CN108033986A - The preparation method of Steviosin - Google Patents
The preparation method of Steviosin Download PDFInfo
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- CN108033986A CN108033986A CN201810121890.XA CN201810121890A CN108033986A CN 108033986 A CN108033986 A CN 108033986A CN 201810121890 A CN201810121890 A CN 201810121890A CN 108033986 A CN108033986 A CN 108033986A
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- China
- Prior art keywords
- steviosin
- stevia rebaudiana
- preparation
- extracting solution
- flow velocity
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- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 244000228451 Stevia rebaudiana Species 0.000 claims abstract description 31
- 235000006092 Stevia rebaudiana Nutrition 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 235000019202 steviosides Nutrition 0.000 claims description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 238000004587 chromatography analysis Methods 0.000 claims description 12
- 239000004383 Steviol glycoside Substances 0.000 claims description 11
- 229930182488 steviol glycoside Natural products 0.000 claims description 11
- 235000019411 steviol glycoside Nutrition 0.000 claims description 11
- 150000008144 steviol glycosides Chemical class 0.000 claims description 11
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000741 silica gel Substances 0.000 claims description 8
- 229910002027 silica gel Inorganic materials 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 7
- 102000004190 Enzymes Human genes 0.000 claims description 7
- 229940088598 enzyme Drugs 0.000 claims description 7
- 108010002430 hemicellulase Proteins 0.000 claims description 7
- 229940059442 hemicellulase Drugs 0.000 claims description 7
- 239000007858 starting material Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 35
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 18
- 238000000605 extraction Methods 0.000 description 16
- 235000019441 ethanol Nutrition 0.000 description 11
- -1 and eluant Substances 0.000 description 7
- 239000003480 eluent Substances 0.000 description 7
- 239000000284 extract Substances 0.000 description 7
- 229940013618 stevioside Drugs 0.000 description 6
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 241000723353 Chrysanthemum Species 0.000 description 4
- 235000007516 Chrysanthemum Nutrition 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 244000269722 Thea sinensis Species 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 229930002875 chlorophyll Natural products 0.000 description 2
- 235000019804 chlorophyll Nutrition 0.000 description 2
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 150000008131 glucosides Chemical class 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 2
- QSRAJVGDWKFOGU-WBXIDTKBSA-N rebaudioside c Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]1(CC[C@H]2[C@@]3(C)[C@@H]([C@](CCC3)(C)C(=O)O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)CC3)C(=C)C[C@]23C1 QSRAJVGDWKFOGU-WBXIDTKBSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229930182490 saponin Natural products 0.000 description 2
- 150000007949 saponins Chemical class 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 239000001512 FEMA 4601 Substances 0.000 description 1
- 239000001776 FEMA 4720 Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- HELXLJCILKEWJH-SEAGSNCFSA-N Rebaudioside A Natural products O=C(O[C@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@@]1(C)[C@@H]2[C@](C)([C@H]3[C@@]4(CC(=C)[C@@](O[C@H]5[C@H](O[C@H]6[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O6)[C@@H](O[C@H]6[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O6)[C@H](O)[C@@H](CO)O5)(C4)CC3)CC2)CCC1 HELXLJCILKEWJH-SEAGSNCFSA-N 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 229940023032 activated charcoal Drugs 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 239000006189 buccal tablet Substances 0.000 description 1
- 229940046011 buccal tablet Drugs 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001013 cariogenic effect Effects 0.000 description 1
- 229940112822 chewing gum Drugs 0.000 description 1
- 235000015218 chewing gum Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- HELXLJCILKEWJH-UHFFFAOYSA-N entered according to Sigma 01432 Natural products C1CC2C3(C)CCCC(C)(C(=O)OC4C(C(O)C(O)C(CO)O4)O)C3CCC2(C2)CC(=C)C21OC(C1OC2C(C(O)C(O)C(CO)O2)O)OC(CO)C(O)C1OC1OC(CO)C(O)C(O)C1O HELXLJCILKEWJH-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 235000019203 rebaudioside A Nutrition 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 210000004885 white matter Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
-
- 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
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)
- Seasonings (AREA)
Abstract
The present invention relates to the preparation method that high-purity STEVIA REBAUDIANA is extracted from STEVIA REBAUDIANA.The method of the present invention step is simple, both avoid traditional Steviosin extracting method and largely use water, the shortcomings that causing water resource to expend, it turn avoid and a large amount of organic solvents or inorganic salts are used in existing method, the shortcomings that increasing follow-up impurity removal process and big loss late, production cost is more reduced, excellent recovery rate is have also obtained while product purity is improved.Steviosin product purity made from the method for the present invention is more than 98.5%, and recovery rate is up to more than 13.95%.
