CN103936878B - A kind of method of sequential simulated mobile chromatograph (SSMB) purification oligomeric isomaltose - Google Patents
A kind of method of sequential simulated mobile chromatograph (SSMB) purification oligomeric isomaltose Download PDFInfo
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- AYRXSINWFIIFAE-SCLMCMATSA-N Isomaltose Natural products OC[C@H]1O[C@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)[C@@H](O)[C@@H](O)[C@@H]1O AYRXSINWFIIFAE-SCLMCMATSA-N 0.000 title claims abstract description 73
- DLRVVLDZNNYCBX-RTPHMHGBSA-N isomaltose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)C(O)O1 DLRVVLDZNNYCBX-RTPHMHGBSA-N 0.000 title claims abstract description 73
- 238000000746 purification Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000006188 syrup Substances 0.000 claims abstract description 29
- 235000020357 syrup Nutrition 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- 150000001768 cations Chemical class 0.000 claims abstract description 4
- 238000001228 spectrum Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 235000008504 concentrate Nutrition 0.000 claims description 14
- 239000012141 concentrate Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 12
- 238000004088 simulation Methods 0.000 claims description 9
- 238000010612 desalination reaction Methods 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 6
- 238000005352 clarification Methods 0.000 claims description 6
- 230000001839 systemic circulation Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 3
- 241000209140 Triticum Species 0.000 claims description 2
- 235000021307 Triticum Nutrition 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000011112 process operation Methods 0.000 abstract description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group 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 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 12
- 238000004587 chromatography analysis Methods 0.000 description 10
- 235000000346 sugar Nutrition 0.000 description 8
- 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 description 6
- 230000008859 change Effects 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 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 description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 241000186016 Bifidobacterium bifidum Species 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- ZCLAHGAZPPEVDX-UHFFFAOYSA-N D-panose Natural products OC1C(O)C(O)C(OC(C(O)CO)C(O)C(O)C=O)OC1COC1C(O)C(O)C(O)C(CO)O1 ZCLAHGAZPPEVDX-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 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 description 2
- 239000002253 acid Substances 0.000 description 2
- 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 description 2
- 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 2
- 238000011097 chromatography purification Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- DBTMGCOVALSLOR-AXAHEAMVSA-N galactotriose Natural products OC[C@@H]1O[C@@H](O[C@@H]2[C@@H](O)[C@H](CO)O[C@@H](O[C@H]3[C@@H](O)[C@H](O)O[C@@H](CO)[C@@H]3O)[C@@H]2O)[C@H](O)[C@H](O)[C@H]1O DBTMGCOVALSLOR-AXAHEAMVSA-N 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- FBJQEBRMDXPWNX-FYHZSNTMSA-N isomaltotriose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](OC[C@@H]2[C@H]([C@H](O)[C@@H](O)C(O)O2)O)O1 FBJQEBRMDXPWNX-FYHZSNTMSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229920001542 oligosaccharide Polymers 0.000 description 2
- 150000002482 oligosaccharides Chemical class 0.000 description 2
- ZCLAHGAZPPEVDX-MQHGYYCBSA-N panose Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@@H](O[C@H]([C@H](O)CO)[C@H](O)[C@@H](O)C=O)O[C@@H]1CO[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 ZCLAHGAZPPEVDX-MQHGYYCBSA-N 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 150000004043 trisaccharides Chemical class 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- -1 dextrinose Chemical class 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 239000003102 growth factor Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 125000003153 isomaltose group Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
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- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 229940100445 wheat starch Drugs 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
Abstract
A kind of method of sequential simulated mobile spectrum purification oligomeric isomaltose, with pretreated oligomeric isomaltose syrup as raw material, use sequential simulated mobile chromatographic equipment purification oligomeric isomaltose, employing deionized water is eluant, operating temperature is 50 70 DEG C, use sodium form highly acidic cation gel resin as work resin, obtain highly purified oligomeric isomaltose syrup and realize higher yields.Whole process operation low cost, energy consumption reduces, and automaticity is high, it is possible to continuous prodution, improving production efficiency.
