CN105199007A - Polyporus seleno-polysaccharide preparation method - Google Patents
Polyporus seleno-polysaccharide preparation method Download PDFInfo
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Abstract
The invention discloses a polyporus seleno-polysaccharide preparation method and belongs to the technical field of traditional Chinese medicine processing. The polyporus seleno-polysaccharide preparation method comprises hydrolyzing a polyporus crude polysaccharide by papain, purifying the hydrolysate by an alumina purifying column to obtain refined polyporus pure polysaccharide, mixing the refined polyporus pure polysaccharide, dehydrated pyridine as a selenylation reaction initiator, selenium oxychloride, barium chloride as a catalyst and a sodium nitrate solution as a chemical stabilizing agent, and carrying out a reaction process to produce polyporus seleno-polysaccharide. The preparation method of the seleno-polysaccharide from polyporus crude polysaccharide has the advantages of fast and high efficiency operation, high product purity, small selenylation agent use amount, high seleno-polysaccharide yield, high stability and high biological value.
Description
Technical field
The invention belongs to Chinese materia medica processing technique field, relate to a kind of preparation method of selenizing polysaccharide, relate to a kind of preparation method of umbellate pore furgus selenizing polysaccharide particularly.
Background technology
Umbellate pore furgus, is commonly called as " umbellate pore furgus ", and in China, distribution is very wide.Sclerotia is one of traditional important Chinese medicine of China, and property is put down, and taste is sweet, light, promoting diuresis to eliminate damp pathogen, for dysuria, oedema, have loose bowels, be with inferior.Chemical composition contains the polyporusum bellatus, ergosterol, vitamin H etc. of similar Pachymose.Research in recent years shows, polyporusum bellatus is a kind of Nonspecific immunity stimulant, significantly can strengthen the cytophagous function of reticuloendothelial system, is that the growth of cancer cells is suppressed; American scientist is affected large quantity research, thinks that umbellate pore furgus is a kind of Chinese medicine of AIDS virus resisting.According to phone predicts, umbellate pore furgus will become one of focus medicinal material in the coming years.
Polyporusum bellatus is one of main active ingredient of umbellate pore furgus, has very high nutrition, medical treatment, health value, and along with the raising of living standards of the people and the enhancing of health care consciousness, polyporusum bellatus product development and application are subject to the favor of people more and more.
Selenium is the trace element of needed by human, and polyporusum bellatus has significant biological activity, the very low selenium of the polysaccharide selenium content extracted from natural umbellate pore furgus, the demand of people can not be met, by manually selenium being combined with polyporusum bellatus, be easier to body absorb and utilize, the physiology of selenium and polysaccharide and pharmacological function are optimized.
CN200910162003.4 discloses a kind of method of preparing seleno-polysaccharide by organic method, the method be with fern amylose or artemisia desertorum polysaccharide for raw material, utilize a kind of selenizing reagent of selenous acid and sulfur oxychloride synthesis, a kind of method of preparation selenizing polysaccharide.CN102276753B discloses a kind of preparation method of polyporus selenium polysaccharide, and the method utilizes H
2seO
3, acetic acid makes selenylation reaction liquid, adding bariumchloride is catalyzer, preparation selenizing polyporusum bellatus.Above-mentioned patent system is comparatively large for the selenizing agent usage quantity of selenium polysaccharide, and the selenylation reaction time is longer, and selenium content is not high, and the selenizing polyporusum bellatus stability of preparation is not high, biological value is low.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, a kind of preparation method of umbellate pore furgus selenizing polysaccharide is provided, the method selenizing agent usage quantity is less, the selenylation reaction time is shorter, selenizing polysaccharide yield is higher, stability is high, biological value is high.