Description
Technical field
The present invention relates to the preparation method of Steviosin, and high-purity sweetleaf is extracted from STEVIA REBAUDIANA more particularly, to one kind
The preparation method of chrysanthemum.
Background technology
Steviosin, also known as steviol glycoside, stevioside, are a kind of natural, high sugarinesses, low in calories, not cariogenic and safe and non-toxic
Sweetener, be widely used in the product of the forms such as food and drink, oral liquid, buccal tablet, chewing gum.Steviosin can be from chrysanthemum
Section's herbaceous plant STEVIA REBAUDIANA (SteviarebaudianaBertoni) extraction obtains.In the glucosides that STEVIA REBAUDIANA contains, content is high
And the glucosides body for having economic value has stevioside, Rebaudioside A, rebaudioside C etc., Steviosin is total for above-mentioned various sweet taste glycosides
Claim.The annual requirement of whole world Steviosin surpasses 10,000 tons, and its demand increases with annual 30% speed；China's year output
For 3000 tons, more than 80% exports to the countries such as Japan, South Korea, the U.S., far can not meet market development demand.Therefore, energetically
Carry out Study on extraction and the exploitation of Steviosin, the development to driving China's Steviosin industry, the drawing to China's national economy
It is dynamic, be of great practical significance.
Containing apolar substances such as a large amount of greases, chlorophyll and essential oil in STEVIA REBAUDIANA blade, while also contain substantial amounts of egg
The water-soluble substanceses such as white matter, organic acid, tannin, saponin(e, pigment, inorganic salts, the extraction of the presence of these materials to Steviosin
Make a big impact.Traditional Steviosin extracting method carries out soak extraction usually using a large amount of water, causes substantial amounts of water resource
Consumption, and due also to the interference of above-mentioned other compositions, can not obtain the higher Steviosin product of purity.In recent years, on sweet tea
The research of the preparation method of chrysanthemum element gradually increases, and a variety of improved methods are proposed from extraction, refined, removal of impurities, modification etc..
For example, CN107474086A disclose a kind of pressurized counter-flow water extraction, activated-charcoal column or resin column decoloration deodorize,
Preparing chromatograph in industry separation, plate-frame filtering, the method for spray drying prepare stevioside, and product purity is up to more than 90%.
CN107118243A discloses a kind of industrial production process of stevioside, including：Soaked with acetum iterative cycles
Bubble extraction stevia rebaudian leaf, obtains extracting solution, and upper adsorption column, is eluted with 0.5-1.0% sodium hydroxides after filtering, and is parsed with ethanol, is obtained
Desorbed solution, is made into sugar juice with water and decolourizes through decolorizing resin after recycling ethanol, is spray-dried, obtains stevia rebaudianum sugar product, total glycosides content
Up to more than 88.9%, wherein RA components more than 52.7%.
The method that CN106146574A discloses steviol glycoside in a kind of microwave-ULTRASONIC COMPLEX stevioside leaf, including：By sweet tea
Ye Juye, which rinses to be placed in absolute ethyl alcohol, to be soaked, and drying process obtains stevioside leaf powder, adds water and complex enzyme is uniformly mixed
Microwave heats afterwards, ultrasonic to obtain extracting solution and filter residue, is centrifuged after filter residue is stirred evenly with ether, by supernatant liquor and extraction
Liquid merges to obtain total extracting solution, liquor ferri trichloridi, calcium hydroxide solution, polyacrylamide solution and total extracting solution is mixed equal
It is even to obtain mixed liquor, supercritical extract after being mixed with aluminum sulfate solution, extract through macroporous resin adsorption, vacuum distillation, concentration,
Dry steviol glycoside crude product, attapulgite is added after being dissolved in water, is refined centrifugal concentrating drying, steviol glycoside is made, purity can
Up to more than 94.1%.
