CN104945534A - Method for preparing polysaccharide available for peritoneal dialysis from cation exchange resin hydrolysis starch - Google Patents
Method for preparing polysaccharide available for peritoneal dialysis from cation exchange resin hydrolysis starch Download PDFInfo
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- 229920002472 Starch Polymers 0.000 title claims abstract description 44
- 235000019698 starch Nutrition 0.000 title claims abstract description 44
- 239000008107 starch Substances 0.000 title claims abstract description 43
- 150000004676 glycans Chemical class 0.000 title claims abstract description 39
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 39
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 19
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 18
- 238000000502 dialysis Methods 0.000 title claims abstract description 12
- 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 title abstract description 6
- 239000003729 cation exchange resin Substances 0.000 title abstract 3
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 33
- 239000000706 filtrate Substances 0.000 claims abstract description 23
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- 230000000694 effects Effects 0.000 claims description 9
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- 238000002360 preparation method Methods 0.000 claims description 8
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- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 8
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- 239000007900 aqueous suspension Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004108 freeze drying Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
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- 239000002253 acid Substances 0.000 description 6
- 239000008120 corn starch Substances 0.000 description 6
- 229920002177 Icodextrin Polymers 0.000 description 5
- 238000010828 elution Methods 0.000 description 5
- 229940016836 icodextrin Drugs 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 3
- 239000000385 dialysis solution Substances 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 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 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 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
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 235000008504 concentrate Nutrition 0.000 description 2
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 2
- 239000008121 dextrose Substances 0.000 description 2
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
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- 238000000746 purification Methods 0.000 description 2
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- 150000003384 small molecules Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
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- 239000004382 Amylase Substances 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing polysaccharide available for peritoneal dialysis from green hydrolysis starch. Compared with traditional hydrolysis starch, enzymolysis and acidolysis, cation exchange resin is adopted as catalyst hydrolysis starch in the invention. A heat source is not introduced in the method, the follow-up desalting problem is avoided, and the polysaccharide obtained by hydrolysis is better for peritoneal dialysis. The method for preparing soluble polysaccharide mainly comprises the following steps: (1) preparing grain starch into certain aqueous suspension, and gelatinizing at 100-120 DEG C, wherein the gelatinizing process is monitored with a rotational viscometer; (2) hydrolyzing at 80-95 DEG C at a certain volume ratio of the cation exchange resin to solvent water, wherein the reaction process is monitored with a Ubbelohde viscometer, and final DE of the hydrolysate is 10-20; and (3) preparing the obtained hydrolysate into a solution of which the polysaccharide content is 15-20% by mass, performing ultrafiltration with a membrane envelop with molecular weight cut-off (NMWCO) of 100KD, and fetching the filtrate; performing ultrafiltration on the filtrate with a membrane envelop with NMWCO of 3KD, and fetching the concentrate, wherein the polysaccharide DE of the concentrate is less than 5.4; drying the obtained concentrate; and performing freeze drying or spray drying to obtain soluble polysaccharide of which the weight-average molecular weight Mw is 10-20KD and the number-average molecular weight Mn is 2,500-7,000.
Description
Technical field
The present invention designs field of medicaments, particularly a kind of preparation method for peritoneal dialysis polysaccharide
Technical background
Main ingredient for peritoneal dialysis solution has two classes, and a class is small molecules, as dextrose, and amino acid; Another kind of is soluble polysaccharide, as icodextrin, and Mw13000 ~ 19000.Dextrose and amino acids peritoneal dialysis solution are to early stage renal failure patient, urea is discharged by ultrafiltration, the body toxic metabolic products such as creatinine have certain effect, but because small molecules is easily absorbed by ultrafiltration through capillary wall on peritonaeum, maintain the osmotic pressure time short, and sugar and the metabolism disorder of nitrogen class can be caused.Polysaccharide peritoneal dialysis solution is used for end-stage renal failure patient and just seems particularly important, icodextrin is exactly wherein a kind of, because the molecular weight distribution of icodextrin is interval, also have containing certain α (1,6)-glycosidic link, this polysaccharide properties is stablized, the sugar of side chain has certain effect to preventing enzymic hydrolysis, these character all make icodextrin can maintain osmotic pressure,effective in a long time, can not be absorbed by capillary vessel ultrafiltration on peritonaeum and cause larger side effect again, have good effect to removing Toxic Metabolites.
