CN106674307A - Method for extracting stevioside from stevia rebaudiana - Google Patents

Method for extracting stevioside from stevia rebaudiana Download PDF

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Publication number
CN106674307A
CN106674307A CN201610947863.9A CN201610947863A CN106674307A CN 106674307 A CN106674307 A CN 106674307A CN 201610947863 A CN201610947863 A CN 201610947863A CN 106674307 A CN106674307 A CN 106674307A
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ethanol
stevia rebaudiana
impurities
removal
ethyl acetate
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贾德军
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Mingguang City A Total Of Stevia Professional Cooperatives
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Mingguang City A Total Of Stevia Professional Cooperatives
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products

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  • 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)
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Abstract

The invention belongs to the technical field of agricultural cultivation, and particularly relates to a method for extracting stevioside from stevia rebaudiana. The method comprises steps as follows: 1), blade treatment; 2), first impurity removal; 3), extraction; 4), second impurity removal; 5), resin adsorption; 6), collection. The method has the beneficial effects as follows: the extraction effect is good, and the purity of the obtained stevioside is high and is 95% or higher averagely.

Description

A kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA
Technical field
The invention belongs to agricultural plantation technology field, and in particular to a kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA.
Background technology
STEVIA REBAUDIANA (stevia rebaudiana) calls sweet chrysanthemum ﹑ sugar grass, category composite family (Compositae), Si Taiweiya Category, original producton location is in South America subtropical zone.China started by sections such as Nanjing Botanical Garden Mem. Sun Yat-Sen, the Chinese Academy of Agricultural Sciences from 1976 Grind unit successively to plant experimentally successfully from Japan's introduction STEVIA REBAUDIANA.STEVIA REBAUDIANA contains 14 kinds of Wei amount Yuan Su 32 kinds of nutrient contents of ﹑, in vivo Not metabolism, do not accumulate, not carcinogenic, nontoxicity, its security obtained recognizing for the tissue such as international FAO and WHO and U.S. FAD Can, therefore it is both fabulous sugar source, is again good source of nutrition.
Stevioside, abbreviation stevioside is the class tool sweet taste extracted from dried STEVIA REBAUDIANA blade Terpenes glycocide, it is main comprising 8 kinds of glucosides with different sugarinesses.Stevioside has high sugariness (for the 200-300 of sucrose The characteristic of times) ﹑ (only the 1/300 of sucrose) low in calories, long-term consumption will not make one to get fat, particularly suitable obesity, diabetes, Hypertension, artery sclerosis, carious tooth patient use, and physics, stable chemical performance, without Fermented, stevia can be extended The shelf-life of glycosides product.Thus increasingly cause the concern and attention of people, in being widely used in food and medicine industry, praised It is the third the natural sugar source after sucrose, beet sugar, is most rising new sugar source.
The content of the invention
It is an object of the invention to provide a kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA.
The invention provides following technical scheme:
A kind of method that steviol glycoside is extracted from STEVIA REBAUDIANA, comprises the steps of,
1)Blade process, by STEVIA REBAUDIANA blade reject impurity and color and luster it is gloomy after, vacuum freeze drying is crushed, is sifted out, and obtains STEVIA REBAUDIANA powder;
2)First time removal of impurities, to step 1) in the STEVIA REBAUDIANA powder that obtains add the n-hexane of its weight 3-5 times, stir 20-40 Minute, filtration, recycling design, take STEVIA REBAUDIANA filter cake, dry, obtain the first removal of impurities powder;
3)Extract, step 2 is added in heating and stirring device)In the first removal of impurities powder for obtaining and its weight 3-5 times ethanol With water mixed solution, the heating-up temperature of heating and stirring device is 40-60 DEG C, and mixing speed is 200-300 rev/min, during process Between be 20-40 minutes, then filter, take filtrate, repeat to extract 1-3 merging filtrate afterwards, filtrate is dried, obtain steviol glycoside Crude product;
4)Second removal of impurities, by step 3)In the steviol glycoside crude product that obtains be dissolved in appropriate water, add and used after bodied ferric sulfate Calcium hydroxide adjusts pH to 7.5, after stirring 5-15 minutes, stands 10-20 minutes, filters, obtains the second removal of impurities is filtered liquid;
5)Resin adsorption;With the HPD-100 purification with macroreticular resin steps 4 through pretreatment)In the second removal of impurities for obtaining Filtrate, by loading after the second removal of impurities is filtered liquid reduced pressure concentration, flow velocity during HPD-100 resin adsorptions is 2 BV/h, adsorption saturation Afterwards, first then eluted with ethyl acetate mixed solvent with ethanol with the pure water rinsing 5-15 minute that flow velocity is 4 BV/h, washed De- speed is 3 BV/h, collects the eluent of ethanol and ethyl acetate mixed solvent, in the ethanol and ethyl acetate mixtures, Ethanol is 5 with the volume ratio of ethyl acetate:2;
6)Collect, the ethanol collected and ethyl acetate mixed solvent eluent are concentrated by evaporation, are dried, obtain final product steviol glycoside.
Preferably, the step 3)Middle ethanol and water mixed solvent, the mass percent of ethanol is 40%-60%.
Contain some atent solvents in general polymeric adsorbent, therefore different depth must be carried out pre- according to needs are applied using before Process:First in extraction column, resin 1-2 hours are washed with clear water adverse current, then just stream washes 1-2 hours.After putting water purification, addition is higher than The ethanol immersion 3-4 hours of 20-30 centimetre of resin bed, then put net cleaning solution, are a cleaning process.With same method repeatedly Outlet cleaning solution sampling is washed till in test tube plus till 3 times of amount water do not show muddiness, then with the abundant drip washing of clear water to without obvious second Alcohol smell, that is, complete preprocessing process.
