CN102702284A - Production process of high-purity sweet tea glycosides - Google Patents
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Abstract
The invention discloses a production process of high-purity sweet tea glycosides. The production process comprises the steps of extracting, condensing, flocculating, clarifying, centrifugally separating, refining macroporous resin, ion exchange resin decolorizing, using desalting resin for desalting, conducting composite decolorizing and condensing, and then conducting spray-drying on thick paste to obtain powder with color of milk white to white, namely, high-purity sweet tea glycosides with content of not less than 98%. The production process has the advantages that the high-purity debitterized sweet tea glycosides with content of not less than 98% and color of milk white to white can be produced in batch, so that the problem that the product can not be produced in batch on the market; the product can occupy the sweetener market; a feasible production process path is found to produce sweet tea glycosides in batch. According to chemical component characteristic of Guangxi sweet tea, key production links such as flocculating, clarifying, macroporous resin refining, ion exchange resin decolorizing and debitterizing, desalting resin for desalting and debitterizing, composite decolorizing and on the like are combined effectively.
Description
Technical field
The present invention relates to the extraction of sweet tea glycosides, specifically is to be the production technique of the sweet tea glycosides of raw material extraction high purity with the Guangxi Folium hydrangeae strigosae leaf.
Background technology
Commercially available sweet tea extract (specification: 70% sweet tea glycosides; HPLC detects) be that the dry leave of Lee is a raw material with the sweet tea Rubus of Rosaceae rubus Suavissmus S, carry → filters → product that macroporous resin → ion exchange resin → concentrated → explained hereafter such as drying are come out through water; Purity≤74% of the sweet tea glycosides of its effective constituent; Color is faint yellow, has the back bitter taste, defines the market of this product.
Mainly contain compositions such as sweet tea glycosides, sweet tea polyphenols and flavones, gallogen, protein, amino acid, chlorophyll in the sweet tea; Easy separation and easy purification not; Cause the purity and the equal difficulty of color of the sweet tea glycosides of product to reach high-quality requirement; Make product have the back bitter taste, need the composition beyond the sweet tea glycosides be removed as far as possible.
At present a domestic only tame enterprise can be with the industrialization of sweet tea glycosides, but quality does not reach high-quality requirement.Mainly be that these technologies and technology exist cost high, use poisonous organic reagent in a large number, characteristics such as production process is loaded down with trivial details are so that be difficult to realize industrialization.
Summary of the invention
The objective of the invention is for overcoming the deficiency of prior art, is the technology that raw material extracts the sweet tea glycosides of high purity and provide a kind of with the Guangxi Folium hydrangeae strigosae leaf.It is white to white that the product color that this extraction process is produced is milk, bitter taste without issue, and the content of sweet tea glycosides reaches more than 98%.
The technical scheme that realizes the object of the invention is:
A kind of high purity is the technology that raw material extracts sweet tea glycosides with the Guangxi Folium hydrangeae strigosae leaf, comprises the steps:
(1) extracts: get Guangxi Folium hydrangeae strigosae leaf dry product; Pulverize the back and drop in the extractor, extract 3 times down in slight boiling condition with tap water, adding from the beginning, the water yield is respectively 8,6,7 times; Extraction time is respectively 1.5h, 1h, 1h, and the filter residue after each the filtration gets into next time and extracts;
(2) concentrate: preceding 2 Guangxi Folium hydrangeae strigosae leaf extracts are concentrated into heavy 3 ~ 4 times of sweet tea cured leaf raw material;
(3) flocculate and clarify: liquid concentrator is cooled to 40 ~ 45 ℃, opens steam then and maintain the temperature within this scope; The water-soluble chitosan that adds Guangxi Folium hydrangeae strigosae raw material weight 0.2% ~ 0.4% fully stirs and makes the water-soluble chitosan dissolving, insulation 2h, and every 40min stirs 1 time;
(4) spinning: will separate with high speed centrifugation through the liquid concentrator of flocculate and clarify, centrifugation is filled, and centrifugate is advanced next step operation;
(5) macroporous resin is refining: centrifugate is advanced macroporous adsorptive resins, is the charging terminal point when not having sweet taste and feeding liquid color and drop to the resin height of bed 4/5 with effluent; After having advanced feed liquid, be washed till the effluent water white transparency with purified water earlier, use 60 ~ 65 degree alcohol desorptions then, collect, collect the stripping liquid that resin bed volume 1.5-2.0 doubly measures volume altogether from pleasantly sweet the beginning;
(6) ion-exchange resin decolorization: with the concentrated ethanol that reclaimed of macroporous adsorbent resin stripping liquid, the control concentrating degree is the Guangxi Folium hydrangeae strigosae leaf raw material: the liquid concentrator volume is 1:1; Then with liquid concentrator through anionite-exchange resin, use the purified water wash-out again, collect from pleasantly sweet the beginning, when being collected into no sweet taste till, must elutriant;
(7) desalination resin desalination: the pleasantly sweet effluent and the elutriant of ion exchange resin are advanced the desalination resin column, and sample size is that every 1000L destainer advances 800kg desalination resin; After having advanced feed liquid, be washed till effluent bitter taste without issue with purified water earlier, with 65 degree alcohol desorptions, collect then, collect the stripping liquid that resin bed volume 2.0-2.5 doubly measures volume altogether from pleasantly sweet the beginning;
(8) composite decoloration: in desalination resin stripping liquid, add composite decoloring agent, fully stir and mix, place 20min, restir 5min use Plate Filtration after leaving standstill 15min, gets clear look shallow destainer;
(9) concentrate: destainer is concentrated reclaim ethanol, process the thick paste of 14 ~ 17 degree Beaume;
(10) the thick paste spraying drying is obtained color and luster and be the white powder of milk, the sweet tea glycosides of the high purity finished product of sweet tea glycosides content >=98% to white.