Tradition is take waxy cereal as raw material for the preparation of peritoneal dialysis polysaccharide method, as waxy corn starch, tapioca (flour), Fructus Hordei Germinatus starch is raw material, with heat-resisting amylase for catalyzer, as thermophilric bacteria α-amylase, random inscribe α (1,4) hydrolysis of glycoside bond starch, obtains the sugar of certain molecular weight section.Or take acid as catalyzer, hydrolyzed starch.Wherein, the main hydrochloric acid of acid, sulfuric acid, nitric acid, phosphoric acid, wherein hydrochloric acid is conventional.
Zeo-karb can make the positively charged ion in liquid phase and solid phase cationic reversibility exchange, to reach removing anions in solution object, particularly metallic cation.Zeo-karb crosslinking structure skeleton mainly contains polystyrene type
polyacrylie-type
zeo-karb is commonly used in softening water preparation, and prepared by refined sugar, senior table syrup purifying, but invention introduces Zeo-karb atypical function, i.e. hydrolyzed starch or polysaccharide.
Resin cation (R.C.) comprises two types, and the first, strongly acidic cation-exchange: main containing highly acid reactive group, as sulfonic group (-SO
3h), this ion exchange resin can exchange all positively charged ions, and this kind of Zeo-karb acidity is stronger, is more suitable for doing Polysaccharides use, as 732 Zeo-karbs; The second, weak-type Zeo-karb: have more weak reactive group, as carboxyl (-COOH), the positively charged ion of this ion exchange resin only in commutative weak base is as Ca
2+, Mg
2+, for the ion in highly basic as Na
+, K
+etc. cannot exchange, this kind of Zeo-karb acidity is slightly weak, wants Polysaccharides, must improve temperature or extend hydrolysis time, as D113 Zeo-karb.
Although enzyme, the method polysaccharide that the preparation of mineral acid hydrolysis starch can be used for peritoneal dialysis is more, but there is following shortcoming: enzymic hydrolysis starch, this method uses protease, easy introduction is to the disadvantageous thermal source of human body, and generally to add the activator that a certain amount of calcium ion does enzyme in reaction process, subsequent technique has used the method removing calcium ions such as ion-exchange, makes technique more loaded down with trivial details.Acid hydrolyzed starches, this method is catalyzer owing to will add strong acid, high to equipment requirements, and reaction terminates to carry out neutralizing acid with corresponding alkali, make in polysaccharide solvent containing a large amount of salt, subsequent technique desalination is cumbersome, and in peritoneal dialysis raw materials quality standard, salts contg controls more accurate, make polysaccharide unstable too much, can catalysis polysaccharide hydrolysis monose under certain humidity, in the sterilizing of high temperature height, monose easily changes into again human muscle and neural virulent 5 hydroxymethyl furfural, this may be that the preparation of current icodextrin is only by the reason of the method for enzymic hydrolysis.
Summary of the invention
The present invention relates to a kind of green amylatic method, the soluble polysaccharide be hydrolyzed into easily does not introduce the material of thermal source containing enzyme etc., and not containing the salt being difficult to remove, simplifies technique, be easy to the preparation of pharmaceutical grade polysaccharide raw material.
The present invention relates to one and can be used for peritoneal dialysis, the polysaccharide that molecular weight distribution is comparatively concentrated, molecular weight becomes normal distribution.
A kind of pretreated method before the present invention relates to Starch Hydrolysis, this method makes the first gelatinization of starch, destroys starch crystals district, be more conducive to cation resin catalyzing hydrolyzed starch.
