CN100354290C - Raffinoses oligosaccharide with stachyose as main materials and method for preparing same - Google Patents
Raffinoses oligosaccharide with stachyose as main materials and method for preparing same Download PDFInfo
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- CN100354290C CN100354290C CNB2005100710459A CN200510071045A CN100354290C CN 100354290 C CN100354290 C CN 100354290C CN B2005100710459 A CNB2005100710459 A CN B2005100710459A CN 200510071045 A CN200510071045 A CN 200510071045A CN 100354290 C CN100354290 C CN 100354290C
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Abstract
The present invention relates to raffinose oligosaccharide with stachyose as a main component and a production method thereof. Raw materials are plants such as rehmanniae, Chinese ortichoke, lycopus roots, etc.; total saccharide in the product accounts for more than 96%, wherein the content of stachyose is 62 to 71%; functional oligosaccharide with stachyose as a main component of raffinose accounts for 75 to 90% in the product and 79 to 92% in the total saccharide. The production technology mainly comprises: chitosan and active carbon cooperate to clarify and decolorize an extracting solution; 1 to 4 group anion and cation exchange resin cooperate for desalting; an extracting solution can be prepared into preparations such as oral liquid, solid powder, granules, etc.
Description
Invention field
The present invention relates to a kind of functional oligose and production method thereof, particularly based on the raffinose family oligose and the production method thereof of stachyose.
Background technology
The raffinose family oligose, what occurring in nature was often deposited three glycan raffinoses (semi-lactosi-glucose-fructose), four glycan stachyoses (semi-lactosi-semi-lactosi-glucose-fructose), five glycan verbascoses (semi-lactosi-semi-lactosi-semi-lactosi-glucose-fructose), oligose more than five glycan arranged, a small amount of derivative that forms in the course of processing in addition such as melibiose (semi-lactosi-glucose), mannotriose (semi-lactosi-semi-lactosi-glucose) etc., these sugar are functional oligose.The raffinose family oligose, the piece root that mainly is present in scrophulariaceae rehmannia glutinosa plant (Rehmannia glutinosa Libosch.), Labiatae betony Rhizome of Bear's-foot Fern (Stachys sieboldii Miq.) rhizome, in bamboo shoot (the Lycopus lucidus Turez) rhizome, and stachyose is its main oligose composition, therefore can be from the raffinose family oligose of extraction in the middle of these plants based on stachyose.
Stachyose is that the function of master's raffinose family oligose is studied report both at home and abroad a lot; it has the bifidus bacillus proliferation function; treatment and prevent flora imbalance due to the multiple reason, reduce enterogenous endotoxin, functions such as treatment diarrhoea, constipation, protection liver, treatment hepatogenic encephalopathy.
Because it is, therefore more to the research of its preparation production method based on the raffinose family oligose wide range of therapeutic health-care effect of stachyose.But present defecation method exists certain not enough: the alcohol deposition method loss of effective components is big, uneconomical; Simple by adjusting the PH clarification, effect is also bad; Mineral acid, mineral alkali, diatomite, acidic white earth fining process carry out to repeated multiple times sedimentation and filter, and make the production operation process numerous and diverse, time-consuming; Burow Solution and oxalic acid clarification, it is residual to have aluminium, and aluminium is the objectionable constituent that cause uremia, dementia.And report all decolouring steps that has at present, and adopt after the clarification filters more, and filtrate adds activated carbon decolorizing, filters again, promptly clarifies and decolouring is divided into two steps and carries out, and carries out twice filtration at least.And filtration difficulty, consuming time, there is gac residual sometimes, influence quality product.Prior art adopted that the anion-cation exchange resin post further decolours, desalination; But do not see the report that is used with many groups zwitterion resin column at present.
Summary of the invention
The object of the invention is to provide a kind of raffinose family oligose extract based on stachyose; Another object of the present invention is to provide a kind of raffinose family oligose method for preparing extractive based on stachyose.
Oligose extract provided by the invention, total reducing sugar accounts for more than 96%, and stachyose content 62-71% wherein is 75-90% based on the raffinose family oligose of stachyose, and the ratio that accounts for total reducing sugar is 79-92%.
The preparation method of said extracted thing can have three kinds:
1, the plant material that will contain the raffinose family oligose, extract with decocting, also can use alcohol or lower concentration ethanol-extracted, or squeezing is extracted, obtain extract (this extract contains the raffinose family oligose), simmer down to concentrates liquid glucose, be heated to 60-80 ℃, the density that concentrates liquid glucose adds powdered active carbon earlier in the 1.02-1.07 scope, the add-on of Powdered Activated Carbon is the 6-10% (w/w) of plant material weight, or the 1.5-2.5% of concentrated liquid glucose volume (w/v), stirring makes abundant absorption, and churning time is 15-25 minute, adds chitosan solution then, the chitosan solution add-on is for concentrating the 2-10% (v/v) of liquid glucose volume, stirring makes and is uniformly dispersed, and is layered as the active carbon layer of lurid supernatant liquor and black, filters supernatant liquor and obtains clarifying decolouring liquid glucose; Adopted according to prior art again that the anion-cation exchange resin post further decolours, desalination, promptly.
