CN103408614A - Novel preparation technique of steviosin and Rebaudioside-A - Google Patents

Novel preparation technique of steviosin and Rebaudioside-A Download PDF

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CN103408614A
CN103408614A CN2013103288073A CN201310328807A CN103408614A CN 103408614 A CN103408614 A CN 103408614A CN 2013103288073 A CN2013103288073 A CN 2013103288073A CN 201310328807 A CN201310328807 A CN 201310328807A CN 103408614 A CN103408614 A CN 103408614A
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resin
water
steviosin
rebaudioside
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李玉山
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Abstract

The invention discloses a novel preparation technique of steviosin and Rebaudioside-A. The preparation technique mainly comprises the following steps: 1), water extraction; 2), flocculation and precipitation; 3), adsorption; 4), desalination; 5), desorption; 6), decolorization; 7), concentration; 8), crystallization and centrifugation; 9), drying; 10), mother liquor treatment. Thus, the high-purity steviosin and Rebaudioside-A are obtained. The novel preparation technique saves resource and is environmental friendly during the whole production process.

Description

The novel preparation technology of a kind of Steviosin and rebaudioside A
Technical field
The present invention relates to the novel preparation technology of a kind of Steviosin and rebaudioside A
Background technology
Steviosin is with steviol glycoside (C 38H 60O 18) be main mixing glycosides, press dry product and calculate, contain steviol glycoside (C 38H 60O 18) must not be less than 95.0%.The main sweet ingredient contained in stevioside leaf is called steviol glycoside (mixing glycosides), comprises rebaudioside A, steviol glycoside, RB, C, D, E, F, steviol B glycosides, sweetleaf immature fruit of Juteleaf Raspberry glycosides, Du Ke glycosides A and B, this,, for tieing up inferior glycosides etc., is divided into monoglycosides and disaccharide glycosides, aglycon is steviol, there is no sweet taste.Sweet Stevia can obtain by extracting purifying the mixture of monomer steviol glycoside or each monomer steviol glycoside.The steviol glycoside structural formula is as follows:
Figure BSA0000093285040000011
Figure BSA0000093285040000012
Figure BSA0000093285040000021
-G represents glucosyl group;-R represents rhamanopyranosyl;-X represents xylosyl.
The somatotype of sweet Stevia and steviol glycoside is with the ratio somatotype of rebaudioside A and steviol glycoside.
The sweet Stevia somatotype:
Or
Figure BSA0000093285040000023
The steviol glycoside somatotype:
Or
Figure BSA0000093285040000031
In Europe, steviol glycoside as a kind of novel sweetener, is more approved by European bag and bottle market as a green health theory, in European market, is contained the huge applications potentiality.China is steviol glycoside big export country, on December 18th, 2008 U.S. FDA announce the two glycosides A of stevioside as sweeting agent be " it is generally acknowledged safe material " (GRAS).On November 11st, 2011, European Parliament and board of management's approval steviol glycoside can be used 27 member statess, and this has created good opportunity for China's export.Europe stevia rebaudianum association (EUSTAS) has proposed steviol glycoside application standard 2007 and 2009 extremely similar in the steviol glycoside standard of promulgation in 2008 to foodstuff additive joint committee (JECFA).Steviol glycoside is by China at present, Japan, and Paraguay, the states such as Brazil produce, and Europe does not have enterprise to produce so far.Our country is from 1975~1978 years, the Chinese Academy of Agricultural Sciences, and the Botanical gardens, Nanjing, the research institutions such as Beijing Botanical Garden are successively from Japanese successful introduction, and have carried out partly plantation.Aspect, current world market, the current market value of the product of Steviosin 95% is 45~50 U.S. dollars, and the price of high purity Steviosin (content 98%) is 180 U.S. dollars.