The present invention relates to the resin cation (R.C.) of catalytic starch hydrolysis, activity unit is sulfonic acid (-SO
3h), carboxylic acid (-COOH); Resin cation (R.C.) skeleton is polystyrene
polyacrylic
The present invention relates to the method for monitoring starch burn degree, be hydrolyzed again to regulation viscosity by rotary viscosity instrument monitoring starch pasting.
The present invention relates to the method controlling starch hydrolysate molecular weight, by measuring the hydrolyzed solution Ubbelohde viscosity elution time, hydrolysate DE value scope controls molecular weight distribution.
The present invention relates to a kind of process for purification of soluble polysaccharide, by the accurate molecular weight cut-off of ultrafiltration, sugar that is excessive and small-molecular-weight excessively in removing soluble sugar.
The present invention relates to different size ultra-filtration membrane bag to the impact of refined polysaccharide molecular weight, and the film bag screening best molecular retention amount carries out refinishing polyose.
The present invention relates to the impact of temperature on ultrafiltration efficiency and refined polysaccharide molecular weight distribution, and screen best ultrafiltrate temperature.
The present invention relates to the mass concentration of the most applicable ultrafiltration sugar, proving that concentration is too high or too low by experiment all can affect ultrafiltration efficiency.
Accompanying drawing explanation
Fig. 1: the polysaccharide molecular weight distribution obtained under different amount ion exchange resin
Fig. 2: the polysaccharide molecular weight distribution that under differing temps, hydrolyzed starch obtains
Fig. 3: the film bag ultrafiltration of differing molecular interception obtains polysaccharide concentrated solution molecular weight distribution
Fig. 4: different ultrafiltration number of times is except small molecular sugar molecular weight distribution
Embodiment
Embodiment 1
732 cation resin hydrolyzing starch are also refining
Get waxy corn starch appropriate, add water and be made into the outstanding slurry of 30% (W/V), gelatinization 20min at 100 DEG C, gelatinization limit, limit is stirred.Measure rotary viscosity 40k ~ 50kmpas, cooling.
Temperature is down to 80 DEG C, adds 732 Zeo-karbs with water different volumes ratio, V/V, 1/5,2/5,3/5,4/5 respectively.Stir hydrolysis reaction 2 ~ 6 hours, detect the elution time with the Ubbelohde viscometer of Φ 0.5-0.6mm, when the elution time at 245 ± 10s time stopped reaction.With 20 object gauze filtered while hot stopped reaction, collect filtrate, the Zeo-karb washing three times of 1/10 volume, merging filtrate.
The filtrate band temperature of gained is down to about 50 DEG C, and with diatomite filtration, removing can not water-soluble sugar or non-hydrolyzed starch particulate.The volume of quantitative gained filtrate, dilutes 2 times by filtrate, be made into mass concentration 15% ~ 20% sugar soln.
By the film bag ultrafiltration of upper sugar soln NMWCO100KD, ultrafiltrate temperature 50 DEG C, pressure 0.4 ~ 0.6bar, is concentrated into volume 1/10, then thin up 3 times, and reconcentration, to volume 1/5, merges and collects filtrate.Filtrate weight-average molecular weight Mw10000D ~ 30000D, number-average molecular weight Mn700 ~ 2000.
The film bag ultrafiltration of filtrate NMWCO3KD, ultrafiltration pressure 1.6bar ~ 2.0bar, temperature 50 C.First time is concentrated into original volume 1/3, redilution 2 times.Reconcentration 3 times, is concentrated into volume 1/3 at every turn afterwards, dilutes 3 times.Get concentrated solution GPC detection molecules amount.Concentrated solution weight-average molecular weight Mw10000 ~ 37000, number average molecular weight Mn2800 ~ 6800, DE < 5.
Concentrated solution is added 1% gac, 60 DEG C of stir process 2h, filter, get filtrate.
Filtrate lyophilize is obtained white polysaccharide solid.
Embodiment 2
Differing temps hydrolyzed starch
Starch pasting method, with embodiment 1, obtains pasted starch.
Add 732 Zeo-karb volumes, resin volume/volume of water 3/5.