Said process also can add chitosan solution earlier, adds gac again, and clarifying effect is fine equally.
The consumption of gac is preferably 8% of plant material weight, or 2% (w/v) of concentrated liquid glucose volume, and the consumption of chitosan solution is preferably the 2-4% (v/v) that concentrates the liquid glucose volume, further preferred 3% (v/v).
Chitosan solution method: chitosan clarifier solution: the 0.5-1.5g chitosan adds the pH scope in the weakly acid soln 100ml of 2.5-3.5, and swelling 24 hours is standby.Preferably being mixed with 1% solution uses.
Also 2 kinds of above-mentioned plant materials or multiple merging can be extracted the raffinose family oligose simultaneously, then extracting solution be carried out decolouring-clarifying treatment of the application, or the extracting solution of 2 kinds or plurality of raw materials is merged, carry out decolouring-clarifying treatment of the application; The consumption of chitosan, powdered active carbon adopts the common consumption in conventional clarification, the decolorization to get final product.
The plant material that 2, will contain the raffinose family oligose, extract with decocting, also can use alcohol or lower concentration ethanol-extracted, or squeezing is extracted, obtain extract (this extract contains the raffinose family oligose), simmer down to concentrates liquid glucose, the density that concentrates liquid glucose is in the 1.02-1.07 scope, after conventional decolouring and/or clarification, obtain supernatant liquor, adopt yin and yang resin to cooperate and handle, negative resin is D280 type or D290 type, the sun resin is D061 type or D001SS type, and the yin and yang resin volume ratio is 2: 1-4: 1; Built-up sequence is: negative resin Zhiyang resin, or positive resin is to negative resin, and the series connection of 1-4 group zwitterion resin column is used, and concentrates liquid glucose and through the flow velocity of resin column be 0.4-1.0 times of per hour resin cumulative volume, collect the following effluent liquid of specific conductivity 10 μ s/cm, promptly.
D280 that the present invention selects for use or D290 strong-basicity styrene series anion exchange resin are with the combination of D061 or D001SS type strongly acidic styrene type cation exchange resin.
3, the plant material that will contain the raffinose family oligose, extract with decocting, also can use alcohol or lower concentration ethanol-extracted, or squeezing is extracted, obtain containing the extract of raffinose family oligose, simmer down to concentrates liquid glucose, the density that concentrates liquid glucose is in the 1.02-1.07 scope, add powdered active carbon earlier, the add-on of Powdered Activated Carbon is the 6-10% of plant material weight, or the 1.5-2.5% of concentrated liquid glucose volume, stirring and make abundant absorption, preferred churning time is 15-25 minute, the chitosan solution add-on is for concentrating the 2-10% of liquid glucose volume, stirring makes and is uniformly dispersed, and is layered as the active carbon layer of lurid supernatant liquor and black, filters supernatant liquor and obtains clarifying decolouring liquid glucose; Through the supernatant liquor after the decolouring-clarification, adopt yin and yang resin to cooperate and handle, negative resin is D280 type or D290 type, and positive resin is D061 type or D001SS type, and the yin and yang resin volume ratio is 2: 1-4: 1; Built-up sequence is: negative resin Zhiyang resin, or positive resin is to negative resin, and the series connection of 1-4 group zwitterion resin column is used, and concentrates liquid glucose and through the flow velocity of resin column be 0.4-1.0 times of per hour resin cumulative volume, collect the following effluent liquid of specific conductivity 10 μ s/cm, promptly.
Said process also can add chitosan solution earlier, adds gac again, and clarifying effect is fine equally.
Three kinds of methods of the present invention are characterised in that:
1) clarification, decolouring are that flocculation agent and the acticarbon of main component is used in combination with chitosan, make solid-liquid phase sharp separation, and a step is finished decolouring and clarification process, has improved decolour clarifying speed and efficient.
2) the decolouring clarifying sugar liquid further adopts the anion-cation exchange resin cooperation to decolour and desalination, and the series connection of 1-4 group yin and yang resin is used, and has improved purification efficiency and resin utilization ratio, has reduced production cost.
3) the present invention selects for use chitosan as flocculation agent, and it is nontoxic, security good, is beneficial to environmental protection, and has outstanding flocculating effect.
Following experimental example is used to further specify the present invention:
Experimental example 1
The present invention has tried out following different combined method in liquid glucose clarification and decolouring step.Experimental technique is: select the decocting of relative density 1.05 to boil the oligose extracting solution that glutinous rehmannia piece root prepares dry, respectively get 100ml, under 70 ℃ of conditions, after requirement adds flocculation agent, gac respectively in the table, pour into immediately in the 100ml measuring bottle, the record Solid-Liquid Separation time, the filter paper filtering time, with Solid-Liquid Separation time and filter paper filtering time as the standard of passing judgment on clarifying effect.Filtrate is measured absorption value, compares with the stoste absorption value, calculates percent of decolourization.The effect of more different combination results is passed judgment on the whole bag of tricks.