Steviol glycoside does not affect the stability of other nutritive ingredients, has the effect of the hydroxyl radical free radical of removing; Reducing heat in diabetic subject 15 and beverage, is the sweeting agent do not contained heat; As correctives, be widely used in syrup, break up in the medicines such as agent tablet, pill; It is the sweeting agent of unlikely carious tooth; Has immunoregulation effect; Their Anti-Oxidant Effect; Strong, hypotensive activity in addition; Clothes can prevent and delay arteriosclerosis for a long time, so treatment diabetes, essential hypertension are suffered to significant curative effect.
The method of extracting Steviosin mainly contains at present: water extraction alcohol precipitation barium (calcium) salt impurity removal method; Water extraction iron (aluminium) salt removal of impurities resin adsorption method; Water extraction molysite removal of impurities n-butanol extraction; Water extraction aluminium salt removal of impurities degreasing ethanol precipitation; Water extraction soda acid removal of impurities n-butanol extraction; The methods such as water extraction iron (aluminium) salt removal of impurities resin adsorption method, but still water extraction iron (aluminium) the salt removal of impurities resin adsorption method of comparative maturity.What produce at present the conventional use of stevioside is the resin that specific surface area is larger, this resinoid has larger adsorptive capacity to steviol glycoside, but because micropore is more, adsorption rate is slower, easily stop up, vulnerable to pollution, do not reach the product specification of producing high-content Steviosin (98%) and high-content rebaudioside A (98%) yet.In order to address this problem, must find novel macroporous adsorbent resin, Fourth Ring diterpene hydrophobic in the steviol glycoside molecule does not partly have sweet taste for aglycon (steviol).Macroporous adsorbent resin is for absorption and screen the parting material that principle combines, and its adsorptivity is that the screening principle is because itself cellular structure determines due to the result of Van der Waals force or generation hydrogen bond.In general, the molecular size range of the compound be adsorbed and the power of polarity directly affect adsorption effect, and because the molecular weight of stevioside is larger, polymeric adsorbent used need have larger specific surface area and aperture.
The present invention has determined that based on rebaudioside A and Steviosin be the novel macroporous adsorbent resin of separate object, this resin screens scope greatly between molecular weight 850~960 to the composition in steviol glycoside, relatively, near the molecular weight 966 of rebaudioside A, also taken into account the screening and separating of other the main sweet ingredients in the sweet Stevia raw material simultaneously.The present invention utilizes a series of combined methods such as unique flocculation sediment, novelty resin absorption, specific solvent crystallization technique, completes step by step from sweet Stevia, extracting and separating Steviosin and high purity rebaudiodside A.
Summary of the invention
The first water liquid extracts: the sweet Stevia cured leaf adds tap water to boil extraction three times, and extracting liquid filtering, both can kill enzyme, can complete again, prevents enzymolysis, improves pleasant impression not good.
The second flocculation sediment: adopt composite flocculation agent, prescription proportioning: polymerized ferric-aluminum chloride: ammoniacal liquor (1: 0.5), first by polymerized ferric-aluminum chloride with water dissolution, be made into 5~10% solution, then by this solution and ammoniacal liquor mixed configuration, after stirring evenly, add in water extraction liquid, fully stir, at 30~50 ℃ of insulation 2~6h, filter liquor adds 1~5% PAM solution again, fully stirs insulation 2~6h, filter, filtrate is treated resin absorption.In water extraction liquid, contain a large amount of protein, organic acid, saponin(e, pigments etc., need flocculation to remove.