These above-mentioned methods have more significant advantage compared with traditional extraction process, but or because of poor selectivity loss late
Reach, or because of cost problem, or because continuous operation property is poor, or the restriction because of many factors such as loss late is excessive, in industrial metaplasia
There is certain obstacle in production.Therefore, for preparing drawbacks described above and deficiency existing for the method for Steviosin in the prior art, the present invention
Purpose provide that a kind of technique is simple, production efficiency is high, Steviosin preparation method easy to operate.
The content of the invention
The present invention provides a kind of preparation method that Steviosin is extracted from STEVIA REBAUDIANA, comprise the following steps：
（1）Take STEVIA REBAUDIANA blade to be placed in extractor, add the water of 1-3 times of raw material weight, add the biology enzyme of 1.0-3.0% with
And the steviol glycoside of raw material weight 0.1-0.5%, 0.5-2h is extracted under room temperature, is filtered, is obtained extracting solution；
（2）The calcium carbonate powder with Stevia rebaudiana starting material equivalent, stirring are added in extracting solution, centrifugation is stood, and filtering, must be handled
Liquid；
（3）Treatment fluid in step (2) is separated by Simulated Moving Bed Chromatography, obtains Steviosin component；
（4）Steviosin component in step (3) is concentrated to, centrifuged, is dried to obtain the Steviosin product of the present invention.
Wherein, step（1）In biology enzyme be preferably the pectase and/or hemicellulase of 1.0-3.0%, more preferably fruit
Glue enzyme and hemicellulase 1:1 mixture.
Wherein, step（4）In, the adsorbent of Simulated Moving Bed Chromatography filling is silica gel, and eluant, eluent is 15% ethanol solution；
Adsorption zone flow velocity 1-2BV/h；Elution zone flow velocity 1-3BV/h；Switching time is 500-800s；Temperature control is at 20 DEG C -30 DEG C；Pressure
Power is controlled in 0.15MPa-0.45MPa；
Steviosin product purity made from the method for the present invention is more than 98.5%, and recovery rate is up to more than 13.95%.
The method of the present invention step is simple, has both avoided traditional Steviosin extracting method and has largely used water, has caused water resource to expend
The shortcomings that, it turn avoid and a large amount of organic solvents or inorganic salts are used in existing method, increase follow-up impurity removal process and loss late
The shortcomings that big, more reduce production cost, and excellent recovery rate is have also obtained while product purity is improved.
It is nonpolar containing a large amount of greases, chlorophyll and essential oil etc. in STEVIA REBAUDIANA blade as pointed by background technology
Material, while also containing the water-soluble substanceses such as substantial amounts of protein, organic acid, tannin, saponin(e, pigment, inorganic salts, these materials
Extraction of the presence to Steviosin make a big impact.Extraction of the prior art for Steviosin, purifying, it is refined carried out it is wide
General research, there is provided the extraction scheme such as enzymolysis, ultrasonic extraction, microwave abstracting, ultra high pressure extraction, supercritical extract, it was also proposed that
Flocculation, macroreticular resin separation, UF membrane, recrystallization etc. purify process for purification.Present inventor is on the basis of the prior art
Upper carry out a large number of experiments, during the experiment discovery add a small amount of steviol glycoside in extraction, can be greatly enhanced recovery rate, and adopt
Unexpected effect is obtained with the impurity-removing method of calcium carbonate.Experimental result provided below is used for the preparation side for showing the present invention
The significant beneficial effect of method.Wherein, the assay method of Steviosin purity and recovery rate is side well known in the art in product
Method.
Experiment material：STEVIA REBAUDIANA, 15% ethanol, pectase, hemicellulase, calcium carbonate, ether, aluminum sulfate, tri-chlorination
Iron, calcium hydroxide, polyacrylamide, 65% ethanol
The method of the present invention：According to the method for embodiment 1, raw material takes 100g STEVIA REBAUDIANAs.