To achieve these goals, the present invention is achieved by the following technical solutions:
A preparation method for umbellate pore furgus selenizing polysaccharide, comprises the following steps:
(1) umbellate pore furgus Crude polysaccharides preparation
1. water extraction: select pure clean sclerotia, through microwave drying, after pulverizer is pulverized, cross 40 ~ 60 mesh sieves, add in the distilled water of 20 ~ 40 times amount, stir, supersound process 5 ~ 10min, power is 600 ~ 700W, under be neutral, temperature being the condition of 90 ~ 100 DEG C in pH, lixiviate 2.5 ~ 3.5h, filtering separation, obtains lixiviate filtrate;
2. concentrated alcohol is analysed: lixiviate filtrate 1. dropped in vacuum decker, 1/10 ~ 1/4 of simmer down to original volume, adds dehydrated alcohol in concentrated solution, make alcohol concn in mixed solution be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, precipitating thing is dry, obtained umbellate pore furgus Crude polysaccharides, for subsequent use;
(2) umbellate pore furgus Crude polysaccharides purifying
1. removal of impurities: by (1)-2. gained umbellate pore furgus Crude polysaccharides add in the distilled water of 6 ~ 10 times amount, centrifugal 10 ~ 20min, removes a small amount of insolubles; Collect clear liquid, drip 2% tan-liquor of reduction of feed volume 1.5% ~ 3% while stirring wherein, boil 10 ~ 15min, isolating protein; Add the sugar decoloration active carbon of reduction of feed volume 1.5% ~ 3%, stir evenly, decolouring 10 ~ 15min, filtered while hot, obtains destainer;
2. enzymolysis crosses post: under the condition of 45 DEG C ~ 55 DEG C, adds the papoid of decolouring liquid measure 1.5% ~ 3%, enzymolysis 30 ~ 45min in destainer, rapid temperature increases to 98 DEG C goes out enzyme, and insulation 10 ~ 15min, is cooled to room temperature, centrifugal 5 ~ 10min, removing anaenzyme, obtains clear liquid; Getting clear liquid adds in 20% ~ 30% ethanol hot solution of 2 ~ 4 times amount, by neutral alumina purification column, detect polysaccharide elution peak, collect elutriant, add dehydrated alcohol, alcohol concn in mixed solution is made to be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, precipitating thing evaporation drying, obtained polyporusum bellatus sterling, for subsequent use;
(3) umbellate pore furgus holosaccharide selenizing
1. tube-nursery: utilize selenous acid and sulfur oxychloride synthesis selenium content be 2 ~ 4% containing seleno reagent oxychlorination selenium;
2. selenylation reaction: quantitatively take (2)-umbellate pore furgus holosaccharide some grams 2., add dry pyridine 3.5 ~ 5.5ml/g, stir, then oxychlorination selenium 0.8 ~ 1.5ml/g is instilled, bariumchloride 0.1 ~ 0.3g/g, sodium nitrate solution 0.5 ~ the 0.8ml/g of mass concentration 3 ~ 4.5% is added after abundant stirring, at normal temperatures, selenylation reaction 8 ~ 10h, then the acetic acid 3 ~ 4.5ml/g adding mass concentration 1 ~ 1.5%, stir 4.5 ~ 5.5h, add dehydrated alcohol, make alcohol concn in mixed solution be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, obtains precipitating thing;
3. to dialyse drying: after dissolving precipitating thing with distilled water, dialysis 6 ~ 8h; Detect without barium ion to dialyzate, then analyse dialyzate with dehydrated alcohol alcohol, pelleting centrifugation, vacuum freezing, dry with tetracol phenixin, obtain Powdered umbellate pore furgus selenizing polysaccharide.
Described step (1)-1. in, a kind of optimal technical scheme is: clean umbellate pore furgus is ground into 60 orders, and add in the distilled water of 30 times amount, stir, supersound process 8min, power is 650W, under be neutral, temperature being the condition of 95 DEG C in pH, lixiviate 3h.
Described step (1)-2. in, a kind of optimal technical scheme is: 1/5 of stoste simmer down to original volume, adds dehydrated alcohol, makes alcohol concn in mixed solution be 75%, leave standstill 10h.
Described step (2)-1. in, a kind of optimal technical scheme is: umbellate pore furgus Crude polysaccharides adds in the distilled water of 8 times amount, centrifugal 15min; Collect clear liquid, drip 2% tan-liquor of reduction of feed volume 2% while stirring wherein, boil 12min; Add the sugar decoloration active carbon of reduction of feed volume 2%, stir evenly, decolouring 12min.
Described step (2)-2. in, a kind of optimal technical scheme is: under the condition of 50 DEG C, adds the papoid of 2.5%, enzymolysis 40min in destainer, and rapid temperature increases to 98 DEG C goes out enzyme, and insulation 12min, is cooled to room temperature, centrifugal 8min; Getting clear liquid adds in 25% ethanol hot solution of 3 times amount, by neutral alumina purification column, detects polysaccharide elution peak, collects elutriant, add dehydrated alcohol, make alcohol concn in mixed solution be 75%, leave standstill 10h.
