CN103450288B - A kind of isolation and purification method of trehalose - Google Patents
A kind of isolation and purification method of trehalose Download PDFInfo
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- CN103450288B CN103450288B CN201310360328.XA CN201310360328A CN103450288B CN 103450288 B CN103450288 B CN 103450288B CN 201310360328 A CN201310360328 A CN 201310360328A CN 103450288 B CN103450288 B CN 103450288B
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- trehalose
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- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 title claims abstract description 131
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 title claims abstract description 131
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002955 isolation Methods 0.000 title claims abstract description 13
- 238000000746 purification Methods 0.000 title claims abstract description 12
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 80
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 239000008103 glucose Substances 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 34
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000004088 simulation Methods 0.000 claims abstract description 18
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 17
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 15
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 15
- 102100029677 Trehalase Human genes 0.000 claims abstract description 14
- 108010087472 Trehalase Proteins 0.000 claims abstract description 14
- 239000000376 reactant Substances 0.000 claims abstract description 14
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 13
- 108010045348 trehalose synthase Proteins 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims description 32
- 229920005989 resin Polymers 0.000 claims description 32
- 239000003729 cation exchange resin Substances 0.000 claims description 25
- 239000003957 anion exchange resin Substances 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 108010089934 carbohydrase Proteins 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 11
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 10
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- 239000002253 acid Substances 0.000 claims description 10
- 229910001424 calcium ion Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 238000007639 printing Methods 0.000 claims description 7
- 230000001172 regenerating effect Effects 0.000 claims description 7
- 238000001223 reverse osmosis Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 230000008719 thickening Effects 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 abstract description 20
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 abstract description 20
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 108090000790 Enzymes Proteins 0.000 abstract description 4
- 102000004190 Enzymes Human genes 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 11
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- 238000005516 engineering process Methods 0.000 description 8
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- 241000219095 Vitis Species 0.000 description 5
- 235000009754 Vitis X bourquina Nutrition 0.000 description 5
- 235000012333 Vitis X labruscana Nutrition 0.000 description 5
- 235000014787 Vitis vinifera Nutrition 0.000 description 5
- 238000005349 anion exchange Methods 0.000 description 5
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- MSXHSNHNTORCAW-GGLLEASOSA-M sodium;(2s,3s,4s,5r,6s)-3,4,5,6-tetrahydroxyoxane-2-carboxylate Chemical compound [Na+].O[C@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O MSXHSNHNTORCAW-GGLLEASOSA-M 0.000 description 5
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- DSLZVSRJTYRBFB-LLEIAEIESA-N D-glucaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O DSLZVSRJTYRBFB-LLEIAEIESA-N 0.000 description 3
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 241000589776 Pseudomonas putida Species 0.000 description 3
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 3
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 description 3
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 235000014633 carbohydrates Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 229960004903 invert sugar Drugs 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
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- 239000000174 gluconic acid Substances 0.000 description 2
- 235000012208 gluconic acid Nutrition 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
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- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 2
- GMWTXQKKRDUVQG-WOPPDYDQSA-N 4-amino-5-bromo-1-[(2r,3s,4s,5r)-4-hydroxy-5-(hydroxymethyl)-3-methyloxolan-2-yl]pyrimidin-2-one Chemical compound C[C@H]1[C@H](O)[C@@H](CO)O[C@H]1N1C(=O)N=C(N)C(Br)=C1 GMWTXQKKRDUVQG-WOPPDYDQSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
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- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
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Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to a kind of isolation and purification method of trehalose, comprise the steps: (1) by the trehalase reactant liquor making with trehalose synthase conversion method through enzymolysis, filter, make the thick liquid of trehalose; (2) the thick liquid of trehalose, through activated carbon decolorizing, filters, and makes mixed liquor; (3) by mixed liquor process ion exchange resin, obtain glucose trehalose liquid glucose; (4) glucose trehalose liquid glucose is through concentrated, then carries out continuous chromatography separation by simulation moving-bed, makes aqueous trehalose and glucose solution. The present invention transforms the glycogenetic trehalase reactant liquor of Fructus Hordei Germinatus as raw material taking trehalose synthase, to be after isomeric maltose transforms with trehalose by enzyme process, again the impurity such as impurity glucose, remaining maltose and albumen, pigment, metal ion are removed, obtained the higher trehalose of purity.
Description
Technical field
The present invention relates to a kind of isolation and purification method of trehalose, particularly one is utilized resin dedicated and SMBCThe method that separates trehalose in the mixed sugar liquid of technology from biofermentation, belongs to sugared field of engineering technology.