Contrast method 1：The method of the embodiment 1 of CN106146574A, raw material take 100g STEVIA REBAUDIANAs.
Contrast method 2：The method of the embodiment 1 of CN107474086 A, raw material take 100g STEVIA REBAUDIANAs.
Contrast method 3：100g STEVIA REBAUDIANA blades are taken, are placed in extractor, add the water of 2 times of raw material weight, add 2.0 weights
Measure the pectase of % and the mixture of hemicellulase（1:1）And 0.2 weight % steviol glycoside, extract 1h under room temperature, filter,
Obtain extracting solution；Extracting solution crosses the removal of impurities of level-one film, is concentrated after secondary membrane, obtains treatment fluid；Treatment fluid is passed through into Simulation moving bed color
Spectrum separation, the adsorbent of Simulated Moving Bed Chromatography filling is silica gel, and eluant, eluent is 15% ethanol solution, adsorption zone flow velocity 1BV/h,
Elution zone flow velocity 2BV/h, switching time 700s, at 30 DEG C, pressure is controlled in 0.3MPa temperature control, obtains Steviosin component,
Concentrate, centrifuge, being dried to obtain Steviosin product.
Contrast method 4：100g STEVIA REBAUDIANA blades are taken, are placed in extractor, add the water of 2 times of raw material weight, add 2.0 weights
Measure the pectase of % and the mixture of hemicellulase（1:1）, 1h is extracted under room temperature, is filtered, is obtained extracting solution；Add in extracting solution
Enter the calcium carbonate powder with Stevia rebaudiana starting material equivalent, stir, centrifugation is stood, and filtering, obtains treatment fluid；Treatment fluid is moved by simulating
Dynamic bed chromatographic isolation, the adsorbent of Simulated Moving Bed Chromatography filling are silica gel, and eluant, eluent is 15% ethanol solution, adsorption zone flow velocity
1BV/h, elution zone flow velocity 2BV/h, switching time 700s, at 30 DEG C, pressure is controlled in 0.3MPa temperature control, obtains Steviosin
Component, concentrates, centrifuges, being dried to obtain Steviosin product.
Contrast method 5：100g STEVIA REBAUDIANA blades are taken, are placed in extractor, the water of 2 times of raw material weight are added, using three-level
Continuous Countercurrent Extraction method, obtains extracting solution；The calcium carbonate powder with Stevia rebaudiana starting material equivalent is added in extracting solution, is stirred, centrifugation
Stand, filtering, obtains treatment fluid；Treatment fluid is separated by Simulated Moving Bed Chromatography, the adsorbent of Simulated Moving Bed Chromatography filling
For silica gel, eluant, eluent is 15% ethanol solution, and adsorption zone flow velocity 1BV/h, elution zone flow velocity 2BV/h, switching time 700s are warm
At 30 DEG C, pressure is controlled in 0.3MPa, obtains Steviosin component for degree control, concentrates, centrifuges, being dried to obtain the Steviosin production of the present invention
Product.
Experimental result see the table below.
It can be seen from the above that the method for the present invention obtains extremely prominent beneficial effect, product purity is high, and recovery rate is high.It is wherein right
The purification process of film process is employed according to method 3, obtains the effect close with the method for the present invention, still, membrane processing method is clear
It is complicated to wash journey, the whole production cycle extends and greatly increases production cost, be not as simple and practicable as the present processes, profit
In industrialized production.
Embodiment
The following specific embodiments are described below illustrates the present invention in more detail.
Embodiment 1
STEVIA REBAUDIANA blade is taken, is placed in extractor, adds the water of 2 times of raw material weight, adds the pectase and half fiber of 2.0 weight %
The mixture of the plain enzyme of dimension（1:1）And 0.2 weight % steviol glycoside, extract 1h under room temperature, filter, obtain extracting solution；In extracting solution
Middle addition and the calcium carbonate powder of Stevia rebaudiana starting material equivalent, stirring, centrifugation are stood, and filtering, obtains treatment fluid；Treatment fluid is passed through into mould
Intend mobile bed chromatic separation, the adsorbent of Simulated Moving Bed Chromatography filling is silica gel, and eluant, eluent is 15% ethanol solution, adsorption zone
Flow velocity 1BV/h, elution zone flow velocity 2BV/h, switching time 700s, at 30 DEG C, pressure is controlled in 0.3MPa temperature control, obtains sweet tea
Chrysanthemum element component, concentrates, centrifuges, being dried to obtain the Steviosin product of the present invention.The Steviosin product purity is up to 99.3%, recovery rate
Up to 14.01%.