Sample three groups, respectively at 85 DEG C, 95 DEG C, stir hydrolysis at 100 DEG C 3 hours.Use 20 object filtered through gauze while hot, resin 1/10 volume washes three times, merging filtrate.
The filtrate of gained is cooled to about 50 DEG C, with diatomite filtration, and removing water-insoluble polysaccharide and non-hydrolyzed starch particle.
Afterwards filtrate is made into the sugar of mass concentration 15% ~ 20%, at 50 DEG C, ultrafiltration is refined, and first gets filtrate with NMWCO100KD film is refining, then gets concentrated solution with the film of NMWCO3KD is refining.Purification condition is with embodiment 1.
To above concentrated solution 1% gac 60 DEG C process 2h, more cryodesiccated white polysaccharide solid.
Embodiment 3
D113 macroporous resin hydrolyzed starch
Take waxy corn starch appropriate, be made into the outstanding slurry of starch of mass concentration (W/V) 30%, gelatinization 20min at 100 DEG C, stops gelatinization when measuring its rotary viscosity 40k ~ 50kmpas.
The starch of gelatinization is cooled to 95 DEG C, adds the D113 Zeo-karb of 4/5 volume water, stirring reaction 5h ~ 6h at 95 DEG C.Detect the elution time with the Ubbelohde viscometer of Φ 0.5-0.6mm, when the elution time at 270 ± 10s time stopped reaction.With 20 object gauze filtered while hot stopped reaction, collect filtrate, the Zeo-karb washing three times of 1/10 volume, merging filtrate.
Deng filtrate temperature be down to 50 DEG C right time, with diatomite filtration, removing can not water-soluble sugar or non-hydrolyzed starch particulate, and dry filter cake polysaccharide and the starch mixture of calculating, according to this for calculating filtrate containing Sugar concentration.Quantitative filtrate volume, adds water and sugar soln is diluted to the solution of 15% ~ 20% mass concentration.These solution D E10 ~ 15.
According to embodiment 1, refine sugar soln, gained concentrated solution activated carbon treatment is decoloured, the thermal source that absorption is introduced, lyophilize, polysaccharide weight-average molecular weight Mw10000 ~ 20000 obtained, number-average molecular weight Mn3000 ~ 6000, DE < 5.
Embodiment 4
Under differing temps, ultrafiltration is on the impact of refinishing polyose effect
With waxy corn starch at 80 DEG C, the product that 732 resin cation (R.C.)s and water volume ratio 3/5 condition are hydrolyzed is refined material, and being made into mass concentration is 15% ~ 20% sugar soln.Be respectively 15 DEG C in temperature, 30 DEG C, under 50 DEG C of conditions, ultrafiltration carried out to hydrolysate and refine.
Ultrafiltration result shows, and along with ultrafiltrate temperature increases, take-off rate is accelerated, and under uniform pressure, at 30 DEG C, ultrafiltration is ultrafiltration liquid take-off rate 1.6 times at 15 DEG C, and the discharge rate at 50 DEG C is equivalent to 2.5 times at 15 DEG C.And experimental result display, along with temperature raises, the film bag of NMWCO3KD is except micromolecular effect increase.By the ultrafiltration and concentration number of times in embodiment 1, the conditions such as volume, at 50 DEG C, the sugared content of molecular weight below 1000 can control below 3% by ultrafiltration, and at 15 DEG C, the sugared content of molecular weight below 1000 can only control below 6% by ultrafiltration.This illustrates raised temperature and be conducive to the little sugar removing of molecular weight.The amount of monose can be controlled, thus decrease the danger producing the harmful by-products such as 5 hydroxymethyl furfural in sterilizing.
Embodiment 5
Differing molecular interception film bag is to refinishing polyose influential effect
With waxy corn starch at 80 DEG C, the product that 732 resin cation (R.C.)s and water volume ratio 3/5 condition are hydrolyzed is refined material, and being made into mass concentration is 15% ~ 20% sugar soln.Get molecular retention amount and be respectively 3KD, the film bag of 5KD, 10KD is refined hydrolysate, ultrafiltrate temperature 50 DEG C, concentrated 2 times, concentrates 1/3 at every turn, dilutes 3 times of volumes.