Background technology
Trehalose is by α, α-1, the irreducibility disaccharide that 1 key is combined into by two glucose molecules. It is extensively present in carefullyIn bacterium, fungi, algae, rudimentary plant and insect. Find after deliberation, this sugar has unique biological function, has protection rawThe large molecule of thing, Cell protection film, the destruction that protected protein matter is avoided is freezing, dry and osmotic pressure variation etc. causes, food,Be used widely in the fields such as medicine, cosmetics, agricultural.
Constantly increase to the demand of trehalose in domestic and international market at present, and its production technology is also constantly being followed after progress. Early stage marine algaSugar product mainly by extracting from yeast cells, and productive rate is low, and cost is high, complex process, the application of restriction trehalose. In recent yearsCome to find trehalose synthase in many microorganisms, can a step transform maltose generation trehalose, this approach does not consume anakinetomer,Do not rely on phosphoric acid, and substrate maltose price is low, is convenient to obtain, have larger price space compared with trehalose. Therefore this wayFootpath is the approach that a utmost point has industrial prospect.
As Chinese patent literature CN101831474A(application number 201010137964.2) disclose one and utilized the false unit cell of stenchBacterium produces the method for trehalose, comprises pseudomonas putida incubation step, beta-mercaptoethanol treatment step and fermentation step. ShouldInvention, taking maltose as substrate, by the saturating sexual cell of preparation pseudomonas putida, utilizes its cell intracellular trehalose synthase by Fructus Hordei GerminatusSugar one step is converted into trehalose. After measured, in the saturating sexual cell solution of pseudomonas putida with beta-mercaptoethanol processing, approximately have 3%～5% trehalose generates.
At present, in the enzyme reaction solution that enzyme transforming process production trehalose obtains, except trehalose, also contain maltose, glucoseDeng carbohydrate, also have in addition the impurity such as albumen, pigment and metal ion. Therefore need just can obtain purity through serial purge processHigher trehalose.
Simulation moving-bed (SMB) chromatographic separation technology be a kind of new-modernization credit of growing up the sixties in 20th century fromTechnology is best suited for and carries out continuity large-scale industrial production in preparative chromatography technology. SMB technology range of application is also continuousExpand, in carbohydrate separates, application constantly obtains enterprise's attention. It is to utilize the difference of certain adsorbent to matrix absorption property,By Xi Fu ?the process of wash-out, make several separating substances that character is very close, and continuous chromatography isolation technics is taking chromatography as singleUnit, utilizes the mechanism such as adverse current, backflow, and the more general bed technology of separative efficiency is high, and in addition, continuous chromatography separation process can haveEffect utilize filler bed, improve the product of constant mass, be particularly suitable among carbohydrate produces.
But due to the complicated component of sugar in the reactant liquor in enzyme transforming process, therefore separation means of the prior art be not suitable for enzymeReactant liquor in conversion method.
Chinese patent CN103113425A(application number 201310016164.9) separating of a kind of trehalose and glucose disclosedMethod. The method utilizes nm of gold to make catalyst, and trehalose and glucose mixed liquor are substrate, in nano gold catalysis mixed liquorGlucose generates gluconic acid, then by chromatographic process, gluconic acid and trehalose is separated.
Because maltose and trehalose are isomerism, therefore technique scheme cannot separate maltose and trehalose, and onState complex process, separation costs costliness.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of isolation and purification method of trehalose is provided.
Technical scheme of the present invention is as follows:
An isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 80～100 DEG C, is incubated 10～30 pointsClock, cooling, then adds carbohydrase, and carbohydrase addition is 12～24U/ml, adjusts pH4.0～7.0, controls saccharification temperatureBe 60～65 DEG C, enzymolysis time 8～12h, is then warming up to 80～100 DEG C, is incubated 10～30 minutes, filters, and makes seaThe thick liquid of algae sugar;
(2) in the thick liquid of trehalose making to step (1), 0.5%～3% addition adds active carbon by weight percentage,Decolour 20～60 minutes, filter, make mixed liquor;
(3) mixed liquor step (2) being made, through ion exchange resin, is removed the metal ion in liquid glucose, obtains electricity and leadsThe glucose trehalose liquid glucose of rate < 50 μ s/cm;
(4) the glucose trehalose liquid glucose that step (3) makes is through being concentrated into liquid glucose mass body volume concentrations≤60%, the g/ml of unit,Then carry out continuous chromatography separation by simulation moving-bed, mobile phase is water, and separation resin is that calcium ion type aggressiveness ethene is gelType strong-acid cation-exchange resin, separation temperature is 35 DEG C～95 DEG C, system pressure≤1Mpa, feed liquid inlet amount is 5-3800mL/min, eluting water inlet amount is 0～3800mL/min, stepping time is 0.1s～99h, make concentration > 6wt%,The glucose solution of the aqueous trehalose of purity >=95wt% and concentration > 8wt%, purity >=91wt%.