Embodiment 2
STEVIA REBAUDIANA blade is taken, is placed in extractor, adds the water of 3 times of raw material weight, adds the pectase and 0.1 of 3.0 weight %
The steviol glycoside of weight %, extracts 1h under room temperature, filters, obtains extracting solution；The carbon with Stevia rebaudiana starting material equivalent is added in extracting solution
Sour calcium powder, stirring, centrifugation are stood, and filtering, obtains treatment fluid；Treatment fluid is separated by Simulated Moving Bed Chromatography, simulation movement
The adsorbent of bed chromatography filling is silica gel, and eluant, eluent is 15% ethanol solution, adsorption zone flow velocity 2BV/h, elution zone flow velocity 3BV/h,
Switching time is 700s, and for temperature control at 25 DEG C, pressure control obtains Steviosin component in 0.35MPa, concentration, centrifugation, dry
To the Steviosin product of the present invention.The Steviosin product purity is up to 98.8%, extraction rate reached 13.99%.
Embodiment 3
Take STEVIA REBAUDIANA blade, be placed in extractor, add 1 times of raw material weight water, add 2.5 weight % pectase and
The steviol glycoside of 0.35 weight %, extracts 2h under room temperature, filters, obtains extracting solution；Added and Stevia rebaudiana starting material equivalent in extracting solution
Calcium carbonate powder, stirring, centrifugation stand, filtering, obtain treatment fluid；Treatment fluid is separated by Simulated Moving Bed Chromatography, is simulated
The adsorbent of mobile bed chromatic filling is silica gel, and eluant, eluent is 15% ethanol solution, adsorption zone flow velocity 1BV/h, elution zone flow velocity
1BV/h, switching time 700s, at 30 DEG C, pressure is controlled in 0.3MPa temperature control, obtains Steviosin component, concentrate, centrifuge,
It is dried to obtain the Steviosin product of the present invention.The Steviosin product purity is up to 99.1%, extraction rate reached 14.02%.
Claims (4)
1. a kind of preparation method that Steviosin is extracted from STEVIA REBAUDIANA, comprises the following steps：
（1）Take STEVIA REBAUDIANA blade to be placed in extractor, add the water of 1-3 times of raw material weight, add the biology enzyme of 1.0-3.0% with
And the steviol glycoside of raw material weight 0.1-0.5%, 0.5-2h is extracted under room temperature, is filtered, is obtained extracting solution；
（2）The calcium carbonate powder with Stevia rebaudiana starting material equivalent, stirring are added in extracting solution, centrifugation is stood, and filtering, must be handled
Liquid；
（3）Treatment fluid in step (2) is separated by Simulated Moving Bed Chromatography, obtains Steviosin component；
（4）Steviosin component in step (3) is concentrated to, centrifuged, is dried to obtain the Steviosin product of the present invention.
2. preparation method as claimed in claim 1, step（1）In biology enzyme be preferably 1.0-3.0% pectase and/or
Hemicellulase, more preferably pectase and hemicellulase 1:1 mixture.
3. preparation method as claimed in claim 1, step（4）In, the adsorbent of Simulated Moving Bed Chromatography filling is silica gel, is washed
De- agent is 15% ethanol solution；Adsorption zone flow velocity 1-2BV/h；Elution zone flow velocity 1-3BV/h；Switching time is 500-800s；Temperature
Control is at 20 DEG C -30 DEG C；Pressure is controlled in 0.15MPa-0.45MPa.
4. preparation method as claimed in claim 1, obtained Steviosin product purity is more than 98.5%, and recovery rate is up to
More than 13.95%.
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