Illustrated by accompanying drawing 3, the film that molecular retention amount is too large, the sugar of the molecular weight removed is more, causes tuple average molecular weight bigger than normal, makes the sugared skewness of different fragments molecule, goes small molecular sugar should select the film bag of molecular retention amount 3KD ~ 5KD.
Embodiment 6
Different ultrafiltration number of times is except small molecular sugar
With waxy corn starch at 80 DEG C, the product that 732 resin cation (R.C.)s and water volume ratio 3/5 condition are hydrolyzed is refined material, and being made into mass concentration is 15% ~ 20% sugar soln.Ultrafiltration pressure, temperature with embodiment 1, first with the ultra-filtration membrane ultrafiltration 2 ~ 4 times of molecular retention amount 100KD, first concentrate volume 1/10 at this, once, dilute 2 times, 1 ~ 3 time of reconcentration 1/2, gets filtrate, then gets the ultra-filtration membrane bag ultrafiltration and concentration 2 respectively of molecular retention amount 3KD, 3,6,8 times, each dilution 3 times, concentrated volume is 1/3 ~ 1/5, gets each concentrated solution GPC and surveys molecular weight distribution.
Ultrafiltration and concentration liquid result shows, the film bag of molecular retention amount 3KD is difficult to remove completely the sugar that molecular weight is less than 3KD, and ultrafiltration number of times can make molecular weight distribution more concentrated 3 ~ 8 times time, presents normal distribution.Weight-average molecular weight 15KD ~ 23KD, number-average molecular weight 3000 ~ 5500.
Claims (9)
1. hydrolyzed starch preparation can be used for the technique of peritoneal dialysis polysaccharide: an a, by first for starch gelatinization before hydrolysis; B, is hydrolyzed with the starch of Zeo-karb to gelatinization; C, refines starch hydrolyzate successively with the ultra-filtration membrane bag of molecular retention amount (NMWCO) 100KD/3KD; D is dry to refining polysaccharide soln.
2. according to claim 1, in starch pasting, starch/water (W/V) 20% ~ 40%, best 30%; Starch gelatinization temperature scope is 100 DEG C ~ 120 DEG C, time 10min ~ 30min, starch paste rotary viscosity 40k ~ 50kmpas.
3., according to claim 1, the Zeo-karb activity unit of hydrolyzed starch is sulfonic acid [-SO
3h], carboxylic acid [-COOH]; Skeleton is polystyrene
polyacrylic
hydrolysis Zeo-karb is 2/5 ~ 4/5 of the water yield (V/V).
4., according to claim 1, Starch Hydrolysis temperature is 75 DEG C ~ 95 DEG C, hydrolysis time 2h ~ 6h; Starch hydrolyzate DE10 ~ 20.
5. according to claim 1, refining with Sugar concentration 10% ~ 20%.
6., according to claim 1, ultrafiltrate temperature is at 40 DEG C ~ 55 DEG C.
7., according to claim 1, NMWCO100KD membrane concentration number of times is at 2 ~ 4 times, and concentrated volume 1/10 ~ 1/2, obtains filtrate Mw > 100kd and be less than 5%; NMWCO3KD membrane concentration 3 ~ 9 times, concentrated volume 1/3 ~ 1/5, obtains Mw < 1kd and is less than 5%.
8. gained is used for polysaccharide Mw14000 ~ 20000 of peritoneal dialysis, Mn3000 ~ 5000, DE < 5.
9. according to claim 8, be applicable to the polysaccharide Mw < 3000 of peritoneal dialysis, limitation 12%; Mw > 50000, limitation 22%; Different molecular weight section polysaccharide content Mw > 50000: Mw < 3000=1.5 ~ 2.0; Mw25000 ~ 50000: Mw3000 ~ 7000=0.6 ~ 1.4; Mw7000 ~ 25000 > 40%.
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