Description
Technical field
The invention belongs to field of food industry, be specifically related to sequential simulated mobile chromatographic separation and purification technology, especially
Relate to the technology of a kind of sequential simulated mobile chromatogram purification oligomeric isomaltose.
Background technology
Oligomeric isomaltose is the oligosaccharide that 2-8 glucose molecule couples together with α-1,6 glycosidic bond.Under normal circumstances,
Oligomeric isomaltose is not fermented by yeast, can be effectively promoted the growth and breeding of beneficial bacteria one bacillus bifidus in human body, therefore
Being also called " positive growth factor for bifidus ", bacillus bifidus has many health cares, and as bacillus bifidus promotive factor
Oligomeric isomaltose the most just receives the concern of people.Oligomeric isomaltose has excellent processing characteristics simultaneously, various
Food is applied production technology without particular/special requirement, in that context it may be convenient to add in food, thus in food and health product
To being widely applied.Owing to oligomeric isomaltose has above-mentioned superperformance, therefore it is widely used.Oligomeric different wheat
The purity of bud sugar is the highest, and health care is the best, and value of the product is the biggest.But in the production of oligomeric isomaltose inevitably
The miscellaneous sugar such as maltose, glucose, the existence of these miscellaneous sugar can be mixed with, reduce the physiology of functional oligose to a great extent
Function.
Chinese invention patent 200610105282.7 discloses a kind of work utilizing distillers yeast to produce high-purity oligomeric isomaltose
Process, this invention applies hydrolysis and the Fermentation that distillers yeast contains multiple enzyme preparation, utilizes its hydrolysis can be by
Macromole sugar in low-purity oligomeric isomaltose hydrolyzes further, makes its saccharifying, transglucosidase preparation consumption relatively reduce；Simultaneously
Utilize its Fermentation glucose, maltose etc. to be fermented, and then improve the branched sugars such as dextrinose, panose and Isomaltotriose
Content produce highly purified oligomeric isomaltose；The open a kind of high-purity of Chinese invention patent 201010136714.7 is low
IMO and alcohol co-production preparation method, this invention makes more than 95% high-purity glucose with compounded saccharifying enzyme, through saccharifying
Enzymatic conversion, then ferment with active dry yeast, (dextrinose+panose+Isomaltotriose contains to prepare ultra-high purity oligomeric isomaltose
Amount >=70%, total oligomeric isomaltose content >=90%, coproduction simultaneously 18% ethanol (response rate >=90%).As seen from the above, existing
Technology is had to be mainly concentrated in preparing oligomeric isomaltose, current China achievement in research in terms of the purification of oligomeric isomaltose
The most fewer.Therefore, the isolated and purified of oligomeric isomaltose has become the difficult problem that manufacturer's letter is to be solved.
The mobile chromatograph of simulation (SMB) is a kind of advanced efficient isolation technics, to modern functions sugar, functional sugar alcohol and in
The development of medical herbs has important function.The most state-of-the-art simulated moving bed chromatography is sequential type simulated moving bed chromatography at present
(SSMB).Many that SSMB is more advanced than traditional SMB, is characterized in that detached dowel quantity reduces, subtracts than traditional chromatographic isolation equipment
Few operating cost 30%-50%, solvent load reduces 20%-40%.On the basis of guarantee is highly purified, there is high separability, height time
The performances such as yield, high efficiency, low cost, high stability.SMB is merely able to carry out the separation of binary composition, and SSMB technology is effective
Solve this problem.