Described step (3)-1. in, a kind of optimal technical scheme is: synthesis selenium content be 3% containing seleno reagent oxychlorination selenium.
Described step (3)-2. in, a kind of optimal technical scheme is: quantitatively take (2)-umbellate pore furgus holosaccharide some grams 2., add dry pyridine 4.5ml/g, stir, then instill oxychlorination selenium 1ml/g, bariumchloride 0.2g/g, the sodium nitrate solution 0.6ml/g of mass concentration 4% is added after abundant stirring, at normal temperatures, selenylation reaction 9h, then the acetic acid 4ml/g adding mass concentration 1.2%, stir 5h, add dehydrated alcohol, make alcohol concn in mixed solution be 75%, leave standstill 10h.
Described step (3)-3. in, a kind of optimal technical scheme is: dialyse after dissolving precipitating thing with distilled water 7h.
Described step (3)-2. in, dry pyridine is the initiator of selenylation reaction, and bariumchloride is the catalyzer of selenylation reaction, and sodium nitrate solution is the chemical stabilizer of umbellate pore furgus selenizing polysaccharide.
The invention has the beneficial effects as follows: compared with prior art, the present invention is prepared into the preparation of selenizing polysaccharide from umbellate pore furgus Crude polysaccharides, efficiently swift to operate, product purity is high, and selenizing agent usage quantity is less, the selenylation reaction time is shorter, selenizing polysaccharide yield is higher, stability is high, biological value is high.
Embodiment
In conjunction with the embodiments and corresponding detected result further the present invention is set forth, be not construed as limiting the invention.
Embodiment 1
Prepared by umbellate pore furgus Crude polysaccharides: select pure clean sclerotia, take 1kg, through microwave drying, after pulverizer is pulverized, cross 40 mesh sieves, add in the distilled water of 20L, stir, supersound process 5min, power is 600W, under be neutral, temperature being the condition of 90 DEG C in pH, lixiviate 2.5h, filtering separation, drops into lixiviate filtrate in vacuum decker, simmer down to 2L, adds 4.7L dehydrated alcohol in concentrated solution, leave standstill 8h, centrifugation, precipitating thing is dry, obtains umbellate pore furgus Crude polysaccharides 312.4g.
Umbellate pore furgus Crude polysaccharides purifying: gained umbellate pore furgus Crude polysaccharides is added in the distilled water of 1.9L, centrifugal 10min, collect clear liquid, drip 2% tan-liquor 28.5ml while stirring wherein, boil 10min, add the sugar decoloration active carbon of 28.5g, stir evenly, decolouring 10min, filtered while hot, under the condition of 45 DEG C, the papoid of 28.5g is added in destainer, enzymolysis 30min, rapid temperature increases to 98 DEG C goes out enzyme, insulation 10min, be cooled to room temperature, centrifugal 5min, getting clear liquid adds in the 20% ethanol hot solution of 3.8L, by neutral alumina purification column, detect polysaccharide elution peak, collect elutriant, add dehydrated alcohol, alcohol concn in mixed solution is made to be 70%, leave standstill 8h, centrifugation, precipitating thing evaporation drying, obtain umbellate pore furgus holosaccharide 203.7g.
Umbellate pore furgus holosaccharide selenizing: added in 713ml dry pyridine by 203.7g umbellate pore furgus holosaccharide, stir, then instills the oxychlorination selenium 163ml of selenium content 2%, bariumchloride 20.4g, adds the sodium nitrate solution 101.9ml of mass concentration 3%, at normal temperatures after fully stirring, selenylation reaction 8h, add the acetic acid 611.1ml of mass concentration 1% again, stir 4.5h, add 3.7L dehydrated alcohol, alcohol concn in mixed solution is made to be 70%, leave standstill 8h, centrifugation, obtains precipitating thing; After dissolving precipitating thing with distilled water, dialysis 6h; Detect without barium ion to dialyzate, then analyse dialyzate with dehydrated alcohol alcohol, pelleting centrifugation, vacuum freezing, dry with tetracol phenixin, obtain Powdered umbellate pore furgus selenizing polysaccharide 237.1g.
