CN106432535A - Cooperative medicament level sodium alginate and alginate-originated oligosaccharide technological method - Google Patents
Cooperative medicament level sodium alginate and alginate-originated oligosaccharide technological method Download PDFInfo
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- CN106432535A CN106432535A CN201610827477.6A CN201610827477A CN106432535A CN 106432535 A CN106432535 A CN 106432535A CN 201610827477 A CN201610827477 A CN 201610827477A CN 106432535 A CN106432535 A CN 106432535A
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- algin
- oligosaccharide
- pharmaceutical grade
- coproduction
- alginate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
Abstract
The application discloses cooperative medicament level sodium alginate and alginate-originated oligosaccharide technological method, wherein the provided steps include taking dry sodium alginate and leaching, digesting, diluting, foaming, floating, and primary fine filtrating, and resulting in clear solution C, exploiting soda solution and regulating pH, adding activated charcoal in the clear solution C and tarnishing through absorption, then fine filtrating two stage through a closed frame filter and paper board filter, conducting weight metal absorption of the filtrating solution through ion exchange resin, and resulting in clear solution F, acidifying, dewatering, rinsing the clear solution F, partially degrading and decomposing by adding lyase, centrifugally separating undissolved acid block, solid neutralizing to result in medicament level sodium alginate, mist spray drying the filtration solution and resulting in alginate-originated oligosaccharide. The composite yield of the two types of products is high, the weight metal content of sodium alginate is low, the endotoxin is low, the weight metal content of alginate-originated oligosaccharide is low, the cooperative medicament level sodium alginate and alginate-originated oligosaccharide technological method satisfies applications in cosmetic industry.
Description
Technical field
The invention belongs to seaweed chemical technical field is and in particular to one kind being capable of coproduction pharmaceutical grade algin and algin widow
The process of sugar.
Background technology
Algin is a kind of material made for raw material extracts separation with brown alga, for white or pale yellow powder.Brown alga
Glue is by the mannuronic acid of different proportion（M）And guluronic acid（G）Composition, M/G ratio is usually determined by raw material,
The ratio of the M/G of bulk kelp preparation is 0.842-1.66, and the algin M/G ratio of sea-tangle preparation is 2.15-2.35.And M/G ratio
The gel that higher alginate product is formed is softer, more meets the demand in market, but lot of documents shows, change at present
The ratio becoming M/G is often to sacrifice raw material yield as cost.In addition, current part pharmaceutical grade algin requires low endotoxin, low
Heavy metal, low viscosity.And algin Adsorption of Heavy Metals itself is very capable, the end product of existing algin production technology
Content of beary metal higher it is impossible to meet the use standard of pharmaceutical grade algin.
Algin oligosaccharide is algin the degree of polymerization obtaining is less and the low molecular weight fraction of good water solubility through hydrolyzing, brown alga
Glue oligosaccharides has multiple physiologically actives, can be widely applied to medicine and cosmetic field, has huge Development volue.
Content of the invention
The invention provides the process of a kind of coproduction pharmaceutical grade algin and algin oligosaccharide, receive not reducing raw material
On the premise of rate, a kind of prepared M/G ratio is higher and meets low endotoxin, low-heavy metal content, low viscous pharmaceutical grade brown alga
Glue, co-production obtains algin oligosaccharide.
To achieve these goals, the present invention is achieved using following technical proposals：
A kind of coproduction pharmaceutical grade algin and the technique of algin oligosaccharide, step is：Dry brown alga process is soaked, digests, diluting,
After foaming floating first time refined filtration, obtain clear liquid C, adjust pH using aqueous slkali, add activated carbon to carry out decolouring in clear liquid C and inhale
Attached, then through closed flame filter press and cardboard filter two-stage refined filtration, filtrate carries out heavy metal by ion exchange resin
Absorption, obtains clear liquid F, after clear liquid F being carried out be acidified, be dehydrated, washing, plus the cracking of lyases part, uncracked acid block through from
The heart separates, and solid neutralization obtains pharmaceutical grade algin, and filtrate is spray-dried to obtain algin oligosaccharide.
Further, described digestion is by the brown alga after cleaning, and puts in digestion reactor, adds water, and stirring is lower to be added
Salt carries out digestion reaction, and amount of water is 2-5 with the mass ratio of dry brown alga:1, salt is 10-20 with the mass ratio of dry brown alga:100, disappear
Change reaction temperature and be 50-70 DEG C, the reaction time is 2.5-3.5h.