Chinese patent 200720141139.3 discloses a kind of sequential type simulation moving bed chromatogram device；Chinese patent
200920274899.0 disclose a kind of sequential type simulated moving bed chromatography purification device.Chinese patent 201210016932.6 is public
A kind of method having opened preparing high-purity isomaltooligosacharifrom from wheat starch, discloses sequential simulated moving bed in its description
The method of separating oligomeric dextrinose, it uses highly acid large aperture resin, and feed flow rate is 1.5-2.5L/h, feeds dense
Degree 58-60%, feeding temperature is 55-75 DEG C, switching time 10-30min, collect oligomeric isomaltose concentration be the stream of 24-30%
Go out liquid, prepare oligomeric isomaltose concentrated solution, simultaneously.This patent uses feed flow rate, controls the balance of material switching time,
It cannot be guaranteed that accuracy；Resin uses highly acid macroporous resin, and the bigger separating effect of particle diameter is poor；Oligomeric isomaltose goes out
The concentration of material mouth only has 24-30%, and concentration is relatively low；The most do not provide purity and the yield of product；Input concentration only has 58-
60%, collect and obtain the glucose effluent that concentration of glucose is but 50-90% and the polysaccharide effluent containing polysaccharide component, and not
Add concentration technology.As seen from the above, the patent in terms of the existing sequential type simulated moving bed chromatography of current China is mainly concentrated
At the research and development manufacture view of device, the application in terms of oligomeric isomaltose purification is not the most ripe.
In this context, inventor have studied the technology of sequential simulated mobile chromatograph efficiently purifying oligomeric isomaltose.
Summary of the invention
Present invention aim to address oligomeric isomaltose cannot the difficult problem of efficiently purifying, have studied one and utilize sequential
The method of the mobile chromatogram purification oligomeric isomaltose of simulation.
A kind of method of sequential simulated movement (SSMB) chromatogram purification oligomeric isomaltose: with after desalination, decolouring
Oligomeric isomaltose crude product syrup is raw material, uses sequential simulated mobile chromatographic technique purification oligomeric isomaltose, obtains height
The oligomeric isomaltose syrup of purity.
In the present invention, oligomeric isomaltose refers to the oligosaccharide composition of more than trisaccharide and trisaccharide, and miscellaneous sugar refers to disaccharide
And monosaccharide components.Wherein, in the sequential simulated continuous adsorption and purification of mobile chromatograph, adsorbent is the exchange of Na+ highly acidic cation
Type gel resin UBK530 Na+、UBK550 Na+、99 Na+-310 or 99 Na+Any one in-320；Eluant is water,
Sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, has charging aperture 2, discharging opening 2, and cleansing temp is 60-70
℃。
Its processing step is:
A) allotment of feed syrup: the oligomeric isomaltose syrup after desalination, decolouring is formulated to concentration is 50-60%；
B) filtering: by step A) the syrup solution micron-rated filter that obtains filters, and prepare clarification can without naked eyes
The liquid seen；
C) sequential simulated mobile chromatogram purification: syrup obtained above is pure through sequential simulated mobile chromatographic equipment
Change.It is 6 root chromatogram columns that chromatographic equipment is moved in the simulation that the present invention uses, and No. 1 post position is divided into following three steps.
The a first step: enter material simultaneously, enter eluant, discharging.Post 1 enters eluant D (deionized water), and post brings out component 1 time
The miscellaneous sugar of A()；Post 4 enters AB (raw material), and post brings out the component B(oligomeric isomaltose of part for 5 times).Entering the eluant water yield is single-column color
The 3%～10% of spectrum column volume, inlet amount is the 2%～10% of single column chromatographic column volume；
B second step: material can not enter, carries out systemic circulation, and liquid stream direction is for be flowed by post 1 to post 6, and circulating load is single-column
The 30%～70% of chromatographic column volume；
C the 3rd step: this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant D (deionized water), post 5
Under bring out another part component B(oligomeric isomaltose), enter that the eluant water yield is single column chromatographic column volume 0.5%～10%；
Above three steps it are sequentially repeated after No. 1 post end of run, except for the difference that, in this first step and the 3rd step, enter,
Unloading position is moved to next post, the most like this procedure operation by post 1 to post 6 direction.