The solid-liquid separation time: the liquid glucose that will add flocculation agent, gac, after pouring in the 100ml measuring bottle, the active carbon layer that moment can be seen black begins to sink, and liquid is divided into boundary two portions clearly immediately, and the upper strata is limpid pale yellow solution, lower floor is the Insta-Char of black, along with the sedimentation of gac, the upper strata constantly enlarges, and lower floor constantly reduces, until the complete sedimentation of gac, the active carbon layer floor height is reduced to minimum.At this moment, the upper strata is limpid pale yellow solution, and lower floor is the active carbon layer of black, and solid-liquid reaches mutually fully and separates.Therefore, the Solid-Liquid Separation time, be from gac and begin to drop to the time that the active carbon layer floor height no longer reduces.
The various defecation method results of table 1 relatively
| NO | The method classification | Clarification, decoloring method | Percent of decolourization (%) | Finish the solid-liquid separation time (branch) | The filter paper filtering time (branch) | The comprehensive evaluation effect |
| 1 2 3 4 5 6 7 | The clarification of the alone powdered active carbon of the alone powdered active carbon of the alone fining agent of alone fining agent and decolouring are divided into that two steps clarified and decolouring is combined as step clarification and decolouring is combined as a step | The chitosan solution that only adds liquid glucose volume 3% does not add gac.Add 3% chitosan solution and 1-2.5% cationic polyelectrolyte, do not add gac.Only add the 2g powdered active carbon, do not add finings.1) adds 2g powdered active carbon, centrifuging carbon removal; 2) use filter paper filtering again.1) adds 3% chitosan solution earlier, filter; 2) add powdered active carbon 2g again, filter.Add gac 2g earlier, add 3% chitosan solution again, filter.Add 3% chitosan solution earlier, add powdered active carbon 2g again, filter. | ＜2％ ＜2％ ＜78％ ＜78％ ＞80％ ＞80％ ＞80％ | Had no Separation of Solid and Liquid in 13 minutes 13 minutes and have no Separation of Solid and Liquid 1) first step sedimentation 13 minutes 2) second step sedimentation 6 minutes 6 minutes 6 minutes | 65-180 divides 40-180 to divide 200 minutes 1) centrifugal filtration carbon removal 2) centrifugal rear Filter paper filtering 6 minutes. 1) filter for the first time the 60-180 branch: 2) filter 6 minutes 3 for the second time) add up to 66-186 to divide 1) Filter paper filtering takes 3-18 and divided 7 fens | Sedimentary particle is less, and looser, and filtration velocity is slower.The two coupling can make tiny flocks crosslinked, forms bigger flocks, and the person is fast in the filtration, but still not ideal enough.Only true decolorizing effect, gac floats on a liquid, and does not see solid-liquid separation.Gac floats on a liquid, and does not see solid-liquid separation, and gac is all removed by centrifugal, and centrifugal burden is very heavy.Centrifugal back filter paper filters very fast.1) it is less only to add the particle of chitosan postprecipitation thing, and looser, and filtration velocity is still slower.2) solid-liquid separation was finished in 6 minutes after filtrate added charcoal, and filtrate is limpid, but two steps are loaded down with trivial details.Beyond thought clarification and decolorizing effect have taken place, impurity such as protein, colloid, pigment and gac, chitosan are assembled and are the common sedimentation of one, fall to the moment generation, solid-liquid separation was finished in 6 minutes, filter easily, filtrate disappears bright.Beyond thought clarification and decolorizing effect have taken place in the same NO6 of effect. |
Above-mentioned experiment shows, can see that from filtyration velocity gac and chitosan are used in combination simultaneously, as long as in certain proportion (NO6, NO7), no matter add charcoal earlier and still add finings earlier, filtyration velocity than non-be used in combination reach 10-30 soon doubly, the clarifying effect optimum also has summation action in addition aspect decolouring.
Chitosan flocculant and acticarbon are used in combination in a step, once filter, not only save heating for multiple times, repeatedly sedimentation, filtering cumbersome procedure repeatedly, make decolouring, clarification process merge into one and go on foot and finish; And beyond thought flocculate and clarify effect and speed taken place, the throw out that this associating using method produces has extraordinary settling property and filterability, moment promptly begins sedimentation, through big production test, can finish whole settling processes in 6-10 minute, it is very easy that the filtration of supernatant liquor also becomes, and can adopt tubular-bowl centrifuge to filter or Plate Filtration or filtration of sand filtration rod or tubular fibre filtration.This method greatly improves the production efficiency of clarify and decolorize step, and cost reduces greatly.
Experimental result shows simple use gac, does not add the method for chitosan; Or use chitosan separately, do not add process of active carbon; Or chitosan and anionic polyelectrolyte and usefulness, do not add process of active carbon; These methods all can't be compared with method of the present invention.In the inventive method, synergy has taken place in gac and chitosan, and the adsorption bleaching function of gac and the flocculate and clarify function of chitosan are all brought into play.
Following experimental example and embodiment only are used for explaining but do not limit the protection domain that this is asked.