Trehalase reactant liquor in described step (1) adopts this area routine techniques to make, as adopted Chinese patent literary compositionOffer CN101831474A(application number 201010137964.2) in the zymotic fluid prepared of method through high pressure cell cracker fragmentation,After filtration, make. In trehalase reactant liquor, sugared composition is maltose, glucose and trehalose.
Preferred according to the present invention, the ion exchange resin in described step (3) is that anion-exchange resin column and cation are handed overChange resin column and separate the metal ion in liquid glucose in the mode of series connection, liquid glucose is at 45～50 DEG C, and pH4.5～5.5 enter ion and hand overChange post, its flow control is 3～4 times of resin volume in the amount that flows through resin per hour, when the electrical conductivity of outlet liquid is greater thanThe pH that the pH value of 50 μ s/cm, cation exchange resin column outlet liquid returns to 4.0, anion-exchange resin column exports liquidWhen value is down to or anion-exchange resin column outlet liquid printing opacity is less than 98%, stop charging at 6～6.5 o'clock, carry out regenerative operation.
Further preferred according to the present invention, described cationic ion-exchange resin is strong acidic ion resin, as 001 × 7 cationResin; Anion exchange resin is strongly basic anionic resin, as 201 × 7 resin anion (R.A.)s.
Preferred according to the present invention, simmer down to vacuum rotating thin film evaporation is concentrated in described step (4), and thickening temperature is 60～110℃。
Preferred according to the present invention, in described step (4), carry out continuous chromatography separation by simulation moving-bed, condition is as follows:Input concentration 20～60%, charging rate is 3～25ml/min, separation temperature is 40～85 DEG C; Further preferred, instituteStating separation temperature is 50～75 DEG C.
Content of trehalose in gained aqueous trehalose is 95～97%; Content of trehalose in gained glucose solution is 4～9%,Concentration is 8～20%. After the simulation moving-bed separation of the present invention, the trehalose in invert sugar and glucose group are divided and are obtained effectivelySeparate, this step is also key of the present invention, not thorough if trehalose separates with glucose, will have a strong impact on after the present inventionThe effect of face, even cannot obtain highly purified crystalline trehalose product.
Preferred according to the present invention, also comprise that it is 65%～80% that the aqueous trehalose that step (4) is made is concentrated into mass concentration,Then 1:(0-4 by volume) add absolute ethyl alcohol, add in 5～40 DEG C of conditions of temperature the crystalline substance that mass percents are 0.1～3%Plant stirred crystallization, cross filtering filtrate, then the dry trehalose that makes.
Further preferred according to the present invention, above-mentioned aqueous trehalose is concentrated into mass concentration be 65%～80% concrete steps asUnder: it is 20～35% that aqueous trehalose is first concentrated into mass concentration through reverse osmosis membrane, and then through Vacuum Concentration to mass concentrationBe 65%～80%.
Further preferred according to the present invention, also comprise that the glucose solution that step (4) is made is after film is concentrated, with upperState filtrate (trehalose crystalline mother solution) mix after, for the production of gluconic acid sodium salt, the mother liquor after gluconic acid sodium salt Crystallization Separation withStep (1) makes after the thick liquid of trehalose mixes and recycles.
Beneficial effect
1, the present invention transforms Fructus Hordei Germinatus glycogenetic trehalase reactant liquor as raw material taking trehalose synthase, by enzyme process will with marine algaSugar is after isomeric maltose transforms, then to impurity glucose, remaining maltose and albumen, pigment, metal ion etc.Impurity is removed, and has obtained the higher trehalose of purity.
2, the present invention adopts moving bed continuous chromatography to separate, and adopts the separation resin of particular type to realize trehalose and glucoseBetween separation completely, resin utilization rate is high;
3, the present invention can realize production process full-automation, and labour intensity is low, and production site is little, and production cost is low, pointFrom every cubic metre of mixed sugar liquid, only need 1.8 cubic metres of-3 cubic metres of water and a small amount of electricity, in production process, do not need useizationProduct, environmental friendliness.
Brief description of the drawings
Fig. 1 is the structural representation of SMBC post;
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is further elaborated, but institute of the present invention protection domain is not limited to this.