D), concentrate: by a) step prepare component solution A concentrate, component solution A is concentrated into 70%～75%, by a),
C) component B that step prepares mixes, then concentrates, and component B solution is concentrated into 70%～75%.
The present invention uses sequential simulated mobile chromatogram purification oligomeric isomaltose, the oligomeric isomaltose group that purification obtains
Point concentration is 20%～35%, purity 85%～95%, yield 85～90%.
Present invention have the advantage that described process operation low cost, product purity (85%～95%) that purification obtains, dense
Degree (20%～35%) and yield (85～90%) are the highest.This technique reduces subsequent concentration cost, simplifies operating procedure, fall
Low produce loss；And can continuous prodution, improve production efficiency.At present, sequential simulated mobile chromatographically pure is used
The research changing oligomeric isomaltose is little, and Chinese patent 201210016932.6 discloses a kind of sequential simulated moving bed separation
The method of oligomeric isomaltose, but the purity of oligomeric isomaltose that this method obtains only has 80%, and yield is relatively low.
Accompanying drawing explanation
Fig. 1 is the production method FB(flow block) of the present invention.
Fig. 2 is the schematic diagram of the first step in the sequential simulated mobile chromatogram purification of the present invention.
Fig. 3 is the schematic diagram of second step in the sequential simulated mobile chromatogram purification of the present invention.
Fig. 4 is the schematic diagram of the 3rd step in the sequential simulated mobile chromatogram purification of the present invention.
Fig. 5 is the liquid-phase chromatographic analysis collection of illustrative plates of oligomeric isomaltose raw material.
Fig. 6 is embodiment 1 oligomeric isomaltose liquid-phase chromatographic analysis collection of illustrative plates after purification.
Detailed description of the invention
Embodiment 1
The method of the sequential simulated mobile chromatogram purification oligomeric isomaltose of the present invention, test uses sequential simulated shifting
Dynamic chromatographic equipment is purified, and the sequential simulated mobile chromatographic equipment that the present invention uses is by 6 root chromatogram columns (diameter 35mm, length
Degree 1000mm) composition, every root chromatogram column 1L, 6L, controls input and output material by electromagnetic valve altogether.It is achieved by the steps of:
A) allotment of feed syrup: the oligomeric isomaltose syrup after desalination, decolouring is formulated to concentration is 60%；
B) filtering: by step A) the syrup solution micron-rated filter that obtains filters, and prepare clarification can without naked eyes
See the liquid of impurity；
C) sequential simulated mobile chromatogram purification: syrup obtained above is pure through sequential simulated mobile chromatographic equipment
Change.It is 6 root chromatogram columns that chromatographic equipment is moved in the simulation that the present invention uses, and No. 1 post position is divided into following three steps.
A) entering material simultaneously, enter eluant, discharging, this step is also known as all-in and all-out.Post 1 enters eluant D(deionized water),
Post brings out the miscellaneous saccharic composition of component A(for 1 time)；Post 4 enters raw material, and post brings out the component B(oligomeric isomaltose component of a part for 5 times).
Entering the eluant water yield is 94.5mL, and inlet amount is 77 mL of chromatographic column volume；
B) material can not enter, carries out systemic circulation, and liquid stream direction is for be flowed by post 1 to post 6, and circulating load is 550 mL；
C) this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant, and post brings out another part component 5 times
B(oligomeric isomaltose component), entering the eluant water yield is 14.8 mL；
Above three steps it are sequentially repeated after No. 1 post end of run, except for the difference that, in this first step and the 3rd step, enter,
Unloading position is moved to next post, the most like this procedure operation by post 1 to post 6 direction.
D) concentrate: the component solution A that step c prepares being concentrated, component solution A is concentrated into 70%～75%, by b), c)
Component B that step prepares mixes, then concentrates, and component B solution is concentrated into 70%～75%.