Experimental example 2Optimization about decolouring-desalination step intermediate ion exchange resin kind and working conditions
In the desalination step, with removing of organic anion impurity and mineral ion is major objective, on the basis of extensive scalping resin, emphasis with 2 kinds of strong basicity macroporous anion exchange resins, 2 kinds of weakly alkaline macroporous anion exchange resins and 2 kinds of macroporous adsorbent resins as the screening object, comparative studies they to the exchange adsorptive capacity of this class impurity, determined to adopt D280 type or D290 type anionite-exchange resin in the purifying oligose technology, and its operational condition has been investigated; Simultaneously, Zeo-karb is also screened, determined employing D061 type or D001SS type Zeo-karb; Yin and yang resin consumption proportion, built-up sequence, combination group number, liquid glucose flow velocity are also investigated.
1, the selection of anionite-exchange resin
The experiment of static exchange adsorption equilibrium: (weight in wet base 5.0g) is respectively charged in the triangular flask with each resin, open and be respectively charged into test liquid 50ml (through the concentrated liquid glucose of above-mentioned decolouring clarification steps, down together), constant speed vibration (100 rev/mins) under the room temperature, measure the different absorption values of test liquid constantly, until reaching the exchange adsorption equilibrium.Measure the absorption value of stoste under co-wavelength simultaneously.Calculate each work exchange adsorptive capacity q of every gram resin constantly with absorption value.q＝(C
0-C)×V/G。C in the formula
0And the absorbance value of C etching solution when being respectively stoste and each, V is the test liquid volume, G is a weight resin.The results are shown in Table 2.
3 kinds of resins of table 2 are to the different adsorptive capacity/g resins that constantly exchange of impurity
| The resin model | 0.5h | 1.5h | 2.5h | 3.5h | 24h |
| D280 D290 D392 | 12.7 12.1 7.5 | 14.3 13.5 10.7 | 14.5 13.9 11.6 | 14.7 14.1 13.8 | 16.1 15.3 15.2 |
Interpretation of result and conclusion:
The work of each resin exchange adsorptive capacity from table, under equal conditions, D280, D290 strongly basic anion exchange resin are all strong to impurity exchange adsorptive power in the solution, the exchange rate of adsorption is all fast, wherein faster with D280, both obviously are better than the D392 weak base anion-exchange resin, therefore select D280, D290 anionite-exchange resin, preferred D280 strongly basic anion exchange resin.
2, the selection of Zeo-karb
This shaker test adopts the method for static exchange, is index with the pH value, investigates various resin cation exchange speed.Method is: get the good above-mentioned resin 5ml of pre-treatment, and in the triangular flask of packing into, and the test liquid 50ml of adding after the anionite-exchange resin exchange, measure the difference pH values in the moment down in whipped state immediately, measure 60 minutes altogether.4 kinds of resin sequential determinations the results are shown in Table 3.
The mensuration (pH value) of 5 kinds of Zeo-karb exchange velocities of table 3
| The resin model time (branch) | D061 | D072 | D001SS | D151 |
| 0 5 10 15 20 60 | 9.908 4.350 3.672 3.249 2.887 2.343 | 9.908 4.539 4.060 3.761 3.576 2.657 | 9.908 4.599 3.967 3.451 3.042 2.412 | 9.908 5.552 5.240 5.065 4.876 4.314 |
Interpretation of result and conclusion:
As seen from the table, 4 kinds of Zeo-karb exchange velocities are different, and the solution that is placed with the D151 resin is higher at the synchronization pH value, unavailable, all can select for use for all the other 3 kinds; The solution that is placed with D061, D001SS, D072 resin is lower at the synchronization pH value, and the hydrogen ion quantity in promptly from the resins exchange to solution is maximum, and exchange velocity is fast, therefore optional these three kinds of resins, preferred D061, D001SS Zeo-karb.
3, resin series connection group number is to the influence of unit volume resin oligose productive rate
Make up by a certain percentage with a kind of negative resin and a kind of positive resin, cumulative volume is 100ml, as 1 group of resin; The 1 group of same resin of connecting then becomes 2 groups of resins; Be composed in series 3 groups, 4 groups resin columns with method, will concentrate liquid glucose by resin column, collect the following liquid glucose of specific conductivity 10 μ s/cm, and concentrating under reduced pressure, drying make and take out loose thing, weigh.The output of Units of Account volume of resins oligose, promptly every gram resin produces the amount of oligose, sees Table 4.
The effect that table 4 is not counted resin combination on the same group compares
| The group number | Yin and yang resin cumulative volume (ml) | Oligose/resin volume (g/ml) |
| 1 2 3 4 | 100 200 300 400 | 0.05 0.22 0.38 0.44 |
By in the table as seen, along with the increase of resin column series connection group number, resin is improving the productive rate of oligose, therefore, the resin column preferred 2-4 that connects organizes more preferably 3 or 4 groups.
Embodiment 1:
Radix Rehmanniae sheet 15kg, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.02, add the powdered active carbon that concentrates liquid long-pending 2% under 80 ℃ of insulations, stirred 25 minutes, and added the chitosan solution of concentrated solution volume 2% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, tubular fibre filters the clarified liq that (aperture 0.2 μ) obtains decolouring, its sugared concentration 12%, specific conductivity 3500 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, the post cumulative volume is 60 liters, flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
Embodiment 2:
Radix Rehmanniae sheet 300g, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into relative density 1.04, add the powdered carbon of material quantity 9% under 70 ℃ of insulations, stirred 20 minutes, add the chitosan solution of concentrated solution volume 4% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, the sand filtration rod filters the clarified liq that obtains decolouring, its sugared concentration 13.5%, specific conductivity 4000 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2.5: 1, the post cumulative volume is 400ml, flow velocity is 0.6 post cumulative volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be condensed into the concentrated solution of relative density 1.20, can 10ml/ props up.