The 3rd absorption: above-mentioned filtered liquid, with macroporous adsorbent resin A absorption, detects with thin-layer chromatography, adsorbs after saturated and stops.
The 4th desalination: the resin after above-mentioned absorption is saturated washs with purified water, stops washing until water lotion detects substantially salt-free constituents, discards water lotion.Not by resin absorption, so used water is washed down it due to the salt constituents.
The 5th desorb: the resin after above-mentioned desalination, with ethanol elution, obtains the wash-out liquid glucose.
The 6th decolouring: with macroporous adsorbent resin B decolouring, pigment is by resin absorption by above-mentioned wash-out liquid glucose, and liquid glucose flows out resin column.
The 7th is concentrated: by above-mentioned liquid glucose vacuum concentration, obtain concentrated solution.
The 8th crystallization: will concentrate the about 250kg of material and enter in the purifying area crystallizer through pipeline, and open water coolant and be down to room temperature, crystallization 24h.
The 9th is centrifugal: crystallisate is centrifugal, obtains the high purity Steviosin.
The tenth mother liquid disposal: mother liquor is managed elsewhere, adds 3.5 times of amount specific solvent systems, and 70 ± 2 ℃ of heated and stirred 30min, open water coolant and be down to room temperature, and crystallization 24h obtains high purity rebaudiodside A.
The 11 drying: open opening for feed, the material that will dry is put into drying machine, closes opening for feed.Close the vacuum pumping valve, drive vacuum pump, keep vacuum tightness-0.08Mpa.Open the thermophore valve, control 40~60 ℃ of temperature, be about 2.5h time of drying.After dry materials completes, first close the heat-carrying valve, then to interlayer, inject water coolant, after waiting material to be cooled to normal temperature, stop vacuumizing, open the vacuum pumping valve, collect dried material with clean plastics bag.
The accompanying drawing explanation
Fig. 1 production technological process
Fig. 2 production unit schema
Embodiment
Sweet Stevia cured leaf 500Kg adds 15 times of amounts (w/w) tap water to boil extraction 2h, and extracting liquid filtering, filter residue boil and extract 1h with tap water again, and 0.5h, consumption are respectively 10 times, 6 times of amounts (w/w).The filtrate flocculation sediment, polymerized ferric-aluminum chloride liquid 750L with 5~10% joins in extracting solution, fully stirs, then adds 350L ammoniacal liquor fully to stir, at 30~50 ℃ of insulation 2~6h, filter, filtrate adds 1~5% PAM solution 150L again, fully stirs, filter, filtrate, with macroporous adsorbent resin A absorption, is detected with thin-layer chromatography, adsorbs after saturated and stops.The resin adsorbed after saturated washs with purified water, stops washing until water lotion detects substantially salt-free constituents, and approximately water 4000~4500L, discard water lotion.Resin after desalination, with 70~90% ethanol elutions, obtains the wash-out liquid glucose.The wash-out liquid glucose is with macroporous adsorbent resin B decolouring, and decolouring liquid glucose vacuum concentration, obtain concentrated solution.To concentrate the about 250kg of material and enter in the purifying area crystallizer through pipeline, and open water coolant and be down to room temperature, crystallization 24h.Crystallisate is centrifugal, and drying obtains high purity Steviosin 61.5Kg.Mother liquor is managed elsewhere, adds 3.5 times of amount specific solvent systems, and 70 ± 2 ℃ of heated and stirred 30min, open water coolant and be down to room temperature, and crystallization 24h is centrifugal, and drying obtains high purity rebaudiodside A14.8Kg.

