granularity 0.25-0.3mm is made through pulverizer for 50-55 DEG C, hot pressing 3min under hot pressing pressure 0.5MPa, obtained solid, i.e.,
Obtain decolorising agent.
Embodiment 4
Be utilized respectively embodiment 1, embodiment 2, embodiment 3, reference examples 1, reference examples 2 to equivalent with batch through double salt precipitation and
Liquid glucose after press filtration carries out desalination bleaching processing, and each reagent dosage is identical, and measures salinity removal efficiency, pigment removal rate and institute
Steviol glycoside content in steviol glycoside crude product is obtained, as shown in table 1.
The desalination bleaching effect of the desalination bleaching technique of the present invention of table 1
| Group | Salinity removal efficiency/% | Pigment removal rate/% | Steviol glycoside content/% |
| Embodiment 1 | 99.6 | 99.7 | 74.5 |
| Embodiment 2 | 99.3 | 99.3 | 81.6 |
| Embodiment 3 | 99.5 | 99.4 | 82.3 |
| Reference examples 1 | 93.4 | 95.6 | 76.4 |
| Reference examples 2 | 82.7 | 79.2 | 63.5 |
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that include the following steps：
(1) single stage desalting decolourizes：By the liquid glucose after double salt precipitation by plate and frame filter press, liquid glucose obtained by press filtration uses sequential
The mobile chromatography of simulation carries out desalination bleaching, obtains salt component, colour component and steviol glycoside component；
The sequential simulated mobile chromatography is made of 6 root chromatogram columns, is followed successively by No. 1 chromatographic column, No. 2 chromatographic columns, No. 3 chromatographies
Column, No. 4 chromatographic columns, No. 5 chromatographic columns, No. 6 chromatographic columns, each cycle are divided into three steps, and first walks out of salt component and colour component, when
Between 350-400s, colour component, No. 6 No. 5 chromatographic column inlet feeds, outlet connection colors are collected in No. 2 chromatographic column imports water inlet, outlet
Column import is composed, No. 6 column outlets collect salt component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are out of service at this time；
Second walks out of steviol glycoside component, and time 450-500s, No. 2 chromatographic column imports are intake, outlet No. 3 chromatographic column imports of connection, No. 3
Column outlet connects No. 4 chromatographic column imports, and No. 4 column outlets connect No. 5 chromatographic column imports, No. 5 column outlet connections 6
Number chromatographic column import, No. 6 column outlets collect steviol glycoside components；3rd step is circulates, time 600-650s, No. 1 chromatography
Column outlet connects No. 2 chromatographic column imports, and No. 2 column outlets connect No. 3 chromatographic column imports, No. 3 column outlets connect No. 4 colors
Column import is composed, No. 4 column outlets connect No. 5 chromatographic column imports, and No. 5 column outlets connect No. 6 chromatographic column imports, No. 6 colors
Compose column outlet and connect No. 1 chromatographic column import；
(2) two level desalination bleaching：Gained steviol glycoside component is first used into bleaching agent bleaching, recycles ion exchange resin to take off
Salt, up to steviol glycoside crude product.
2. the liquid glucose desalination bleaching technique according to claim 1 using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that：
During the double salt precipitation 9 are adjusted to as inorganic agent, liquid glucose pH value using ferric trichloride and calcium hydroxide.
3. the liquid glucose desalination bleaching technique according to claim 1 using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that：
Release agent used in the sequential simulated mobile chromatography is the Ca of granularity 0.25-0.35mm2+Type cation exchange resin.
4. the liquid glucose desalination bleaching technique according to claim 1 using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that：
The separation temperature of the sequential simulated mobile chromatography is controlled at 50-60 DEG C.
5. the liquid glucose desalination bleaching technique according to claim 1 using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that：
The ion exchange resin includes cation exchange resin and anion exchange resin, anion exchange resin for alkalescent the moon from
Sub-exchange resin.