Embodiment 3:
Radix Rehmanniae sheet 300g, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.05, the powdered carbon that adds material quantity 8% under 60 ℃ of insulations, stirred 15 minutes, and added the chitosan solution of concentrated solution volume 6% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, and cooling is below 40 ℃, and is centrifugal through tubular-bowl centrifuge, the clarified liq that obtains decolouring, its sugared concentration 14%, specific conductivity 4300 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-280 anion-exchange resin column → D-061 cation exchange resin column in proper order, and zwitterion column volume ratio is 3: 1, assembles 3 groups of posts, cumulative volume is 400ml,, flow velocity is 0.7 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming, the extruding type dry granulation becomes granule, is packaged as the 3g/ bag.
Embodiment 4:
Rehmannia Root 1500g, section, 20% extraction using alcohol 2 times, refluxed 0.5 hour by each 4 times, united extraction liquid, filter, filtrate decompression is concentrated into the powdered carbon that adds material quantity 7% under 1.06,65 ℃ of insulations of relative density, stirred 15 minutes, the chitosan solution that adds concentrated solution volume 8% then, stirring makes and is uniformly dispersed, and places and makes sedimentation in 10 minutes, incline and supernatant liquor, cooling is below 40 ℃, and is centrifugal through tubular-bowl centrifuge, and the sand filtration rod filters, the clarified liq that obtains decolouring, its sugared concentration 15%, specific conductivity 4800 μ S/cm; According to ordinary method, decolouring, desalination, be evaporated to relative density 1.40, can 100ml/ bottle.
Embodiment 5:
Radix Rehmanniae sheet 300g, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into relative density 1.07, after preliminary decolouring and/or clarification, the clarified liq that obtains decolouring, its sugared concentration 16%, specific conductivity 5400 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, and zwitterion column volume ratio is 4: 1, assembles 4 groups of posts, cumulative volume is 400ml, flow velocity is 1.0 total column volumes per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, is evaporated to relative density 1.10, spraying drying powder-forming, the extruding type dry granulation, packing, 5g/ bag.
Embodiment 6:
Radix Rehmanniae sheet 300g, water extraction 3 times adds 10 times of medicinal material amount deionized waters at every turn, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into the chitosan solution that adds concentrated solution volume 10% under 1.07,65 ℃ of insulations of relative density, stirs to make to be uniformly dispersed, the powdered carbon that adds material quantity 6% then stirred 15 minutes, placed 60 minutes, incline and supernatant liquor, sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 16%, specific conductivity 5500 μ S/cm; According to ordinary method, decolouring, desalination, be evaporated to relative density 1.10, spraying drying powder-forming.
Embodiment 7:
The bright product 1500g of Rhizome of Bear's-foot Fern cleans, squeeze extract 600ml, add water 2000ml again, the 1800ml that squeezes the juice merges the 2400ml that squeezes the juice, measure the chitosan solution that 1.02,70 ℃ of insulations of relative density add concentrated solution volume 5% down, stirring makes and is uniformly dispersed, the powdered carbon that adds material quantity 9% then stirred 20 minutes, placed to make sedimentation in 10 minutes, incline and supernatant liquor, sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 13%, specific conductivity 4100 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-290 anion-exchange resin column → D-001SS cation exchange resin column in proper order, zwitterion column volume ratio is 2.5: 1, assemble 2 groups of posts, the post cumulative volume is 400ml, and flow velocity is 0.6 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be condensed into the concentrated solution of relative density 1.30, can 100ml/ bottle.
Embodiment 8:
Ground dried bamboo shoots sheet 400g, water extraction 3 times adds 10 times of medicinal material amount deionized waters at every turn, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into the chitosan solution that adds concentrated solution volume 6% under 1.05,60 ℃ of insulations of relative density, stirs to make to be uniformly dispersed, the powdered carbon that adds material quantity 8% then stirred 15 minutes, placed to make sedimentation in 10 minutes, incline and supernatant liquor, sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 14%, specific conductivity 4800 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-290 anion-exchange resin column → D-001SS cation exchange resin column in proper order, zwitterion column volume ratio is 3: 1, assemble 3 groups of posts, the post cumulative volume is 600ml, and flow velocity is 0.7 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
Embodiment 9:
Ground dried bamboo shoots sheet 300g, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into relative density 1.06,65 ℃ of insulations add the chitosan solution of concentrated solution volume 7% down, stir to make to be uniformly dispersed, and make its sedimentation, the filtering precipitation, the powdered carbon that adds material quantity 7% then stirred 15 minutes, placed to make sedimentation in 20 minutes, incline and supernatant liquor, sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 15%, specific conductivity 5000 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-0072 cation exchange resin column → D-290 anion-exchange resin column zwitterion post in proper order, volume ratio is 4: 1, assemble 4 groups of posts, the post cumulative volume is 400ml, and flow velocity is 1.0 total column volumes per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.10, spraying drying powder-forming.