Claims (4)

1. the novel preparation technology of a Steviosin and rebaudioside A, is characterized in that, take sweet Stevia as raw material through following steps:
(1) water liquid extracts: the sweet Stevia cured leaf adds tap water to boil extraction three times, and 15 times of amounts (W/W) are extracted 2h, and 10 times of amounts (W/W) are extracted 1h, and 6 times of amounts (W/W) are extracted 0.5h, filters, and obtains extracting solution.
(2) flocculation sediment: adopt composite flocculation agent (inorganic and combination), polymerized ferric-aluminum chloride: ammoniacal liquor (1: 0.5), polymerized ferric-aluminum chloride is made into to 5~10% solution, this liquid is mixed with ammoniacal liquor after stirring evenly to add in water extraction liquid and fully stir, insulation, filter, filtrate adds 1~5% PAM solution fully to stir again, insulation, filter, and filtrate is treated resin absorption.
(3) absorption: filtered liquid, with macroporous adsorbent resin A absorption, detects with thin-layer chromatography, adsorbs after saturated and stops.
(4) desalination: the resin adsorbed after saturated washs with purified water, removes the zwitterion in water, stops washing until water lotion detects substantially salt-free constituents, discards water lotion.
(5) desorb: eluent has larger solubleness can obtain the elutriant of high density to solute.The eluent of selecting is carried out to desorb with certain flow velocity by resin bed, collect stripping liquid.Resin after desalination, with ethanol elution, obtains the wash-out liquid glucose.
(6) decolouring: in the wash-out liquid glucose, contain a large amount of water colo(u)rs, must remove, with macroporous adsorbent resin B adsorption bleaching, pigment is by resin absorption, and liquid glucose flows out resin column.
(7) concentrated: the liquid glucose vacuum concentration obtains concentrated solution.
(8) crystallization: will concentrate the about 250kg of material and enter in the purifying area crystallizer through pipeline, and open water coolant and be down to room temperature, crystallization 24h.
(9) centrifugal: crystallisate is centrifugal, obtains the high purity Steviosin, and mother liquor is managed elsewhere.
(10) mother liquid disposal: in centrifuge mother liquor, add 3.5 times of amount specific solvent systems, 70 ± 2 ℃ of heated and stirred 30min, open water coolant and be down to room temperature, and crystallization 24h obtains high purity rebaudiodside A.
(11) drying: open opening for feed, the material that will dry is put into drying machine, closes opening for feed.Close the vacuum pumping valve, drive vacuum pump, keep vacuum tightness-0.08Mpa.Open the thermophore valve, control 40~60 ℃ of temperature, be about 2.5h time of drying.After dry materials completes, first close the heat-carrying valve, then to interlayer, inject water coolant, after waiting material to be cooled to normal temperature, stop vacuumizing, open the vacuum pumping valve, collect dried material with clean plastics bag, record weight, the broken post of powder feeding.
2. the novel preparation technology of a kind of Steviosin as described as right 1 and rebaudioside A, is characterized in that, with composite flocculation agent, processes in step (2), and the filtrate purity obtained is higher, limpider bright.
3. the novel preparation technology of a kind of Steviosin as described as right 1 and rebaudioside A, it is characterized in that, in step (3) and step (6), adopt novel macroporous adsorbent resin A, well adsorbed effective constituent, removed the salt constituents, novel macroporous adsorbent resin B has adsorbed pigment effectively, and to steviol glycoside substantially without adsorption.The surface-area of macroporous resin is large, exchange velocity is very fast, physical strength is high, contamination resistance is strong, thermally-stabilised good, in the aqueous solution and non-aqueous solution, can use, easily regeneration, can Reusability.
4. the novel preparation technology of a kind of Steviosin as described as right 1 and rebaudioside A, is characterized in that, adopts that specific solvent systems is extraordinary obtains highly purified rebaudioside A in step (10).
CN2013103288073A 2013-07-31 2013-07-31 Novel preparation technique of steviosin and Rebaudioside-A Pending CN103408614A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104049047B (en) * 2014-06-25 2015-09-02 曲阜圣香远生物科技有限公司 A kind of method evaluating quality of stevioside
CN105732739A (en) * 2016-01-29 2016-07-06 滁州润海甜叶菊高科有限公司 Technique for extracting and purifying stevioside from stevia
CN105801640A (en) * 2016-04-08 2016-07-27 江苏健佳药业有限公司 Preparation method of steviosin

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5910520A (en) * 1982-07-08 1984-01-20 Kikkoman Corp Production of soybean saponin
CN101100477A (en) * 2007-08-01 2008-01-09 江南大学 Method for extracting high pure rebaudioside A from stevia sugar
CN101220062A (en) * 2008-01-23 2008-07-16 石任兵 Method for preparing stevioside and rebaudiodside A simultaneously
CN102050850A (en) * 2009-10-30 2011-05-11 兴化格林生物制品有限公司 New extraction technology of stevioside and high purity rebaudioside A
CN102199178A (en) * 2011-04-10 2011-09-28 胡玮 Extraction process of rebaudioside A (RA)
CN102286040A (en) * 2011-08-09 2011-12-21 山东千千药业有限公司 Refining method of high-purity steviosin

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JPS5910520A (en) * 1982-07-08 1984-01-20 Kikkoman Corp Production of soybean saponin
CN101100477A (en) * 2007-08-01 2008-01-09 江南大学 Method for extracting high pure rebaudioside A from stevia sugar
CN101220062A (en) * 2008-01-23 2008-07-16 石任兵 Method for preparing stevioside and rebaudiodside A simultaneously
CN102050850A (en) * 2009-10-30 2011-05-11 兴化格林生物制品有限公司 New extraction technology of stevioside and high purity rebaudioside A
CN102199178A (en) * 2011-04-10 2011-09-28 胡玮 Extraction process of rebaudioside A (RA)
CN102286040A (en) * 2011-08-09 2011-12-21 山东千千药业有限公司 Refining method of high-purity steviosin

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104049047B (en) * 2014-06-25 2015-09-02 曲阜圣香远生物科技有限公司 A kind of method evaluating quality of stevioside
CN105732739A (en) * 2016-01-29 2016-07-06 滁州润海甜叶菊高科有限公司 Technique for extracting and purifying stevioside from stevia
CN105801640A (en) * 2016-04-08 2016-07-27 江苏健佳药业有限公司 Preparation method of steviosin

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