Resin source
Calcium ion type aggressiveness ethene described in embodiment 1 is that gel-type strong-acid cation-exchange resin is purchased from FinexOy company;
Calcium ion type aggressiveness ethene described in embodiment 2 is that gel-type strong-acid cation-exchange resin is purchased from purolite company;
Calcium ion type aggressiveness ethene described in embodiment 3 is that gel-type strong-acid cation-exchange resin is purchased from Shandong Lu Kangli section medicineThing Chemical Co., Ltd.;
Described 001 × 7 resin cation is purchased from purolite company; 201 × 7 resin anion (R.A.)s are purchased from purolite company.
Trehalase reactant liquor in embodiment adopts Chinese patent literature CN101831474A(application number201010137964.2) zymotic fluid prepared by the method in makes after high pressure cell cracker fragmentation, filtration. Trehalase is anti-Answering sugared composition in liquid is maltose, glucose and trehalose.
Carbohydrase is purchased from letter (China) Bioisystech Co., Ltd of Novi.
Separation equipment
Simulation moving-bed five Disengagement zone that are made up of 20 rotary chromatographic columns that comprise, I district is 1～No. 3 Coupled columns groupBecome, II district is 4～No. 9 Coupled columns compositions, and III district is 10～No. 11 Coupled columns compositions, and IV district is 12～No. 19Coupled columns composition, V district is No. 20 chromatographic columns, No. 20 chromatographic column adopting reversal connection modes, the inlet in I district respectively withWater inlet storage tank is connected with recirculated water surge tank, and the liquid outlet in I district is connected by the inlet in glucose surge tank YuⅡ districtConnect, the liquid outlet in the liquid outlet HeⅢ district in II district expects that by centre the inlet in surge tank YuⅣ district is connected, the inlet in III districtBe connected with head tank, the liquid outlet in IV district is connected by the inlet in trehalose surge tank YuⅤ district, the liquid outlet in V district withRecirculated water surge tank is connected; No. 10 chromatographic column inlet place's continuous feeds, No. 3 and No. 19 chromatographic column liquid outlet places differenceCollect continuously glucose solution and aqueous trehalose.
In described 1～No. 20 chromatographic column, filling calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin.
Described 1～No. 19 chromatographic column rotation direction is to rotate by the clockwise direction at charging aperture visual angle, and No. 20 chromatographic columns are for pressing inThe counter clockwise direction at material mouthful visual angle is rotated.
Embodiment 1
An isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 100 DEG C, is incubated 10 minutes, cooling,Then add carbohydrase, carbohydrase addition is 24U/ml, adjusts pH4.5, and controlling saccharification temperature is 60 DEG C, enzymolysis time 8h,Then be warming up to 100 DEG C, be incubated 10 minutes, filter, make the thick liquid of trehalose;
(2) in the thick liquid of trehalose making to step (1), 3% addition adds active carbon by weight percentage, decolouring 20Minute, filter, make mixed liquor;
(3) mixed liquor step (2) being made is through ion exchange resin, and described ion exchange resin is anion exchange treeFat (201 × 7) post separates the metal ion in liquid glucose with cationic ion-exchange resin (001 × 7) post in the mode of series connection, and liquid glucose exists45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control the amount that flows through resin per hour be 3 of resin volume～4 times, the pH value that is greater than 50 μ s/cm, cation exchange resin column outlet liquid when the electrical conductivity of outlet liquid returns to 4.0,The pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than98% time, stop charging, carry out regenerative operation. Remove the metal ion in liquid glucose, obtain the grape of electrical conductivity < 50 μ s/cmSugar trehalose liquid glucose;
After testing, in glucose trehalose liquid glucose, total sugar concentration is 10wt%, and wherein content of trehalose accounts for the 59wt% of total sugar content,Glucose accounts for the 41wt% of total sugar content.
(4) the glucose trehalose liquid glucose that step (3) makes carries out continuous chromatography separation by simulation moving-bed, and mobile phase isWater, separation resin is that calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin.
Simulation moving-bed operating condition is as follows: 60 DEG C of separation temperatures, and system pressure≤0.5Mpa, feed liquid inlet amount is15.7mL/min, eluting water inlet amount is 25.5mL/min, stepping time 11min, charging reached balance after 2 hours.
After testing, the trehalose purity in gained aqueous trehalose is 99wt%, and average quality concentration is 43.2g/L; Gained grapeContent of trehalose in sugar juice is 5.4wt%.