Embodiment 10:
Rhizome of Bear's-foot Fern dry plate 200g and Radix Rehmanniae sheet 100g, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid, filter, filtrate decompression is concentrated into the chitosan solution that adds concentrated solution volume 4% under 1.03,80 ℃ of insulations of relative density, stirring makes and is uniformly dispersed, the powdered active carbon that adds material quantity 10% then stirred 25 minutes, placed to make sedimentation and be cooled to room temperature, incline and supernatant liquor, centrifugal through tubular-bowl centrifuge, as to obtain decolouring clarified liq, its sugared concentration 12%, specific conductivity 3700 μ S/cm.Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-001SS cation exchange resin column → D-290 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, and the post cumulative volume is 500ml, and flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming, extruding type dry granulation, packing, the 5g/ bag.
Embodiment 11:
Radix Rehmanniae sheet 300g, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into relative density 1.07, after preliminary decolouring and/or clarification, the clarified liq that obtains decolouring, its sugared concentration 16%, specific conductivity 5400 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 3: 1, assemble 2 groups of posts, flow velocity is 0.6 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.10, spraying drying powder-forming, extruding type dry granulation, packing.
Embodiment 12:
Radix Rehmanniae sheet 15kg, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.02, add the powdered active carbon that concentrates liquid long-pending 2% under 80 ℃ of insulations, stirred 20 minutes, and added the chitosan solution of concentrated solution volume 8% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, tubular fibre filters the clarified liq that obtains decolouring, its sugared concentration 12%, specific conductivity 3500 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, the post cumulative volume is 60 liters, flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
Above embodiment quality product following (pressing dry product calculates):
| NNO | Total reducing sugar (%) | Stachyose (%) | Functional oligose total amount (%) | Functional oligose/total reducing sugar ratio (%) |
| 11 22 33 44 55 66 77 88 99 110 | 96.01 96.12 96.10 96.20 96.37 96.00 96.07 96.10 97.10 97.50 | 64.65 64.30 63.21 62.11 63.65 67.60 71.00 68.01 69.00 66.08 | 76.28 79.35 78.69 76.67 75.82 82.28 82.00 88.89 90.12 87.40 | 79.46 82.55 81.88 79.70 78.68 85.71 85.35 92.50 92.81 89.64 |
Described decolouring-the defecation method of the application and decolouring-desalination method not only can be used in combination, and are used for the purifying of raffinose family oligose extract; Also can be respectively and other purification process combination, be used for the purifying of raffinose family oligose extract; Or use respectively separately, only as the method for extract decolouring-clarification of raffinose family oligose or decolouring-desalination.
Claims (14)
1, a kind of raffinose family oligose preparation method of extract based on stachyose is characterized in that this method is:
The plant material that will contain the raffinose family oligose, decocting or ethanol-extracted, or squeezing is extracted, obtain extract, the extract simmer down to concentrates liquid glucose, the density that concentrates liquid glucose adds powdered active carbon earlier in the 1.02-1.07 scope, the add-on of Powdered Activated Carbon is the 6-10% of plant material weight, or the 1.5-2.5% of concentrated liquid glucose volume, stirring makes abundant absorption, and churning time is 15-25 minute, adds chitosan solution then, the chitosan solution add-on is for concentrating the 2-10% of liquid glucose volume, stirring makes and is uniformly dispersed, and is layered as the active carbon layer of lurid supernatant liquor and black, filters supernatant liquor and obtains the clarifying sugar liquid that decolours; Adopted according to prior art again that the anion-cation exchange resin post further decolours, desalination, promptly.
2, a kind of raffinose family oligose preparation method of extract based on stachyose is characterized in that this method is:
The plant material that will contain the raffinose family oligose, decocting or ethanol-extracted, or squeezing is extracted, obtain extract, the extract simmer down to concentrates liquid glucose, the density that concentrates liquid glucose is in the 1.02-1.07 scope, concentrate and add chitosan solution in the liquid glucose earlier, the chitosan solution add-on is for concentrating the 2-10% of liquid glucose volume, and stirring makes and is uniformly dispersed, and then adds powdered active carbon, the add-on of Powdered Activated Carbon is the 6-10% of plant material weight, or the 1.5-2.5% of concentrated liquid glucose volume, churning time is 15-25 minute, stirs to make abundant absorption; Separation of supernatant, clarifying sugar liquid must decolour; Adopted according to prior art again that the anion-cation exchange resin post further decolours, desalination, promptly.
3, preparation method of extract according to claim 1 is characterized in that this method is:
The Rehmannia Root section, 20% extraction using alcohol 2 times refluxed 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.06, add the powdered carbon of material quantity 7% under 65 ℃ of insulations, stirred 15 minutes, add the chitosan solution of concentrated solution volume 8% then, stirring makes and is uniformly dispersed, and places to make sedimentation in 10 minutes, and inclining supernatant liquor, cooling is below 40 ℃, and is centrifugal through tubular-bowl centrifuge, and the sand filtration rod filters, the clarified liq that obtains decolouring, its sugared concentration 15%, specific conductivity 4800 μ S/cm; According to ordinary method decolouring-desalination, be evaporated to relative density 1.40, promptly again.