The said solvent extraction process of step (1) is No. the 3rd extracting solution of the 1st batch materials, as the 1st extraction solvent of the 2nd batch materials, applies mechanically extraction.
The said spinning mode of step (4) is the centrifugal or disc-type spinning of tubular type.
The kind of the said macroporous adsorbent resin of step (5) is D-101-I macroporous adsorbent resin, DM-130 macroporous adsorbent resin or CD-80 macroporous adsorbent resin; The desorb alcoholic acid number of degrees are the ethanol of 60 ~ 65 degree; The stripping liquid volume is that resin bed volume 1.5-2.0 doubly measures.
The kind of the said ion exchange resin of step (6) is D301, D958 or D762 anionite-exchange resin; Eluting solvent is a purified water.
The kind of the said desalination resin of step (7) is LX-11 or LX-60 desalination resin; The stripping liquid volume is 2.0 ~ 2.5 times of amounts of resin bed volume.
The kind of the said composite decoloring agent of step (8) is powdered carbon and bleaching clay; The add-on of discoloring agent is that powdered carbon is a stripping liquid volume 0.3% ~ 0.5%, and bleaching clay is 0.1% ~ 0.2%.
Advantage of the present invention is:
(1) industrialized mass production has gone out sweet tea glycosides >=98%, color is the white high-quality sweet tea extract to white, removal back bitter taste of milk, and having solved does not still have the problem of supplying this product in batches on the market, capture high-end sweeting agent market;
(2) look for a practicable production process route, produced sweet tea glycoside product in batches.According to the chemical ingredients characteristics of Guangxi Folium hydrangeae strigosae leaf, with flocculate and clarify, macroporous adsorbent resin is purified and debitterize, ion-exchange resin decolorization and debitterize, and desalination of desalination resin and debitterize, crucial manufacture link such as composite decoloration effectively combines.
Embodiment
To describe several embodiment below and further specify the present invention, but content of the present invention completion is not limited to therewith.
Embodiment 1:
A kind of is the production technique that raw material extracts the sweet tea glycosides of high purity with the Guangxi Folium hydrangeae strigosae leaf, comprises the steps:
(1) extracts: get Guangxi Folium hydrangeae strigosae leaf 1000kg; Pulverize the back and drop in the extractor, extract 3 times down in slight boiling condition with tap water, adding from the beginning, the water yield is respectively 8,6,7 times; No. the 3rd extracting solution of the 1st batch materials applied mechanically; As No. the 1st extracting solution of the 2nd batch materials, extraction time is respectively 1.5h, 1h, 1h, and the filter residue after each the filtration gets into next time and extracts;
(2) concentrate: preceding 2 Guangxi Folium hydrangeae strigosae leaf extracts are concentrated into heavy 3 times of sweet tea cured leaf raw material, are about 3000L;
(3) flocculate and clarify: liquid concentrator is cooled to 40 ~ 45 ℃, opens steam then and maintain the temperature within this scope; The water-soluble chitosan that adds Guangxi Folium hydrangeae strigosae raw material weight 0.3% fully stirs and makes the water-soluble chitosan dissolving, insulation 2h, and every 40min stirs 1 time;
(4) spinning: will use the tubular type spinning through the liquid concentrator of flocculate and clarify, centrifugation is filled, and centrifugate is advanced next step operation;
(5) macroporous resin is refining: centrifugate is advanced D-101-I macroporous adsorbent resin, is the charging terminal point when not having sweet taste and feeding liquid color and drop to the resin height of bed 4/5 with effluent; After having advanced feed liquid, be washed till the effluent water white transparency with purified water earlier, use 60 ~ 65 degree alcohol desorptions then, collect, collect the stripping liquid that resin bed volume 1.5-2.0 doubly measures volume altogether from pleasantly sweet the beginning;
(6) ion-exchange resin decolorization: with the concentrated ethanol that reclaimed of macroporous adsorbent resin stripping liquid, the control concentrating degree is the Guangxi Folium hydrangeae strigosae leaf raw material: the liquid concentrator volume is 1:1, and promptly the 1000kg raw material is concentrated into 1000L; Then with liquid concentrator through D301 anionite-exchange resin, use the purified water wash-out again, collect from pleasantly sweet the beginning, when being collected into no sweet taste till, must elutriant;