Further, described first time refined filtration is first through centrifuge coarse filtration after foaming floating, adds diatomite, diatom
The native mass ratio with dry brown alga is 10-30:100, use plate and frame filter press press filtration.
In order to fully remove the endotoxin in removing glue liquid, charcoal absorption is taken to add the side of cardboard filter refined filtration twin-stage removal
Method, described activated carbon is 20-50 with the mass ratio of dry brown alga:100, described granularity of activated carbon is less than 200 mesh.
In order to ensure adsorbing be smoothed out, and do not destroy gelatin viscosity, the temperature using charcoal absorption is 40-
70 DEG C, stirring insulation 40-60min.
In order to ensure the adsorption effect of heavy metal, it is 9-11 that described clear liquid C uses NaOH solution to adjust pH.
Further, described ion exchange resin is polystyrene schiff bases chelating resin or Na type ion exchange resin.
Further, described lyases is guluronic acid lyases.
In order to realize the part cracking to algin, the addition of described guluronic acid lyases is the 5%- of dry brown alga
20%, the enzyme activity of described guluronic acid lyases is 20unit/mL.
In order to crack generation algin oligosaccharide, improve the M/G ratio of not cleaved algin simultaneously, plus cracking enzymatic lysis
Alignic 1/3.
Compared with prior art, advantages of the present invention and good effect are：The present invention takes full advantage of brown alga raw material coproduction
Obtain pharmaceutical grade algin and algin oligosaccharide, initially with charcoal absorption and closed flame filter press, cardboard filter
Two-stage removes the endotoxin in removing glue liquid, then adopts ion exchange resin to reduce the content of heavy metal in algin, finally adopts
Enzymolysis part alginic acid block, thus improve the ratio of pharmaceutical grade algin M/G.Two kinds of product comprehensive yield are high, algin weight
Tenor is low, and endotoxin is low, and algin oligosaccharide content of beary metal is low, can meet the application of cosmetic industry.
Brief description
Fig. 1. the product process flow figure of the present invention.
Specific embodiment
With reference to specific embodiment, technical scheme is described in further detail.
The present embodiment is related to the technique of a kind of coproduction pharmaceutical grade algin and algin oligosaccharide, and step is：By dry brown alga warp
After crossing immersion, digestion, dilution, foaming floating first time refined filtration, obtain clear liquid C, adjust pH using NaOH solution, to clear liquid C
Middle addition activated carbon carries out decolorization adsorption, and then through closed flame filter press and cardboard filter two-stage refined filtration, filtrate is passed through
Ion exchange resin carries out heavy metal adsorption, obtains clear liquid F, after clear liquid F being carried out be acidified, be dehydrated, washing, plus lyases part
Degraded, undissolved acid block is centrifuged, and solid neutralization obtains pharmaceutical grade algin, and filtrate is spray-dried to obtain algin
Oligosaccharides.
The present embodiment takes full advantage of brown alga raw material coproduction and obtains pharmaceutical grade algin and algin oligosaccharide, initially with work
Property charcoal absorption and closed flame filter press, the cardboard filter two-stage endotoxin that goes in removing glue liquid, then adjust glue pH, adopt
Adsorb the content reducing heavy metal in algin with ion exchange resin, finally using enzymolysis part alginic acid block, thus improve doctor
The ratio of medicine level algin M/G.Two kinds of product comprehensive yield are high, and algin content of beary metal is low, and endotoxin is low, algin oligosaccharide
Content of beary metal is low, can meet the application of cosmetic industry.
Specifically operating procedure is：
1）Take dry brown alga, amount of water is 10-20cm3/g（VWater/mBrown alga）, be soaked in water under normal temperature 2-5h, so that brown alga is fully soaked molten
Swollen, it is cut into the strip of 4-8cm after control water with vegetable-chopper, wash 3-5 time, wash away silt and the salt on sea-tangle surface.