It is 30% that the above-mentioned aqueous trehalose that makes is first concentrated into mass concentration through reverse osmosis membrane, and then through Vacuum Concentration to matterAmount concentration 80%, then 1:2 adds absolute ethyl alcohol by volume, and crystallization under 20 DEG C of conditions of temperature is crossed filtering filtrate, thenThe dry trehalose that makes; After testing, the purity of trehalose is 99.0%, the rate of recovery 42.1%;
Then glucose solution step (4) being made is after concentrated, after mixing with above-mentioned filtrate, for the production of glucoseAcid sodium, the mother liquor of gluconic acid sodium salt crystallization after separating makes the thick liquid of trehalose with step (1) and mixes rear recycling, grapeSodium saccharate crystallization drying obtains finished product.
Can be found out by the above results, after the simulation moving-bed separation of the present invention, the trehalose in invert sugar and glucose componentEffectively separated, this step obtains high-purity crystallized trehalose product and provides safeguard for follow-up simultaneously.
Embodiment 2
An isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 100 DEG C, is incubated 10 minutes, cooling,Then add carbohydrase, carbohydrase addition is 24U/ml, adjusts pH4.2, and controlling saccharification temperature is 63 DEG C, enzymolysis time 8h,Then be warming up to 100 DEG C, be incubated 10 minutes, filter, make the thick liquid of trehalose;
(2) in the thick liquid of trehalose making to step (1), 1% addition adds active carbon by weight percentage, decolouring 20Minute, filter, make mixed liquor;
(3) mixed liquor step (2) being made is through ion exchange resin, and described ion exchange resin is anion exchange treeFat (201 × 7) post separates the metal ion in liquid glucose with cationic ion-exchange resin (001 × 7) post in the mode of series connection, and liquid glucose exists45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control the amount that flows through resin per hour be 3 of resin volume～4 times, the pH value that is greater than 50 μ s/cm, cation exchange resin column outlet liquid when the electrical conductivity of outlet liquid returns to 4.0,The pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than98% time, stop charging, carry out regenerative operation. Remove the metal ion in liquid glucose, obtain the grape of electrical conductivity < 50 μ s/cmSugar trehalose liquid glucose;
After testing, in glucose trehalose liquid glucose, total sugar concentration is 30wt%, and wherein content of trehalose accounts for the 62wt% of total sugar content,Glucose accounts for the 38wt% of total sugar content.
(4) the glucose trehalose liquid glucose that step (3) makes is concentrated into liquid glucose mass body volume concentrations through vacuum rotating thin film evaporation35%, the g/ml of unit, thickening temperature is 110 DEG C, then carries out continuous chromatography separation by simulation moving-bed, mobile phase is water,Separation resin is that calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin.
Simulation moving-bed operating condition is as follows: 60 DEG C of separation temperatures, and system pressure≤1.0Mpa, feed liquid inlet amount is13.8mL/min, eluting water inlet amount is 29.9mL/min, stepping time 11min, charging reached balance after 2 hours.
After testing, the content of trehalose in gained aqueous trehalose is 97.6wt%, and average quality concentration is 58.1g/L; Gained PortugalContent of trehalose in grape sugar juice is 4wt%.
It is 35% that the above-mentioned aqueous trehalose that makes is first concentrated into mass concentration through reverse osmosis membrane, and then through Vacuum Concentration to matterAmount concentration 75%, then 1:3 adds absolute ethyl alcohol by volume, and crystallization under 30 DEG C of conditions of temperature is crossed filtering filtrate, thenThe dry trehalose that makes; After testing, the purity of trehalose is 99.0%, the rate of recovery 85.2%;
Then glucose solution step (4) being made is after concentrated, after mixing with above-mentioned filtrate, for the production of glucoseAcid sodium, the mother liquor of gluconic acid sodium salt crystallization after separating makes the thick liquid of trehalose with step (1) and mixes rear recycling, grapeSodium saccharate crystallization obtains finished product after drying.
Embodiment 3
An isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 100 DEG C, is incubated 10 minutes, cooling,Then add carbohydrase, carbohydrase addition is 24U/ml, adjusts pH4.5, and controlling saccharification temperature is 65 DEG C, enzymolysis time 8h,Then be warming up to 100 DEG C, be incubated 10 minutes, filter, make the thick liquid of trehalose;
(2) in the thick liquid of trehalose making to step (1), 3% addition adds active carbon by weight percentage, decolouring 20Minute, filter, make mixed liquor;
(3) mixed liquor step (2) being made is through ion exchange resin, and described ion exchange resin is anion exchange treeFat (201 × 7) post separates the metal ion in liquid glucose with cationic ion-exchange resin (001 × 7) post in the mode of series connection, and liquid glucose exists45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control the amount that flows through resin per hour be 3 of resin volume～4 times, the pH value that is greater than 50 μ s/cm, cation exchange resin column outlet liquid when the electrical conductivity of outlet liquid returns to 4.0,The pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than98% time, stop charging, carry out regenerative operation. Remove the metal ion in liquid glucose, obtain the grape of electrical conductivity < 50 μ s/cmSugar trehalose liquid glucose;
After testing, in glucose trehalose liquid glucose, total sugar concentration is 30wt%, and wherein content of trehalose accounts for the 63wt% of total sugar content,Glucose accounts for the 37wt% of total sugar content.