4, as preparation method of extract as described in the claim 2, it is characterized in that this method is:
The Radix Rehmanniae sheet, water extraction 3 times adds 10 times of medicinal material amount deionized waters at every turn, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into the chitosan solution that adds concentrated solution volume 10% under 1.07,65 ℃ of insulations of relative density, stirs to make to be uniformly dispersed, the powdered carbon that adds material quantity 6% then stirred 15 minutes, placed 60 minutes, incline and supernatant liquor, sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 16%, specific conductivity 5500 μ S/cm; According to ordinary method, decolouring, desalination, be evaporated to relative density 1.10, spraying drying powder-forming.
5, preparation method of extract according to claim 1 is characterized in that this method is:
Must decolour behind the clarifying sugar liquid, through the supernatant liquor after the decolouring-clarification, adopt yin and yang resin to cooperate and handle, negative resin is D280 type or D290 type, and positive resin is D061 type or D001SS type, and the yin and yang resin volume ratio is 2: 1-4: 1; Built-up sequence is: negative resin Zhiyang resin, or positive resin is to negative resin, and the series connection of 1-4 group zwitterion resin column is used; The flow velocity of extracting solution process resin column is 0.4-1.0 a times of per hour resin cumulative volume, collects the following effluent liquid of specific conductivity 10 μ s/cm, promptly.
6, as preparation method of extract as described in the claim 2, it is characterized in that this method is:
Must decolour behind the clarifying sugar liquid, through the supernatant liquor after the decolouring-clarification, adopt yin and yang resin to cooperate and handle, negative resin is D280 type or D290 type, and positive resin is D061 type or D001SS type, and the yin and yang resin volume ratio is 2: 1-4: 1; Built-up sequence is: negative resin Zhiyang resin, or positive resin is to negative resin, and the series connection of 1-4 group zwitterion resin column is used; The flow velocity of extracting solution process resin column is 0.4-1.0 a times of per hour resin cumulative volume, collects the following effluent liquid of specific conductivity 10 μ s/cm, promptly.
7, as preparation method of extract as described in claim 5 or 6, it is characterized in that this method is:
The Radix Rehmanniae sheet obtains decolouring behind the clarifying sugar liquid, liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, and zwitterion column volume ratio is 4: 1, assembles 4 groups of posts, flow velocity is 1.0 total column volumes per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.10, spraying drying powder-forming, the extruding type dry granulation, packing.
8, as preparation method of extract as described in claim 5 or 6, it is characterized in that this method is:
The Radix Rehmanniae sheet obtains decolouring behind the clarifying sugar liquid, liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, and zwitterion column volume ratio is 3: 1, assembles 2 groups of posts, flow velocity is 0.6 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.10, spraying drying powder-forming, the extruding type dry granulation, packing.
9, preparation method as claimed in claim 5 is characterized in that this method is:
The Radix Rehmanniae sheet, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.02, add the powdered active carbon that concentrates liquid long-pending 2% under 80 ℃ of insulations, stirred 20 minutes, and added the chitosan solution of concentrated solution volume 8% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, tubular fibre filters the clarified liq that obtains decolouring, its sugared concentration 12%, specific conductivity 3500 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, the post cumulative volume is 60 liters, flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
10, preparation method as claimed in claim 5 is characterized in that this method is:
The Radix Rehmanniae sheet, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.02, add the powdered active carbon that concentrates liquid long-pending 2% under 80 ℃ of insulations, stirred 25 minutes, and added the chitosan solution of concentrated solution volume 2% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, tubular fibre filters the clarified liq that obtains decolouring, its sugared concentration 12%, specific conductivity 3500 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, the post cumulative volume is 60 liters, flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
11, preparation method as claimed in claim 5 is characterized in that this method is:
The Radix Rehmanniae sheet, water extraction 3 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid filters, filtrate decompression is concentrated into relative density 1.04, add the powdered carbon of material quantity 9% under 70 ℃ of insulations, stirred 20 minutes, add the chitosan solution of concentrated solution volume 4% then, stirring makes and is uniformly dispersed, place and made sedimentation in 10 minutes, inclining supernatant liquor, is cooled to below 40 ℃, centrifugal through tubular-bowl centrifuge, the sand filtration rod filters the clarified liq that obtains decolouring, its sugared concentration 1 3.5%, specific conductivity 4000 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-061 cation exchange resin column → D-280 anion-exchange resin column → D-061 cation exchange resin column → D-280 anion-exchange resin column in proper order, zwitterion column volume ratio is 2.5: 1, the post cumulative volume is 400ml, flow velocity is 0.6 post cumulative volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be condensed into the concentrated solution of relative density 1.20, can 10ml/ props up.