6. the liquid glucose desalination bleaching technique according to claim 1 using STEVIA REBAUDIANA extraction steviol glycoside, it is characterised in that：
The decolorising agent selects activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711221887.7A CN107936066A (en) | 2017-11-29 | 2017-11-29 | A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711221887.7A CN107936066A (en) | 2017-11-29 | 2017-11-29 | A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107936066A true CN107936066A (en) | 2018-04-20 |
Family
ID=61950534
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711221887.7A Pending CN107936066A (en) | 2017-11-29 | 2017-11-29 | A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107936066A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368716A (en) * | 2019-07-31 | 2019-10-25 | 赛普特环保技术(厦门)有限公司 | A kind of sugar, inorganic salts separation system and method |
| CN114213477A (en) * | 2021-12-21 | 2022-03-22 | 黑龙江八一农垦大学 | Starch syrup decoloring method based on simulated mobile chromatography |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101503435A (en) * | 2009-03-26 | 2009-08-12 | 李善汪 | Method for purifying stevioside by secondary ion exchange |
| CN102775452A (en) * | 2012-06-14 | 2012-11-14 | 甘肃普华甜菊糖开发有限公司 | Stevioside purification process |
| CN102786565A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Process for purifying stevia glycosides by multi-column resin series connection and alcoholic absorption |
| CN102786567A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Method for preparing high-purity stevioside through multi-column serial resins absorption and separated column analysis |
| CN106366137A (en) * | 2016-08-27 | 2017-02-01 | 山东绿健生物技术有限公司 | Desalting and decolorizing method of isomerized lactose liquid |
| CN106749448A (en) * | 2016-12-07 | 2017-05-31 | 辽宁科技大学 | A kind of method that SMBC method extracts steviol glycoside in STEVIA REBAUDIANA |
| CN107383128A (en) * | 2017-08-01 | 2017-11-24 | 江南大学 | A kind of discoloration method of steviol glycoside aqueous extract |
-
2017
- 2017-11-29 CN CN201711221887.7A patent/CN107936066A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101503435A (en) * | 2009-03-26 | 2009-08-12 | 李善汪 | Method for purifying stevioside by secondary ion exchange |
| CN102775452A (en) * | 2012-06-14 | 2012-11-14 | 甘肃普华甜菊糖开发有限公司 | Stevioside purification process |
| CN102786565A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Process for purifying stevia glycosides by multi-column resin series connection and alcoholic absorption |
| CN102786567A (en) * | 2012-09-07 | 2012-11-21 | 谱赛科（江西）生物技术有限公司 | Method for preparing high-purity stevioside through multi-column serial resins absorption and separated column analysis |
| CN106366137A (en) * | 2016-08-27 | 2017-02-01 | 山东绿健生物技术有限公司 | Desalting and decolorizing method of isomerized lactose liquid |
| CN106749448A (en) * | 2016-12-07 | 2017-05-31 | 辽宁科技大学 | A kind of method that SMBC method extracts steviol glycoside in STEVIA REBAUDIANA |
| CN107383128A (en) * | 2017-08-01 | 2017-11-24 | 江南大学 | A kind of discoloration method of steviol glycoside aqueous extract |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368716A (en) * | 2019-07-31 | 2019-10-25 | 赛普特环保技术(厦门)有限公司 | A kind of sugar, inorganic salts separation system and method |
| CN110368716B (en) * | 2019-07-31 | 2023-11-14 | 赛普特环保技术(厦门)有限公司 | Sugar and inorganic salt separation system and method |
| CN114213477A (en) * | 2021-12-21 | 2022-03-22 | 黑龙江八一农垦大学 | Starch syrup decoloring method based on simulated mobile chromatography |
| CN114213477B (en) * | 2021-12-21 | 2023-08-15 | 黑龙江八一农垦大学 | Starch syrup decoloring method based on simulated mobile chromatography |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR102600268B1 (en) | Industrial use method of Stevia rebaudiana and its stevioside and chlorogenic acid | |
| KR100864471B1 (en) | A processed ginseng using extract of herb medicine and a producing method thereof | |
| CN104262413B (en) | Preparation method of trehalose anhydrous | |
| KR102580703B1 (en) | Stevia rebaudiana industrialized method for simultaneously producing chlorogenic acid and stevioside | |
| CN102924240B (en) | Method for extracting total magnolol according to alcoholic-alkaline method | |
| CN107936066A (en) | A kind of liquid glucose desalination bleaching technique using STEVIA REBAUDIANA extraction steviol glycoside | |
| CN102936534A (en) | Process for simultaneously extracting phosphatide, gossypol and pigments from cottonseed oil | |
| CN102492054B (en) | Preparation method of soybean episperm pectin gel polysaccharide | |
| CN108558971A (en) | A kind of preparation method of roselle anthocyanin | |
| CN107955047A (en) | A kind of STEVIA REBAUDIANA water puies forward the flocculation purification method of liquid glucose | |
| CN103435682B (en) | Wheat germ protein source antioxidative peptide, and preparation method and application thereof | |
| CN105237654A (en) | Method for extracting pectin from orange peel | |
| CN103012544B (en) | A kind of method extracting saponin and polysaccharide from tea seed grouts | |
| CN100575357C (en) | A kind of method of from glutinous rehmannia, extracting rehmannia root oligose and Dihuang polysaccharide simultaneously | |
| CN107011457B (en) | A method of extracting preparation non-starch polysaccharide and small molecule nutrient molecule from sweet potato waste water | |
| CN104387498B (en) | Technical method for simultaneously preparing premna microphylla pectin and premna microphylla sodium copper chlorophyll from premna microphylla | |
| CN109971365B (en) | Production process of fresh pigskin gelatin | |
| CN104926719B (en) | A kind of method that trigonelline is extracted from fructus cannabis | |
| CN103146476A (en) | Green extraction technique capable of comprehensively and efficiently utilizing sophora flower bud | |
| CN106834383B (en) | Method for improving quality of lycium barbarum polysaccharide and application thereof | |
| EP1241155B1 (en) | Method of obtaining pinitol from carob extracts | |
| CN1329362C (en) | Method for extracting chlorogenic acid and sunflower protein from sunflower seed cake | |
| CN103242362B (en) | Membrane technique prepares the production method of High-purity Phytic Acid calcium | |
| CN103265583A (en) | Method for preparing stachyose crystal | |
| CN101289461A (en) | Process for extracting phytic acid from virus-free waste liquid of rapeseed extraction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180420 |
|
| RJ01 | Rejection of invention patent application after publication |