(4) the glucose trehalose liquid glucose that step (3) makes is concentrated into liquid glucose mass body volume concentrations through vacuum rotating thin film evaporation55wt%, the g/ml of unit, thickening temperature is 110 DEG C, then carries out continuous chromatography separation by simulation moving-bed, mobile phase isWater, separation resin is that calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin.
Simulation moving-bed operating condition is as follows: 60 DEG C of separation temperatures, and system pressure≤1.0Mpa, feed liquid inlet amount is11.6mL/min, eluting water inlet amount is 25.1mL/min, stepping time 11min, charging reached balance after 2 hours.
After testing, the content of trehalose in gained aqueous trehalose is 89wt%, and average quality concentration is 143g/L, gained grapeContent of trehalose in sugar juice is 9wt%.
It is 30～35% that the above-mentioned aqueous trehalose making is first concentrated into mass concentration through reverse osmosis membrane, and then through Vacuum ConcentrationTo mass concentration 70%, then 1:4 adds absolute ethyl alcohol by volume, and filtering filtrate is crossed in crystallization under 10 DEG C of conditions of temperature,Then the dry trehalose that makes; After testing, the purity of trehalose is 98.0%,, the rate of recovery 81.6%;
Then glucose solution step (4) being made is after concentrated, after mixing with above-mentioned filtrate, for the production of glucoseAcid sodium, the mother liquor of gluconic acid sodium salt crystallization after separating makes the thick liquid of trehalose with step (1) and mixes rear recycling, grapeSodium saccharate crystallization obtains finished product after drying.
Comparative example 1
An isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 100 DEG C, is incubated filtration in 10 minutes,Make the thick liquid of trehalose;
(2) in the thick liquid of trehalose making to step (1), 1% addition adds active carbon by weight percentage, decolouring 20Minute, filter, make mixed liquor;
(3) mixed liquor step (2) being made is through ion exchange resin, and described ion exchange resin is anion exchange treeFat (201 × 7) post separates the metal ion in liquid glucose with cationic ion-exchange resin (001 × 7) post in the mode of series connection, and liquid glucose exists45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control the amount that flows through resin per hour be 3 of resin volume～4 times, the pH value that is greater than 50 μ s/cm, cation exchange resin column outlet liquid when the electrical conductivity of outlet liquid returns to 4.0,The pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than98% time, stop charging, carry out regenerative operation. Remove the metal ion in liquid glucose, obtain the grape of electrical conductivity < 50 μ s/cmSugar trehalose liquid glucose;
After testing, in mixed sugar liquid, total sugar concentration is 35wt%, and wherein content of trehalose accounts for the 60wt% of total sugar content, maltoseAccount for the 38wt% of total sugar content.
(4) the glucose trehalose liquid glucose warp that step (3) makes is by simulation moving-bed continuous chromatography separation, the mobile phase of carrying outFor water, separation resin is that calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin.
Simulation moving-bed operating condition is as follows: 60 DEG C of separation temperatures, and system pressure≤1.0Mpa, feed liquid inlet amount is13.0mL/min, eluting water inlet amount is 28.6mL/min, stepping time 11min, charging reached balance after 2 hours.
After testing, the content of trehalose in gained aqueous trehalose is 82wt%, and average quality concentration is 63g/L; Gained Fructus Hordei GerminatusContent of trehalose in sugar juice is 43wt%.
It is 35% that the above-mentioned aqueous trehalose that makes is first concentrated into mass concentration through reverse osmosis membrane, and then through Vacuum Concentration to matterAmount concentration 70%～80%, then 1:3 adds absolute ethyl alcohol by volume, and filtering filtrate is crossed in crystallization under 30 DEG C of conditions of temperature,Then the dry trehalose that makes; After testing, the purity of trehalose is 82.5.0%, the rate of recovery 80.3%;
Then maltose solution step (4) being made is after concentrated, after mixing with above-mentioned filtrate, for following of conversion fluidRing utilizes.
Can be found out by the above results, after the simulation moving-bed separation of the present invention, the trehalose in invert sugar and maltose componentEffectively do not separated, again because maltose and trehalose are isomer, produced so cannot obtain high-purity crystallized trehaloseProduct.