(7) desalination resin desalination: the pleasantly sweet effluent and the elutriant of ion exchange resin are advanced LX-11 desalination resin column, and sample size is that every 1000L destainer advances 800kg desalination resin; After having advanced feed liquid, be washed till effluent bitter taste without issue with purified water earlier, with 65 degree alcohol desorptions, collect then, collect the stripping liquid that resin bed volume 2.0-2.5 doubly measures volume altogether from pleasantly sweet the beginning;
(8) composite decoloration: in desalination resin stripping liquid, add powdered carbon and bleaching clay; The add-on of discoloring agent is that powdered carbon is a stripping liquid volume 0.3% ~ 0.5%, and bleaching clay is 0.1% ~ 0.2%, fully stirs and mixes, and places 20min, and restir 5min use Plate Filtration after leaving standstill 15min, gets clear look shallow destainer;
(9) concentrate: destainer is concentrated reclaim ethanol, process the thick paste of 14 ~ 17 degree Beaume;
(10) the thick paste spraying drying is obtained the powder that output 37.0 ~ 45.0kg, color and luster are white in color, the sweet tea glycosides of the high purity finished product of sweet tea glycosides content >=98%.Product yield 3.7% ~ 4.5%, sweet tea glycosides is 98.3%.
Products obtained therefrom is through checking: sweet tea glycosides is that chemical structure is similar with stevioside by the tetracyclic diterpene glycosides of steviol and glucose be combined into, and difference only is C
13Connect 1 molecule glucose on the position less.Its structural formula is following:
Sweet tea glycosides Rubusosode
The sweet tea glycosides of these article accounts for 5% of Guangxi Folium hydrangeae strigosae cured leaf, have high sugariness, low in calories, safety non-toxic remarkable advantage, sugariness is 200 times of sucrose, heat but has only 5% of sucrose.So sweet tea glycosides is specially adapted to mellitus, hyperpietic, the crowd of unsuitable sugar such as obesity uses.
Embodiment 2:
A kind of is the production technique that raw material extracts the sweet tea glycosides of high purity with the Guangxi Folium hydrangeae strigosae leaf, comprises the steps:
(1) extracts: get Guangxi Folium hydrangeae strigosae leaf 1000kg; Pulverize the back and drop in the extractor, extract 3 times down in slight boiling condition with tap water, adding from the beginning, the water yield is respectively 8,6,7 times; No. the 3rd extracting solution of the 1st batch materials applied mechanically; As No. the 1st extracting solution of the 2nd batch materials, extraction time is respectively 1.5h, 1h, 1h, and the filter residue after each the filtration gets into next time and extracts;
(2) concentrate: preceding 2 Guangxi Folium hydrangeae strigosae leaf extracts are concentrated into heavy 3 times of sweet tea cured leaf raw material, are about 3000L;
(3) flocculate and clarify: liquid concentrator is cooled to 40 ~ 45 ℃, opens steam then and maintain the temperature within this scope; The water-soluble chitosan that adds Guangxi Folium hydrangeae strigosae raw material weight 0.3% fully stirs and makes the water-soluble chitosan dissolving, insulation 2h, and every 40min stirs 1 time;
(4) spinning: will use the tubular type spinning through the liquid concentrator of flocculate and clarify, centrifugation is filled, and centrifugate is advanced next step operation;
(5) macroporous resin is refining: centrifugate is advanced the DM-130 macroporous adsorbent resin, is the charging terminal point when not having sweet taste and feeding liquid color and drop to the resin height of bed 4/5 with effluent; After having advanced feed liquid, be washed till the effluent water white transparency with purified water earlier, use 60 ~ 65 degree alcohol desorptions then, collect, collect the stripping liquid that resin bed volume 1.5-2.0 doubly measures volume altogether from pleasantly sweet the beginning;
(6) ion-exchange resin decolorization: with the concentrated ethanol that reclaimed of macroporous adsorbent resin stripping liquid, the control concentrating degree is the Guangxi Folium hydrangeae strigosae leaf raw material: the liquid concentrator volume is 1:1, and promptly the 1000kg raw material is concentrated into 1000L; Then with liquid concentrator through D762 anionite-exchange resin, use the purified water wash-out again, collect from pleasantly sweet the beginning, when being collected into no sweet taste till, must elutriant;