Wherein, in the sequential simulated continuous adsorption and purification of mobile chromatograph, adsorbent is resin UBK530 Na+；Eluant is
Water, sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, has charging aperture 2, discharging opening 2, and cleansing temp is 65
℃；
The present invention uses sequential simulated mobile chromatographic technique purification oligomeric isomaltose, the oligomeric different Fructus Hordei Germinatus that purification obtains
Saccharic composition concentration is 34.5%, oligomeric isomaltose purity 92.6%, yield 85.5%.
Embodiment 2
The method of the sequential simulated mobile chromatogram purification oligomeric isomaltose of the present invention, test uses sequential simulated shifting
Dynamic chromatographic equipment is purified, and the sequential simulated mobile chromatographic equipment that the present invention uses is by 6 root chromatogram columns (diameter 35mm, length
Degree 1000mm) composition, every root chromatogram column 1L, 6L, controls input and output material by electromagnetic valve altogether.It is achieved by the steps of:
A) allotment of feed syrup: the oligomeric isomaltose syrup after desalination, decolouring is formulated to concentration is 60%；
B) filtering: by step A) the syrup solution micron-rated filter that obtains filters, and prepare clarification can without naked eyes
See the liquid of impurity；
C) sequential simulated mobile chromatogram purification: syrup obtained above is pure through sequential simulated mobile chromatographic equipment
Change.It is 6 root chromatogram columns that chromatographic equipment is moved in the simulation that the present invention uses, and No. 1 post position is divided into following three steps.
A) entering material simultaneously, enter eluant, discharging, this step is also known as all-in and all-out.Post 1 enters eluant D(deionized water),
Post brings out the miscellaneous saccharic composition of component A(for 1 time)；Post 4 enters raw material, and post brings out the component B(oligomeric isomaltose component of a part for 5 times).
Entering the eluant water yield is 338.5mL, and inlet amount is 156.9 mL；
B) material can not enter, carries out systemic circulation, and liquid stream direction is for be flowed by post 1 to post 6, and circulating load is 546 mL；
C) this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant, and post brings out another part component 5 times
B(oligomeric isomaltose component), entering the eluant water yield is 5.3 mL；
Above three steps it are sequentially repeated after No. 1 post end of run, except for the difference that, in this first step and the 3rd step, enter,
Unloading position is moved to next post, the most like this procedure operation by post 1 to post 6 direction.
D) concentrate: the component solution A that step c prepares being concentrated, component solution A is concentrated into 70%～75%, b, c are walked
Rapid component B prepared mixes, then concentrates, and component B solution is concentrated into 70%～75%.
Wherein, in the sequential simulated continuous adsorption and purification of mobile chromatograph, adsorbent is resin 99 Na+-310；Eluant is
Water, sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, has charging aperture 2, discharging opening 2, and cleansing temp is 60
℃；
The present invention uses sequential simulated mobile chromatographic technique purification oligomeric isomaltose, the oligomeric different Fructus Hordei Germinatus that purification obtains
Saccharic composition concentration is 24%, oligomeric isomaltose purity 94.6%, yield 90.1%.
Embodiment 3
The method of the sequential simulated mobile chromatogram purification oligomeric isomaltose of the present invention, test uses sequential simulated shifting
Dynamic chromatographic equipment is purified, and the sequential simulated mobile chromatographic equipment that the present invention uses is by 6 root chromatogram columns (diameter 35mm, length
Degree 1000mm) composition, every root chromatogram column 1L, 6L, controls input and output material by electromagnetic valve altogether.It is achieved by the steps of:
A) allotment of feed syrup: the oligomeric isomaltose syrup after desalination, decolouring is formulated to concentration is 60%；
B) filter: syrup solution micron-rated filter step a) obtained filters, prepare clarification can without naked eyes
See the liquid of impurity；
C) sequential simulated mobile chromatogram purification: syrup obtained above is pure through sequential simulated mobile chromatographic equipment
Change.It is 6 root chromatogram columns that chromatographic equipment is moved in the simulation that the present invention uses, and No. 1 post position is divided into following three steps.