Comparative example 2
An isolation and purification method for trehalose, comprises the steps:
(1) by the trehalase making with trehalose synthase conversion method, total sugar content 35%, reactant liquor is heated to 100 DEG C,Be incubated 10 minutes, cooling, obtains trehalose maltose mixed liquor.
(2) in the thick liquid of trehalose making to step (1), add 2% saccharomyces cerevisiae bacterial classification (CICC1202) to fermentCultivate, incubation time is 24h, centrifugal 5000rpm, and 10min, separated yeast, gets supernatant.
(3) by 1% the addition interpolation active carbon by weight percentage of supernatant in 2, decolour 20 minutes, filter, makeMixed liquor;
(4) mixed liquor step (2) being made is through ion exchange resin, and described ion exchange resin is anion exchange treeFat (201 × 7) post separates the metal ion in liquid glucose with cationic ion-exchange resin (001 × 7) post in the mode of series connection, and liquid glucose exists45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control the amount that flows through resin per hour be 3 of resin volume～4 times, the pH value that is greater than 50 μ s/cm, cation exchange resin column outlet liquid when the electrical conductivity of outlet liquid returns to 4.0,The pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than98% time, stop charging, carry out regenerative operation. Remove the metal ion in liquid glucose, obtain the grape of electrical conductivity < 50 μ s/cmSugar trehalose liquid glucose;
After testing, in maltose trehalose liquid glucose, total sugar concentration is 15.52wt%, and wherein content of trehalose accounts for total sugar content88.7wt%, maltose accounts for the 11.3wt% of total sugar content.
(5) step (4) make aqueous trehalose to be first concentrated into mass concentration through reverse osmosis membrane be 35%, and then through trueSky is concentrated into mass concentration 80%, and then 1:3 adds absolute ethyl alcohol by volume, and filtering is crossed in crystallization under 30 DEG C of conditions of temperatureFiltrate, the then dry trehalose that makes; After testing, the purity of trehalose is 89.0%, the rate of recovery 78%;
Can be found out by the above results, in everybody conventional trehalose separation method, utilize fermentation method to remove the wheat in conversion fluidBud sugar effect is undesirable, in fermentation by saccharomyces cerevisiae process, can not only consume maltose, consumes trehalose simultaneously, therefore reducesThe total amount of trehalose, increase production cost. In gained mixed sugar liquid, maltose content is still very high, is therefore unfavorable for obtaining heightPurity trehalose.
Claims (1)
1. an isolation and purification method for trehalose, comprises the steps:
(1) the trehalase reactant liquor making with trehalose synthase conversion method is heated to 80～100 DEG C, be incubated 10～30 minutes, cooling, then adds carbohydrase, carbohydrase addition is 12～24U/ml, adjust pH4.0～7.0, controlling saccharification temperature is 60～65 DEG C, enzymolysis time 8～12h, then be warming up to 80～100 DEG C, be incubated 10～30 minutes, filter, make the thick liquid of trehalose;
(2) in the thick liquid of trehalose making to step (1), 0.5%～3% addition adds active carbon by weight percentage, decolours 20～60 minutes, filters, and makes mixed liquor;
(3) mixed liquor step (2) being made, through ion exchange resin, is removed the metal ion in liquid glucose, obtains the glucose trehalose liquid glucose of electrical conductivity < 50 μ s/cm;
Described ion exchange resin is that anion-exchange resin column separates the metal ion in liquid glucose with cation exchange resin column in the mode of series connection, liquid glucose is at 45～50 DEG C, pH4.5～5.5 enter ion exchange column, its flow control is 3～4 times of resin volume in the amount that flows through resin per hour, when the electrical conductivity of outlet liquid is greater than 50 μ s/cm, the pH value of cation exchange resin column outlet liquid returns to 4.0, when the pH value of anion-exchange resin column outlet liquid is down to 6～6.5 o'clock or anion-exchange resin column outlet liquid printing opacity is less than 98%, stop charging, carry out regenerative operation,
Described cationic ion-exchange resin is strong acidic ion resin; Anion exchange resin is strongly basic anionic resin;
(4) the glucose trehalose liquid glucose that step (3) makes is concentrated into liquid glucose mass body volume concentrations≤60% through vacuum rotating thin film evaporation, the g/ml of unit, and thickening temperature is 60～110 DEG C; Then carry out continuous chromatography separation by simulation moving-bed, mobile phase is water, separation resin is that calcium ion type aggressiveness ethene is gel-type strong-acid cation-exchange resin, separation temperature is 50 DEG C～75 DEG C, system pressure≤1Mpa, feed liquid inlet amount is 3～25mL/min, eluting water inlet amount is 0～3800mL/min, stepping time is 0.1s～99h, makes the aqueous trehalose of concentration > 6wt%, purity >=95wt% and the glucose solution of concentration > 8wt%, purity >=91wt%; It is 20～35% that aqueous trehalose is first concentrated into mass concentration through reverse osmosis membrane, and then be 65%～80% through Vacuum Concentration to mass concentration, then 1:(0～4 by volume) add absolute ethyl alcohol, add in 5～40 DEG C of conditions of temperature the crystal seed stirred crystallization that mass percent is 0.1～3%, cross filtering filtrate, then the dry trehalose that makes;
Describedly carry out continuous chromatography separation by simulation moving-bed, condition is as follows: input concentration 20～60%.