(7) desalination resin desalination: the pleasantly sweet effluent and the elutriant of ion exchange resin are advanced LX-60 desalination resin column, and sample size is that every 1000L destainer advances 800kg desalination resin; After having advanced feed liquid, be washed till effluent bitter taste without issue with purified water earlier, with 65 degree alcohol desorptions, collect then, collect the stripping liquid that resin bed volume 2.0-2.5 doubly measures volume altogether from pleasantly sweet the beginning;
(8) composite decoloration: in desalination resin stripping liquid, add powdered carbon and bleaching clay; The add-on of discoloring agent is that powdered carbon is a stripping liquid volume 0.3% ~ 0.5%, and bleaching clay is 0.1% ~ 0.2%, fully stirs and mixes, and places 20min, and restir 5min use Plate Filtration after leaving standstill 15min, gets clear look shallow destainer;
(9) concentrate: destainer is concentrated reclaim ethanol, process the thick paste of 14 ~ 17 degree Beaume;
(10) the thick paste spraying drying is obtained the powder that output 37.0 ~ 45.0kg, color and luster are white in color, the sweet tea glycosides of the high purity finished product of sweet tea glycosides content >=98%.Product yield 3.7% ~ 4.5%, sweet tea glycosides is 99.1%.
Claims (8)
1. one kind is the production technique that raw material extracts the sweet tea glycosides of high purity with the Guangxi Folium hydrangeae strigosae leaf, comprises the steps:
(1) extracts: get Guangxi Folium hydrangeae strigosae leaf dry product; Pulverize the back and drop in the extractor, extract 3 times down in slight boiling condition with tap water, adding from the beginning, the water yield is respectively 8,6,7 times; Extraction time is respectively 1.5h, 1h, 1h, and the filter residue after each the filtration gets into next time and extracts;
(2) concentrate: preceding 2 Guangxi Folium hydrangeae strigosae leaf extracts are concentrated into heavy 3 ~ 4 times of sweet tea cured leaf raw material;
(3) flocculate and clarify: liquid concentrator is cooled to 40 ~ 45 ℃, opens steam then and maintain the temperature within this scope; The water-soluble chitosan that adds Guangxi Folium hydrangeae strigosae raw material weight 0.2% ~ 0.4% fully stirs and makes the water-soluble chitosan dissolving, insulation 2h, and every 40min stirs 1 time;
(4) spinning: will separate with high speed centrifugation through the liquid concentrator of flocculate and clarify, centrifugation is filled, and centrifugate is advanced next step operation;
(5) macroporous resin is refining: centrifugate is advanced macroporous adsorptive resins, is the charging terminal point when not having sweet taste and feeding liquid color and drop to the resin height of bed 4/5 with effluent; After having advanced feed liquid, be washed till the effluent water white transparency with purified water earlier, use 60 ~ 65 degree alcohol desorptions then, collect, collect the stripping liquid that resin bed volume 1.5-2.0 doubly measures volume altogether from pleasantly sweet the beginning;
(6) ion-exchange resin decolorization: with the concentrated ethanol that reclaimed of macroporous adsorbent resin stripping liquid; The control concentrating degree is the Guangxi Folium hydrangeae strigosae leaf raw material: the liquid concentrator volume is 1:1; Then liquid concentrator is passed through anionite-exchange resin, use the purified water wash-out again, collect from pleasantly sweet the beginning; Till when being collected into no sweet taste, elutriant;
(7) desalination resin desalination: the pleasantly sweet effluent and the elutriant of ion exchange resin are advanced the desalination resin column, and sample size is that every 1000L destainer advances 800kg desalination resin; After having advanced feed liquid, be washed till effluent bitter taste without issue with purified water earlier, with 65 degree alcohol desorptions, collect then, collect the stripping liquid that resin bed volume 2.0-2.5 doubly measures volume altogether from pleasantly sweet the beginning;
(8) composite decoloration: in desalination resin stripping liquid, add composite decoloring agent, fully stir and mix, place 20min, restir 5min use Plate Filtration after leaving standstill 15min, gets clear look shallow destainer;
(9) concentrate: destainer is concentrated reclaim ethanol, process the thick paste of 14 ~ 17 degree Beaume;
(10) the thick paste spraying drying is obtained color and luster and be the white powder of milk, the sweet tea glycosides of the high purity finished product of sweet tea glycosides content >=98% to white.