The invention has the beneficial effects as follows:Extraction effect is good, and the steviol glycoside purity for obtaining is high, average out to more than 95%.
Specific embodiment
Embodiment 1
It is a kind of from STEVIA REBAUDIANA extract steviol glycoside method, by STEVIA REBAUDIANA blade reject impurity and color and luster it is gloomy after, vacuum is cold Jelly dry, pulverize, sift out, and obtain STEVIA REBAUDIANA powder;
Take the above-mentioned g of STEVIA REBAUDIANA powder 500 and add 1.5 Kg n-hexanes, stirring 20 minutes, filtration, recycling design take STEVIA REBAUDIANA filter Cake, dry, obtain the first removal of impurities powder;Add in heating and stirring device the ethanol of 3 times of the first removal of impurities powder and its weight with In water mixed solution, the ethanol and water mixed solvent, the mass percent of ethanol is 40%, the heating temperature of heating and stirring device Spend for 40 DEG C, mixing speed is 200 revs/min, and process time is 20 minutes, is then filtered, and takes filtrate, and filtrate is dried, and is obtained To steviol glycoside crude product;Steviol glycoside crude product is dissolved in into appropriate water, add after bodied ferric sulfate with calcium hydroxide adjust pH to 7.5, after stirring 5 minutes, 10 minutes are stood, filter, obtain the second removal of impurities is filtered liquid;With the HPD-100 macropores through pretreatment Purification on adsorbent resins the second removal of impurities is filtered liquid, by loading after the second removal of impurities is filtered liquid reduced pressure concentration, during HPD-100 resin adsorptions Flow velocity is 2 BV/h, after adsorption saturation, first with the pure water rinsing that flow velocity is 4 BV/h 5 minutes, then with ethanol and ethyl acetate Mixed solvent is eluted, and elution speed is 3 BV/h, collects the eluent of ethanol and ethyl acetate mixed solvent, the ethanol In ethyl acetate mixtures, ethanol is 5 with the volume ratio of ethyl acetate:2;By the ethanol collected and ethyl acetate mixed solvent Eluent is concentrated by evaporation, drying, obtains final product steviol glycoside, and the purity of gained steviol glycoside is 95.8%.
Embodiment 2
It is a kind of from STEVIA REBAUDIANA extract steviol glycoside method, by STEVIA REBAUDIANA blade reject impurity and color and luster it is gloomy after, vacuum is cold Jelly dry, pulverize, sift out, and obtain STEVIA REBAUDIANA powder;
Take the above-mentioned g of STEVIA REBAUDIANA powder 500 and add 2.0 Kg n-hexanes, stirring 30 minutes, filtration, recycling design take STEVIA REBAUDIANA filter Cake, dry, obtain the first removal of impurities powder;Add in heating and stirring device the ethanol of 4 times of the first removal of impurities powder and its weight with In water mixed solution, the ethanol and water mixed solvent, the mass percent of ethanol is 50%, the heating temperature of heating and stirring device Spend for 50 DEG C, mixing speed is 250 revs/min, and process time is 30 minutes, is then filtered, and takes filtrate, and filtrate is dried, and is obtained To steviol glycoside crude product;Steviol glycoside crude product is dissolved in into appropriate water, add after bodied ferric sulfate with calcium hydroxide adjust pH to 7.5, after stirring 10 minutes, 15 minutes are stood, filter, obtain the second removal of impurities is filtered liquid;With the HPD-100 macropores through pretreatment Purification on adsorbent resins the second removal of impurities is filtered liquid, by loading after the second removal of impurities is filtered liquid reduced pressure concentration, during HPD-100 resin adsorptions Flow velocity is 2 BV/h, after adsorption saturation, first with the pure water rinsing that flow velocity is 4 BV/h 10 minutes, then with ethanol and ethyl acetate Mixed solvent is eluted, and elution speed is 3 BV/h, collects the eluent of ethanol and ethyl acetate mixed solvent, the ethanol In ethyl acetate mixtures, ethanol is 5 with the volume ratio of ethyl acetate:2;By the ethanol collected and ethyl acetate mixed solvent Eluent is concentrated by evaporation, drying, obtains final product steviol glycoside, and the purity of gained steviol glycoside is 96.5%.
Embodiment 3
It is a kind of from STEVIA REBAUDIANA extract steviol glycoside method, by STEVIA REBAUDIANA blade reject impurity and color and luster it is gloomy after, vacuum is cold Jelly dry, pulverize, sift out, and obtain STEVIA REBAUDIANA powder;
Take the above-mentioned g of STEVIA REBAUDIANA powder 500 and add 2.5 Kg n-hexanes, stirring 40 minutes, filtration, recycling design take STEVIA REBAUDIANA filter Cake, dry, obtain the first removal of impurities powder;Add in heating and stirring device the ethanol of 5 times of the first removal of impurities powder and its weight with In water mixed solution, the ethanol and water mixed solvent, the mass percent of ethanol is 60%, the heating temperature of heating and stirring device Spend for 60 DEG C, mixing speed is 300 revs/min, and process time is 40 minutes, is then filtered, and takes filtrate, and filtrate is dried, and is obtained To steviol glycoside crude product;Steviol glycoside crude product is dissolved in into appropriate water, add after bodied ferric sulfate with calcium hydroxide adjust pH to 7.5, after stirring 15 minutes, 20 minutes are stood, filter, obtain the second removal of impurities is filtered liquid;With the HPD-100 macropores through pretreatment Purification on adsorbent resins the second removal of impurities is filtered liquid, by loading after the second removal of impurities is filtered liquid reduced pressure concentration, during HPD-100 resin adsorptions Flow velocity is 2 BV/h, after adsorption saturation, first with the pure water rinsing that flow velocity is 4 BV/h 15 minutes, then with ethanol and ethyl acetate Mixed solvent is eluted, and elution speed is 3 BV/h, collects the eluent of ethanol and ethyl acetate mixed solvent, the ethanol In ethyl acetate mixtures, ethanol is 5 with the volume ratio of ethyl acetate:2;By the ethanol collected and ethyl acetate mixed solvent Eluent is concentrated by evaporation, drying, obtains final product steviol glycoside, and the purity of gained steviol glycoside is 97.2%.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, although with reference to aforementioned reality Apply example to be described in detail the present invention, for a person skilled in the art, it still can be to aforementioned each enforcement Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic.All essences in the present invention Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (2)