Embodiment 2
Prepared by umbellate pore furgus Crude polysaccharides: select pure clean sclerotia, take 1kg, through microwave drying, after pulverizer is pulverized, cross 60 mesh sieves, add in the distilled water of 30L, stir, supersound process 8min, power is 650W, under be neutral, temperature being the condition of 95 DEG C in pH, lixiviate 3h, filtering separation, lixiviate filtrate is dropped in vacuum decker, simmer down to 6L, adds 18L dehydrated alcohol in concentrated solution, make alcohol concn in mixed solution be 75%, leave standstill 10h, centrifugation, precipitating thing is dry, obtains umbellate pore furgus Crude polysaccharides 331.6g.
Umbellate pore furgus Crude polysaccharides purifying: gained umbellate pore furgus Crude polysaccharides is added in the distilled water of 2.7L, centrifugal 15min, collect clear liquid, drip 2% tan-liquor 54ml while stirring wherein, boil 12min, add the sugar decoloration active carbon of 54g, stir evenly, decolouring 12min, filtered while hot, under the condition of 50 DEG C, the papoid of 68g is added in destainer, enzymolysis 40min, rapid temperature increases to 98 DEG C goes out enzyme, insulation 12min, be cooled to room temperature, centrifugal 8min, getting clear liquid adds in 20% ethanol hot solution of 2 times amount, by neutral alumina purification column, detect polysaccharide elution peak, collect elutriant, add dehydrated alcohol, alcohol concn in mixed solution is made to be 75%, leave standstill 10h, centrifugation, precipitating thing evaporation drying, obtain umbellate pore furgus holosaccharide 221.7g.
Umbellate pore furgus holosaccharide selenizing: added in 997.6ml dry pyridine by 221.7g umbellate pore furgus holosaccharide, stir, then instills the oxychlorination selenium 221.7ml of selenium content 3%, bariumchloride 44.3g, adds the sodium nitrate solution 133ml of mass concentration 4%, at normal temperatures after fully stirring, selenylation reaction 9h, add the acetic acid 886.8ml of mass concentration 1.2% again, stir 5h, add 6.7L dehydrated alcohol, alcohol concn in mixed solution is made to be 75%, leave standstill 10h, centrifugation, obtains precipitating thing; After dissolving precipitating thing with distilled water, dialysis 7h; Detect without barium ion to dialyzate, then analyse dialyzate with dehydrated alcohol alcohol, pelleting centrifugation, vacuum freezing, dry with tetracol phenixin, obtain Powdered umbellate pore furgus selenizing polysaccharide 259.8g.
Embodiment 3
Prepared by umbellate pore furgus Crude polysaccharides: select pure clean sclerotia, take 1kg, through microwave drying, after pulverizer is pulverized, cross 80 mesh sieves, add in the distilled water of 40L, stir, supersound process 10min, power is 700W, under be neutral, temperature being the condition of 100 DEG C in pH, and lixiviate 3.5h, filtering separation, obtains lixiviate filtrate; Lixiviate filtrate dropped in vacuum decker, simmer down to 10L, adds 40L dehydrated alcohol in concentrated solution, make alcohol concn in mixed solution be 80%, leaves standstill 10h, centrifugation, and precipitating thing is dry, obtains umbellate pore furgus Crude polysaccharides 324.3g.
Umbellate pore furgus Crude polysaccharides purifying: gained umbellate pore furgus Crude polysaccharides is added in the distilled water of 3.2L, centrifugal 20min, collect clear liquid, drip 2% tan-liquor 96ml while stirring wherein, boil 15min, add the sugar decoloration active carbon of 96g, stir evenly, decolouring 15min, filtered while hot, under the condition of 55 DEG C, the papoid of 96g is added in destainer, enzymolysis 45min, rapid temperature increases to 98 DEG C goes out enzyme, insulation 15min, be cooled to room temperature, centrifugal 10min, getting clear liquid adds in 20% ethanol hot solution of 4 times amount, by neutral alumina purification column, detect polysaccharide elution peak, collect elutriant, add dehydrated alcohol, alcohol concn in mixed solution is made to be 80%, leave standstill 12h, centrifugation, precipitating thing evaporation drying, obtain umbellate pore furgus holosaccharide 214.2g.