2. extraction process according to claim 1 is characterized in that: the said solvent method of use of step (1) is No. the 3rd extracting solution of the 1st batch materials, applies mechanically as No. the 1st extracting solution solvent of the 2nd batch materials.
3. extraction process according to claim 1 is characterized in that: the said spinning mode of step (4) is the centrifugal or disc-type spinning of tubular type.
4. extraction process according to claim 1 is characterized in that: the kind of the said macroporous adsorbent resin of step (5) is D-101-I macroporous adsorbent resin, DM-130 macroporous adsorbent resin or CD-80 macroporous adsorbent resin; The desorb alcoholic acid number of degrees are the ethanol of 60 ~ 65 degree; The stripping liquid volume is that resin bed volume 1.5-2.0 doubly measures.
5. extraction process according to claim 1 is characterized in that: the kind of the said ion exchange resin of step (6) is D301, D958 or D762 anionite-exchange resin; Eluting solvent is a purified water.
6. extraction process according to claim 1 is characterized in that: the kind of the said desalination resin of step (7) is LX-11 or LX-60 desalination resin; The stripping liquid volume is 2.0 ~ 2.5 times of amounts of resin bed volume.
7. extraction process according to claim 1 is characterized in that: the kind of the said composite decoloring agent of step (8) is powdered carbon and bleaching clay; The add-on of discoloring agent is that powdered carbon is a stripping liquid volume 0.3% ~ 0.5%, and bleaching clay is 0.1% ~ 0.2%.
8. the sweet tea glycosides of high purity of content >=98% of producing with the described production technique of one of claim 1-7.
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| CN104193788A (en) * | 2014-09-05 | 2014-12-10 | 广西大学 | Extraction method of rubusoside |
| CN104262425A (en) * | 2014-08-15 | 2015-01-07 | 桂林莱茵生物科技股份有限公司 | Novel method for extracting rubusoside |
| CN104351444A (en) * | 2014-10-22 | 2015-02-18 | 浙江中烟工业有限责任公司 | Method for selecting and collecting aroma components in green tea leaves and aroma components prepared according to method |
| CN104370981A (en) * | 2014-09-30 | 2015-02-25 | 桂林市一峰食品有限公司 | Method for extraction of rubusoside from sweet tea |
| CN104926892A (en) * | 2015-06-04 | 2015-09-23 | 广西大学 | Method for extracting rubusoside from sweet tea |
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| CN108752392B (en) * | 2018-05-04 | 2020-10-02 | 湖南华诚生物资源股份有限公司 | Method for recovering sweet tea polyphenol from sweet tea flocculation residues after sweet tea glycoside extraction |
| CN108516997B (en) * | 2018-07-05 | 2020-06-26 | 湖南绿果甜品有限公司 | Method for extracting rubusoside from sweet tea leaves |
| CN108516997A (en) * | 2018-07-05 | 2018-09-11 | 湖南华诚生物资源股份有限公司 | A method of extracting Rubusoside from sweet tea |
| WO2020155494A1 (en) | 2019-01-30 | 2020-08-06 | 湖南绿蔓生物科技股份有限公司 | Sweetener composition and preparation method and use thereof |
| CN110078775A (en) * | 2019-05-08 | 2019-08-02 | 湖南华诚生物资源股份有限公司 | The environment-protection production method of high-content Rubusoside, sweet tea tannins |
| CN111227245A (en) * | 2020-01-14 | 2020-06-05 | 湖南华诚生物资源股份有限公司 | Preparation method and application of sweet tea instant powder rich in ellagic acid |
| CN111994921A (en) * | 2020-08-04 | 2020-11-27 | 宁夏锦华化工有限公司 | Monocyanamide decoloring method |
| CN113017063A (en) * | 2021-03-15 | 2021-06-25 | 湖南华诚生物资源股份有限公司 | Sweetener for improving taste and flavor of rubusoside and preparation method thereof |
| CN113017063B (en) * | 2021-03-15 | 2022-07-29 | 湖南华诚生物资源股份有限公司 | Sweetener for improving taste and flavor of rubusoside and preparation method thereof |
| CN113017066A (en) * | 2021-04-16 | 2021-06-25 | 湖南华诚生物资源股份有限公司 | Sugar substitute for improving sweet taste performance of rubusoside and preparation method thereof |
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