1. it is a kind of from STEVIA REBAUDIANA extract steviol glycoside method, it is characterised in that comprise the steps of,
1)Blade process, by STEVIA REBAUDIANA blade reject impurity and color and luster it is gloomy after, vacuum freeze drying is crushed, is sifted out, and obtains STEVIA REBAUDIANA powder;
2)First time removal of impurities, to step 1) in the STEVIA REBAUDIANA powder that obtains add the n-hexane of its weight 3-5 times, stir 20-40 Minute, filtration, recycling design, take STEVIA REBAUDIANA filter cake, dry, obtain the first removal of impurities powder;
3)Extract, step 2 is added in heating and stirring device)In the first removal of impurities powder for obtaining and its weight 3-5 times ethanol With water mixed solution, the heating-up temperature of heating and stirring device is 40-60 DEG C, and mixing speed is 200-300 rev/min, during process Between be 20-40 minutes, then filter, take filtrate, repeat to extract 1-3 merging filtrate afterwards, filtrate is dried, obtain steviol glycoside Crude product;
4)Second removal of impurities, by step 3)In the steviol glycoside crude product that obtains be dissolved in appropriate water, add and used after bodied ferric sulfate Calcium hydroxide adjusts pH to 7.5, after stirring 5-15 minutes, stands 10-20 minutes, filters, obtains the second removal of impurities is filtered liquid;
5)Resin adsorption, with the HPD-100 purification with macroreticular resin steps 4 through pretreatment)In the second removal of impurities for obtaining Filtrate, by loading after the second removal of impurities is filtered liquid reduced pressure concentration, flow velocity during HPD-100 resin adsorptions is 2 BV/h, adsorption saturation Afterwards, first then eluted with ethyl acetate mixed solvent with ethanol with the pure water rinsing 5-15 minute that flow velocity is 4 BV/h, washed De- speed is 3 BV/h, collects the eluent of ethanol and ethyl acetate mixed solvent, in the ethanol and ethyl acetate mixtures, Ethanol is 5 with the volume ratio of ethyl acetate:2;
6)Collect, the ethanol collected and ethyl acetate mixed solvent eluent are concentrated by evaporation, are dried, obtain final product steviol glycoside.
2. it is according to claim 1 it is a kind of from STEVIA REBAUDIANA extract steviol glycoside method, it is characterised in that the step 3)Middle ethanol and water mixed solvent, the mass percent of ethanol is 40%-60%.
CN201610947863.9A 2016-11-03 2016-11-03 Method for extracting stevioside from stevia rebaudiana Withdrawn CN106674307A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107312548A (en) * 2017-07-17 2017-11-03 河海大学 A kind of organic improvement base for promoting solonchak sodium ion exchange
CN107722082A (en) * 2017-09-30 2018-02-23 江苏艾斯维特生物科技有限公司 A kind of production method of stevioside
WO2020063894A1 (en) * 2018-09-30 2020-04-02 晨光生物科技集团股份有限公司 Industrial utilization method for stevia rebaudiana and stevioside and chlorogenic acid of stevia rebaudiana
CN111153944A (en) * 2019-09-26 2020-05-15 内蒙古昶辉生物科技股份有限公司 Method for extracting stevioside by adopting simulated moving bed chromatography