Umbellate pore furgus holosaccharide selenizing: added in 1178.1ml dry pyridine by 214.2g umbellate pore furgus holosaccharide, stir, then instills the oxychlorination selenium 321.3ml of selenium content 4%, bariumchloride 64.3g, adds the sodium nitrate solution 171.4ml of mass concentration 4.5%, at normal temperatures after fully stirring, selenylation reaction 10h, add the acetic acid 963.9ml of mass concentration 1.5% again, stir 5.5h, add 10.5L dehydrated alcohol, alcohol concn in mixed solution is made to be 80%, leave standstill 12h, centrifugation, obtains precipitating thing; After dissolving precipitating thing with distilled water, dialysis 8h; Detect without barium ion to dialyzate, then analyse dialyzate with dehydrated alcohol alcohol, pelleting centrifugation, vacuum freezing, dry with tetracol phenixin, obtain Powdered umbellate pore furgus selenizing polysaccharide 250.2g.
The selenium content of above-described embodiment 1 ~ 3 in fluorescence spectrometry the finished product umbellate pore furgus selenizing polysaccharide, concrete outcome is as shown in the table:
The detected result display of upper table:
1, in the present invention, every kilogram of umbellate pore furgus raw material oxychlorination seleno reagent used is not more than 221.7ml, and the umbellate pore furgus selenizing polysaccharide yield of umbellate pore furgus raw material is not less than 23.7%, and in every gram of umbellate pore furgus selenizing polysaccharide, selenium content is at least 27790ug.
2, in the present invention, the embodiment 2 utilizing preferred implementation condition to carry out has higher umbellate pore furgus selenizing polysaccharide yield.
Claims (8)
1. a preparation method for umbellate pore furgus selenizing polysaccharide, is characterized in that: comprise the following steps:
(1) umbellate pore furgus Crude polysaccharides preparation
1. water extraction: select pure clean sclerotia, through microwave drying, after pulverizer is pulverized, cross 40 ~ 60 mesh sieves, add in the distilled water of 20 ~ 40 times amount, stir, supersound process 5 ~ 10min, power is 600 ~ 700W, under be neutral, temperature being the condition of 90 ~ 100 DEG C in pH, lixiviate 2.5 ~ 3.5h, filtering separation, obtains lixiviate filtrate;
2. concentrated alcohol is analysed: lixiviate filtrate 1. dropped in vacuum decker, 1/10 ~ 1/4 of simmer down to original volume, adds dehydrated alcohol in concentrated solution, make alcohol concn in mixed solution be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, precipitating thing is dry, obtained umbellate pore furgus Crude polysaccharides, for subsequent use;
(2) umbellate pore furgus Crude polysaccharides purifying
1. removal of impurities: by (1)-2. gained umbellate pore furgus Crude polysaccharides add in the distilled water of 6 ~ 10 times amount, centrifugal 10 ~ 20min, removes a small amount of insolubles; Collect clear liquid, drip 2% tan-liquor of reduction of feed volume 1.5% ~ 3% while stirring wherein, boil 10 ~ 15min, isolating protein; Add the sugar decoloration active carbon of reduction of feed volume 1.5% ~ 3%, stir evenly, decolouring 10 ~ 15min, filtered while hot, obtains destainer;
2. enzymolysis crosses post: under the condition of 45 DEG C ~ 55 DEG C, adds the papoid of decolouring liquid measure 1.5% ~ 3%, enzymolysis 30 ~ 45min in destainer, rapid temperature increases to 98 DEG C goes out enzyme, and insulation 10 ~ 15min, is cooled to room temperature, centrifugal 5 ~ 10min, removing anaenzyme, obtains clear liquid; Getting clear liquid adds in 20% ~ 30% ethanol hot solution of 2 ~ 4 times amount, by neutral alumina purification column, detect polysaccharide elution peak, collect elutriant, add dehydrated alcohol, alcohol concn in mixed solution is made to be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, precipitating thing evaporation drying, obtained polyporusum bellatus sterling, for subsequent use;
(3) umbellate pore furgus holosaccharide selenizing
1. tube-nursery: utilize selenous acid and sulfur oxychloride synthesis selenium content be 2 ~ 4% containing seleno reagent oxychlorination selenium;
2. selenylation reaction: quantitatively take (2)-umbellate pore furgus holosaccharide some grams 2., add dry pyridine 3.5 ~ 5.5ml/g, stir, then oxychlorination selenium 0.8 ~ 1.5ml/g is instilled, bariumchloride 0.1 ~ 0.3g/g, sodium nitrate solution 0.5 ~ the 0.8ml/g of mass concentration 3 ~ 4.5% is added after abundant stirring, at normal temperatures, selenylation reaction 8 ~ 10h, then the acetic acid 3 ~ 4.5ml/g adding mass concentration 1 ~ 1.5%, stir 4.5 ~ 5.5h, add dehydrated alcohol, make alcohol concn in mixed solution be 70% ~ 80%, leave standstill 8 ~ 12h, centrifugation, obtains precipitating thing;
3. to dialyse drying: after dissolving precipitating thing with distilled water, dialysis 6 ~ 8h; Detect without barium ion to dialyzate, then analyse dialyzate with dehydrated alcohol alcohol, pelleting centrifugation, vacuum freezing, dry with tetracol phenixin, obtain Powdered umbellate pore furgus selenizing polysaccharide.
2. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, it is characterized in that: described step (1)-1. in clean umbellate pore furgus be ground into 60 orders, add in the distilled water of 30 times amount, stir, supersound process 8min, power is 650W, under be neutral, temperature being the condition of 95 DEG C in pH, and lixiviate 3h.
3. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, is characterized in that: described step (1)-2. in stoste simmer down to original volume 1/5, add dehydrated alcohol, make alcohol concn in mixed solution be 75%, leave standstill 10h.
4. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, is characterized in that: described step (2)-1. in umbellate pore furgus Crude polysaccharides add in the distilled water of 8 times amount, centrifugal 15min; Collect clear liquid, drip 2% tan-liquor of reduction of feed volume 2% while stirring wherein, boil 12min; Add the sugar decoloration active carbon of reduction of feed volume 2%, stir evenly, decolouring 12min.
5. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, is characterized in that: described step (2)-2. in destainer, under the condition of 50 DEG C, add the papoid of 2.5%, enzymolysis 40min, rapid temperature increases to 98 DEG C goes out enzyme, insulation 12min, is cooled to room temperature, centrifugal 8min; Getting clear liquid adds in 25% ethanol hot solution of 3 times amount, by neutral alumina purification column, detects polysaccharide elution peak, collects elutriant, add dehydrated alcohol, make alcohol concn in mixed solution be 75%, leave standstill 10h.
6. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, is characterized in that: described step (3)-1. in synthesis containing seleno reagent oxychlorination selenium selenium content is 3%.
7. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, it is characterized in that: described step (3)-2. in, quantitatively take (2)-umbellate pore furgus holosaccharide some grams 2., add dry pyridine 4.5ml/g, stir, then oxychlorination selenium 1ml/g is instilled, bariumchloride 0.2g/g, adds the sodium nitrate solution of mass concentration 4%, at normal temperatures after fully stirring, selenylation reaction 9h, add the acetic acid 25ml/g of mass concentration 1.2% again, stir 5h, add dehydrated alcohol, make alcohol concn in mixed solution be 75%, leave standstill 10h.
8. the preparation method of a kind of umbellate pore furgus selenizing polysaccharide as claimed in claim 1, is characterized in that: described step (3)-3. in dissolve precipitating thing with distilled water after to dialyse 7h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859910A (en) * | 2016-01-07 | 2016-08-17 | 浙江海洋学院 | Method for preparing selenized oligomeric aminopolysaccharide |
| WO2020000788A1 (en) * | 2018-06-26 | 2020-01-02 | 爱美中科硒科技（天津）有限公司 | Esterified selenium polysaccharide and preparation method and use therefor |
-
2014
- 2014-05-26 CN CN201410226150.4A patent/CN105199007A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859910A (en) * | 2016-01-07 | 2016-08-17 | 浙江海洋学院 | Method for preparing selenized oligomeric aminopolysaccharide |
| CN105859910B (en) * | 2016-01-07 | 2020-12-29 | 浙江海洋学院 | Preparation method of selenized oligomeric amino polysaccharide |
| WO2020000788A1 (en) * | 2018-06-26 | 2020-01-02 | 爱美中科硒科技（天津）有限公司 | Esterified selenium polysaccharide and preparation method and use therefor |
| US11345761B2 (en) | 2018-06-26 | 2022-05-31 | Ai-May Zhong Ke Selenium Technology (Tianjin) Co., Ltd | Esterified selenium polysaccharide and preparation method and use therefor |
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Application publication date: 20151230 |