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| CN103980327B (en) * | 2014-05-07 | 2016-09-14 | 国家海洋局第三海洋研究所 | A kind of high-purity trehalose preparation method that can be used for pharmaceutical injection agent |
| CN103981293B (en) * | 2014-05-19 | 2016-01-13 | 山东省鲁洲食品集团有限公司 | A kind of method preventing malt syrup from producing and deposit pH value decline in process |
| CN104017027B (en) * | 2014-06-12 | 2017-05-24 | 大庆柯迈特色谱分离技术开发有限公司 | Method for purifying trehalose and glucose by SSMB (sequential simulated moving bed) chromatography |
| CN105349599A (en) * | 2014-08-22 | 2016-02-24 | 义守大学 | Trehalose production method |
| CN104262413B (en) * | 2014-09-19 | 2017-03-22 | 保龄宝生物股份有限公司 | Preparation method of trehalose anhydrous |
| CN104478949B (en) * | 2014-11-24 | 2018-10-30 | 华东理工大学 | A kind of chromatography separating method of trehalose and maltose |
| CN106381347A (en) * | 2016-11-22 | 2017-02-08 | 保龄宝生物股份有限公司 | Crystallization technical method for industrially producing trehalose |
| CN107488689B (en) * | 2017-10-10 | 2021-04-27 | 溧阳维信生物科技有限公司 | Method for preparing alpha, alpha-trehalose dihydrate by adopting electrodialysis technology |
| CN108774273B (en) * | 2018-08-24 | 2021-06-25 | 湖南汇升生物科技有限公司 | Trehalose crystallization process |
| CN108866125A (en) * | 2018-08-24 | 2018-11-23 | 湖南汇升生物科技有限公司 | A method of reducing trehalose turbidity |
| CN109265495B (en) * | 2018-11-22 | 2021-10-22 | 湖南汇升生物科技有限公司 | One-step crystallization process for producing crystallized trehalose |
| CN110818753B (en) * | 2019-11-12 | 2021-05-28 | 湖南汇升生物科技有限公司 | Method for recycling crystallized trehalose mother liquor |
| CN111909224B (en) * | 2020-08-14 | 2023-07-28 | 江苏省奥谷生物科技有限公司 | Method for separating and purifying trehalose from mixture containing trehalose and maltose |
| CN112044478A (en) * | 2020-09-02 | 2020-12-08 | 广东力恩普健康产业科技有限公司 | Method for removing harmful metal ions in pineapple peel juice |
| CN113913483B (en) * | 2021-11-23 | 2023-06-23 | 常州大学 | Method for co-production of trehalose and gluconic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0619951A2 (en) * | 1993-03-16 | 1994-10-19 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Energy-supplementing saccharide source and its uses |
| CN1807465A (en) * | 2006-01-11 | 2006-07-26 | 胡耀辉 | Mycose separation and purification method |
| CN101831474A (en) * | 2010-04-02 | 2010-09-15 | 山东轻工业学院 | Production method of trehalose |
| CN103113425A (en) * | 2013-01-16 | 2013-05-22 | 南京工业大学 | Method for separating mycose from glucose |
-
2013
- 2013-08-16 CN CN201310360328.XA patent/CN103450288B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0619951A2 (en) * | 1993-03-16 | 1994-10-19 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Energy-supplementing saccharide source and its uses |
| CN1807465A (en) * | 2006-01-11 | 2006-07-26 | 胡耀辉 | Mycose separation and purification method |
| CN101831474A (en) * | 2010-04-02 | 2010-09-15 | 山东轻工业学院 | Production method of trehalose |
| CN103113425A (en) * | 2013-01-16 | 2013-05-22 | 南京工业大学 | Method for separating mycose from glucose |
Non-Patent Citations (1)
| Title |
|---|
| "模拟移动床色谱分离海藻糖和葡萄糖";杨亚威，等;《食品工业科技》;20130424;第34卷(第14期);第251-253，258页 * |
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