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WO2011112892A1 (en) * 2010-03-12 2011-09-15 Purecircle Usa Inc. High-purity steviol glycosides
CN102295668A (en) * 2010-12-03 2011-12-28 恩施清江生物工程有限公司 Method for preparing high-purity steviosides from stevia
CN105294790A (en) * 2015-12-07 2016-02-03 湖南华诚生物资源股份有限公司 Method for extracting high-purity steviol glycosides from stevia rebaudiana
CN106046075A (en) * 2016-06-17 2016-10-26 蚌埠市华东生物科技有限公司 Method for extracting stevioside from stevia rebaudiana leaves

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011112892A1 (en) * 2010-03-12 2011-09-15 Purecircle Usa Inc. High-purity steviol glycosides
CN102295668A (en) * 2010-12-03 2011-12-28 恩施清江生物工程有限公司 Method for preparing high-purity steviosides from stevia
CN105294790A (en) * 2015-12-07 2016-02-03 湖南华诚生物资源股份有限公司 Method for extracting high-purity steviol glycosides from stevia rebaudiana
CN106046075A (en) * 2016-06-17 2016-10-26 蚌埠市华东生物科技有限公司 Method for extracting stevioside from stevia rebaudiana leaves

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107312548A (en) * 2017-07-17 2017-11-03 河海大学 A kind of organic improvement base for promoting solonchak sodium ion exchange
CN107312548B (en) * 2017-07-17 2020-06-09 河海大学 Organic state improved base for promoting sodium ion exchange of saline soil
CN107722082A (en) * 2017-09-30 2018-02-23 江苏艾斯维特生物科技有限公司 A kind of production method of stevioside
CN107722082B (en) * 2017-09-30 2020-02-04 江苏艾斯维特生物科技有限公司 Production method of stevioside
WO2020063894A1 (en) * 2018-09-30 2020-04-02 晨光生物科技集团股份有限公司 Industrial utilization method for stevia rebaudiana and stevioside and chlorogenic acid of stevia rebaudiana
KR20210076030A (en) * 2018-09-30 2021-06-23 첸광 바이오테크 그룹 캄파니 리미티드 Industrial use method of Stevia rebaudiana and its stevioside and chlorogenic acid
KR102600268B1 (en) 2018-09-30 2023-11-10 첸광 바이오테크 그룹 캄파니 리미티드 Industrial use method of Stevia rebaudiana and its stevioside and chlorogenic acid
US11891411B2 (en) 2018-09-30 2024-02-06 Chenguang Biotech Group Co., Ltd. Industrial utilization method for Stevia rebaudiana and stevioside and chlorogenic acid of Stevia rebaudiana
CN111153944A (en) * 2019-09-26 2020-05-15 内蒙古昶辉生物科技股份有限公司 Method for extracting stevioside by adopting simulated moving bed chromatography

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Application publication date: 20170517