12, preparation method as claimed in claim 6 is characterized in that this method is:
The bright product 1500g of Rhizome of Bear's-foot Fern cleans, squeeze extract 600ml, add water 2000ml again, the 1800ml that squeezes the juice merges the 2400ml that squeezes the juice, and measures relative density 1.02,70 ℃ of insulations add the chitosan solution of concentrated solution volume 5% down, stir to make to be uniformly dispersed, and add the powdered carbon of material quantity 9% then, stirred 20 minutes, place and made sedimentation in 10 minutes, inclining supernatant liquor, and sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 13%, specific conductivity 4100 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-290 anion-exchange resin column → D-001SS cation exchange resin column in proper order, zwitterion column volume ratio is 2.5: 1, assemble 2 groups of posts, the post cumulative volume is 400ml, flow velocity is 0.6 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, is condensed into the concentrated solution of relative density 1.30.
13, preparation method as claimed in claim 6 is characterized in that this method is:
Ground dried bamboo shoots sheet water extraction 3 times adds 10 times of medicinal material amount deionized waters at every turn, decocts 0.5 hour, united extraction liquid filters, and filtrate decompression is concentrated into relative density 1.05,60 ℃ of insulations add the chitosan solution of concentrated solution volume 6% down, stir to make to be uniformly dispersed, and add the powdered carbon of material quantity 8% then, stirred 15 minutes, place and made sedimentation in 10 minutes, inclining supernatant liquor, and sheet frame filters, the clarified liq that obtains decolouring, its sugared concentration 14%, specific conductivity 4800 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-290 anion-exchange resin column → D-001SS cation exchange resin column in proper order, zwitterion column volume ratio is 3: 1, assemble 3 groups of posts, the post cumulative volume is 600ml, and flow velocity is 0.7 total column volume per hour, collects the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
14, preparation method as claimed in claim 6 is characterized in that this method is:
Rhizome of Bear's-foot Fern dry plate and Radix Rehmanniae sheet, water extraction 2 times, 10 times of medicinal material amount deionized waters of each adding, decocted 0.5 hour, united extraction liquid, filter, filtrate decompression is concentrated into the chitosan solution that adds concentrated solution volume 4% under 1.03,80 ℃ of insulations of relative density, stirring makes and is uniformly dispersed, the powdered active carbon that adds material quantity 10% then stirred 25 minutes, placed to make sedimentation and be cooled to room temperature, incline and supernatant liquor, centrifugal through tubular-bowl centrifuge, as to obtain decolouring clarified liq, its sugared concentration 12%, specific conductivity 3700 μ S/cm; Liquid glucose passes through the anion-cation exchange resin post under room temperature, post is D-001SS cation exchange resin column → D-290 anion-exchange resin column in proper order, zwitterion column volume ratio is 2: 1, the post cumulative volume is 500ml, flow velocity is 0.5 total column volume per hour, collect the following effluent liquid of specific conductivity 10 μ s/cm, be evaporated to relative density 1.15, spraying drying powder-forming.
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| CN100537583C (en) * | 2005-12-30 | 2009-09-09 | 上海中医药大学附属曙光医院 | Dried rehmannia root oligosaccharide and its preparation method and uses |
| CN100457765C (en) * | 2007-01-16 | 2009-02-04 | 广东太阳神集团有限公司 | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root |
| CN101633676B (en) * | 2009-06-04 | 2011-06-08 | 中国食品发酵工业研究院 | Method for preparing high-purity stachyose by using plant chromatographic separation technology |
| CN102028801B (en) * | 2009-09-30 | 2013-03-20 | 上海中医药大学附属曙光医院 | Radix Rehmanniae oligosaccharide pulmonary delivery traditional Chinese medicinal preparation as well as preparation method and application thereof |
| CN103131744A (en) * | 2013-02-04 | 2013-06-05 | 中国食品发酵工业研究院 | Preparation method of high-purity plant source oligomerization galactose |
| CN103265583B (en) * | 2013-03-05 | 2016-01-13 | 中国食品发酵工业研究院 | A kind of preparation method of stachyose crystal |
| CN105693783B (en) * | 2016-01-23 | 2018-10-23 | 内蒙古昶辉生物科技股份有限公司 | The preparation method of gossypose is extracted in a kind of dregs of rice from cotton seed |
| CN107383128B (en) * | 2017-08-01 | 2019-06-18 | 江南大学 | A kind of discoloration method of steviol glycoside aqueous extract |
| CN114028836A (en) * | 2021-09-26 | 2022-02-11 | 承创(常熟)医药科技有限公司 | Method for removing pigment and odor from plant extract |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1223265A (en) * | 1998-01-12 | 1999-07-21 | 济南三株药业有限公司 | Process for preparing stachyose and its products and application |
| CN1300857A (en) * | 1999-12-23 | 2001-06-27 | 中国食品发酵工业研究所 | Stachyose and its preparing process |
| CN1339443A (en) * | 2000-08-25 | 2002-03-13 | 陈梅英 | Extracting method for stachyose |
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| CN1223265A (en) * | 1998-01-12 | 1999-07-21 | 济南三株药业有限公司 | Process for preparing stachyose and its products and application |
| CN1300857A (en) * | 1999-12-23 | 2001-06-27 | 中国食品发酵工业研究所 | Stachyose and its preparing process |
| CN1339443A (en) * | 2000-08-25 | 2002-03-13 | 陈梅英 | Extracting method for stachyose |
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