A) entering material simultaneously, enter eluant, discharging, this step is also known as all-in and all-out.Post 1 enters eluant D(deionized water),
Post brings out the miscellaneous saccharic composition of component A(for 1 time)；Post 4 enters raw material, and post brings out the component B(oligomeric isomaltose component of a part for 5 times).
Entering the eluant water yield is 569.3mL, and inlet amount is 286.8 mL；
B) material can not enter, carries out systemic circulation, and liquid stream direction is for be flowed by post 1 to post 6, and circulating load is 591.5 mL；
C) this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant, and post brings out another part component 5 times
B(oligomeric isomaltose component), entering the eluant water yield is 59.2 mL；
Above three steps it are sequentially repeated after No. 1 post end of run, except for the difference that, in this first step and the 3rd step, enter,
Unloading position is moved to next post, the most like this procedure operation by post 1 to post 6 direction.
D) concentrate: the component solution A that step c prepares being concentrated, component solution A is concentrated into 70%～75%, b, c are walked
Rapid component B prepared mixes, then concentrates, and component B solution is concentrated into 70%～75%.
Wherein, in the sequential simulated continuous adsorption and purification of mobile chromatograph, adsorbent is resin 99 Na+-320；Eluant is
Water, sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, has charging aperture 2, discharging opening 2, and cleansing temp is 65
℃；
The present invention uses sequential simulated mobile chromatographic technique purification oligomeric isomaltose, the oligomeric different Fructus Hordei Germinatus that purification obtains
Saccharic composition concentration is 20.5%, oligomeric isomaltose purity 86.4%, yield 85.1%.
Embodiment 4
The method of the sequential simulated mobile chromatogram purification oligomeric isomaltose of the present invention, test uses sequential simulated shifting
Dynamic chromatographic equipment is purified, and the sequential simulated mobile chromatographic equipment that the present invention uses is by 6 root chromatogram columns (diameter 35mm, length
Degree 1000mm) composition, every root chromatogram column 1L, 6L, controls input and output material by electromagnetic valve altogether.It is achieved by the steps of:
A) allotment of feed syrup: the oligomeric isomaltose crude product syrup after desalination, decolouring is formulated to concentration is
50%；
B) filtering: by step A) the syrup solution micron-rated filter that obtains filters, and prepare clarification can without naked eyes
See the liquid of impurity；
C) sequential simulated mobile chromatogram purification: syrup obtained above is pure through sequential simulated mobile chromatographic equipment
Change.It is 6 root chromatogram columns that chromatographic equipment is moved in the simulation that the present invention uses, and is divided into following three steps during No. 1 post position.
A) first step: entering material simultaneously, enter eluant, discharging, this step is also known as all-in and all-out.Post 1 enters eluant D(and goes
Ionized water), post brings out the miscellaneous saccharic composition of component A(for 1 time)；Post 4 enters raw material, and post brings out the oligomeric different Fructus Hordei Germinatus of component B(of a part for 5 times
Saccharic composition).Entering the eluant water yield is 539.3mL, and inlet amount is 251.3 mL of chromatographic column volume；
B) second step: material can not enter, carries out systemic circulation, liquid stream direction is for be flowed by post 1 to post 6, and circulating load is 637
mL；
C) the 3rd step: this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant, and post brings out another 5 times
Constituent part B(oligomeric isomaltose component), entering the eluant water yield is 11.5 mL；
Above three steps it are sequentially repeated after No. 1 post end of run, except for the difference that, in this first step and the 3rd step, enter,
Unloading position is moved to next post, the most like this procedure operation by post 1 to post 6 direction.
D) concentrate: by c) step prepare component solution A concentrate, component solution A is concentrated into 70%～75%, by b),
C) component B that step prepares mixes, then concentrates, and component B solution is concentrated into 70%～75%.
Wherein, in the sequential simulated continuous adsorption and purification of mobile chromatograph, adsorbent is resin UBK550 Na+；Eluant is
Water, sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, has charging aperture 2, discharging opening 2, and cleansing temp is 60
℃；
The present invention uses sequential simulated mobile chromatographic technique purification oligomeric isomaltose, the oligomeric different Fructus Hordei Germinatus that purification obtains
Saccharic composition concentration is 20%, oligomeric isomaltose purity 90.2%, yield 89.8%.
The core technology of the present invention is sequential simulated mobile chromatogram purification oligomeric isomaltose technology, obtains purity and receipts
The oligomeric isomaltose syrup that rate is the highest, this technique not only ensure that oligomeric isomaltose high-purity and high yield, also whole
The aspects such as the cost savings of individual technique, process are easy have the characteristic of distinctness.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people being familiar with this specialty
Member, in the range of without departing from technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or modification
For the Equivalent embodiments of equivalent variations, as long as being without departing from technical solution of the present invention content, according to the technical spirit of the present invention,
Within the spirit and principles in the present invention, any simple amendment, equivalent and the improvement etc. that above example is made, the most still
Within belonging to the protection domain of technical solution of the present invention.
Claims (1)
1. a method for sequential simulated mobile chromatogram purification oligomeric isomaltose, with oligomeric isomaltose crude product as raw material,
It is characterized in that including following step: A) allotment of feed syrup: by the oligomeric isomaltose syrup after desalination, decolouring
Being formulated to concentration is 60%；
B) filtering: by step A) the syrup solution micron-rated filter that obtains filters, and prepares being visible by naked eyes of clarification miscellaneous
The liquid of matter；
C) sequential simulated mobile chromatogram purification: by syrup obtained above through sequential simulated mobile chromatographic equipment purification, adopt
Simulation to move chromatographic equipment be 6 root chromatogram columns, No. 1 post position is divided into following three steps:
A) entering material simultaneously, enter eluant, discharging, this step is also known as all-in and all-out, and post 1 enters eluant deionized water, post 1 lower end
Impurity removal saccharic composition A；Post 4 enters raw material, and post brings out oligomeric isomaltose component B of a part for 5 times, and entering the eluant water yield is single-column color
The 3%～10% of spectrum column volume, inlet amount is the 2%～10% of single column chromatographic column volume；
B) material can not enter, carries out systemic circulation, and liquid stream direction is for be flowed by post 1 to post 6, and circulating load is single column chromatographic column volume
30%～50%；
C) this step is partial circulating, only enters eluant deionized water, and post 1 enters eluant, and post brings out the oligomeric different wheat of another part for 5 times
Bud saccharic composition B, enter that the eluant water yield is single column chromatographic column volume 0.5%～10%；
Be sequentially repeated above three steps after No. 1 post end of run, except for the difference that, this) and c) in, charging and discharging position is by post
1 to post 6 direction moves to next post, the most like this procedure operation；
D) concentrate: the component solution A that a) step prepares being concentrated, component solution A is concentrated into 70%～75%, by a), c) step
Rapid component B prepared mixes, then concentrates, and component B solution is concentrated into 70%～75%；
The oligomeric isomaltose concentration of component that after mixing, purification obtains is 20%～35%, purity is 85%～95%, yield be 85～
90%；
Wherein in three steps of step a)-c) in the purification of sequential simulated mobile chromatograph, adsorbent is Na+ highly acidic cation
Crossover gel resin；Eluant is deionized water, and sequential simulated mobile chromatographic equipment comprises 6 root chromatogram columns, described absorption
Agent Na+ highly acidic cation crossover gel resin is UBK530 Na+With UBK550 Na+In one.
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| CN114213477B (en) * | 2021-12-21 | 2023-08-15 | 黑龙江八一农垦大学 | Starch syrup decoloring method based on simulated mobile chromatography |
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