2）Brown alga after cleaning, puts in digestion reactor, adds water, and stirring is lower to add salt to carry out digestion reaction, makes not
The alginate of dissolubility generates soluble alginate with reactant salt；Described amount of water is 2-5 with the mass ratio of dry brown alga:1,
Described salt is 10-20 with the mass ratio of dry brown alga:100, described salt can be sodium carbonate or sodium fluoride.Control digestion reaction temperature
For 50-70 DEG C, insulation reaction 2.5-3.5h, using mechanical system, sea-tangle is broken into sticky state, obtains brown alga digestion glue
Liquid A.
3）In step 2）Water dilution is added, being diluted with water to Engler degree is 120-180 in the brown alga digestion glue A obtaining
Second, using compressed air, glue is foamed, after foaming, floating standing 1-3h, obtains glue liquid B.
4）By step 3）The glue liquid B obtaining, after centrifuge coarse filtration, adds diatomite as filter aid, diatomite is brown with dry
The mass ratio of algae is 10-30:100, use plate and frame filter press press filtration, filter off insoluble material in solution, obtain clear liquid C, use
It is 9-11 that NaOH adjusts pH.
5）Add activated carbon in clear liquid C, activated carbon is 20-50 with the mass ratio of dry brown alga:100, described activated carbon grain
Degree is less than 200 mesh, at 40-70 DEG C, stirring insulation 40-60min, and temperature is too high, then destroy gelatin viscosity, and temperature is too low, then
It is unfavorable for adsorbing.Using the endotoxin in charcoal absorption glue, obtain clear liquid D.
6）Clear liquid D is carried out initial filter through closed flame filter press, then carries out refined filtration through cardboard filter, through two-stage
It is filtered to remove the activated carbon of absorption, and endotoxin is removed further by refined filtration, obtain clear liquid E.
7）Clear liquid E is passed through ion exchange resin, removes the most of heavy metal in clear liquid, obtain clear liquid F.In order to ensure weight
The adsorption effect of metal, before clear liquid E passes through ion exchange resin, namely in step 4）Middle regulation pH is 9-11.Described ion
Exchanger resin is polystyrene schiff bases chelating resin or Na type ion exchange resin.
8）Add the acid solution that mass percent concentration is 10% in clear liquid F, the sodium alginate acidifying in clear liquid obtains
To alginic acid solid, after draining, plus pure water stirring and washing, proceed to squeezer after draining again, alginic acid is carried out press dewatering
It is less than 70% to moisture content, obtain alginic acid G.Described acid solution can be sulfuric acid solution or hydrochloric acid solution.
9）The pure water of 1-1.2 times of quality is added in alginic acid G, plus the gulose being equivalent to the 5%-20% of dry sea-tangle quality
Aldehydic acid lyases（Enzyme activity 20unit/mL）, after stirring 1.5-2.5h, alginic acid is digested 1/3 about.
The present embodiment carries out Partial digestion, described guluronic acid lyases using guluronic acid lyases to alginic acid
By the part guluronic acid in algin（G）It is degraded to algin oligosaccharide, therefore can get two kinds of products, improve and do not split
The M/G ratio of the algin of solution, improves the utilization rate of raw material, obtains a kind of algin of higher M type.
10）Alginic acid after enzymolysis is centrifuged, and obtains solid and supernatant, in solids plus in alkali and after obtain
Pharmaceutical grade algin, carries out spray drying to supernatant and obtains algin oligosaccharide.
Embodiment 1
Prepare pharmaceutical grade algin and algin oligosaccharide in the following manner：
（1）100 kilograms of dry sea-tangle, soaks 3h with the water of 1.5m, so that sea-tangle is fully soaked swelling, is cut into 5 with vegetable-chopper after control water
Centimetre bar, wash three times.
（2）Sea-tangle after cleaning, puts in digestion pot, adds 300 kilograms of running water, the lower fluorination adding 12kg of stirring
Sodium, insulation reaction 3 hours at 60 DEG C, with machinery, sea-tangle is broken into sticky state, obtains sea-tangle digestion glue.
（3）Add 10 cubic metres of water dilution in the sea-tangle digestive juice that step 2 obtains, using compressed air, glue is sent out
Bubble, floating standing 2h after foaming.
（4）The glue that step 3 is obtained, after centrifuge coarse filtration, adds 20 kilograms of diatomite, uses plate and frame filter press press filtration,
Obtain clear liquid, adjusting glue pH using NaOH is 10.
（5）30 kilograms of activated carbon is added in the clear liquid that step 4 obtains, at 50 DEG C, stirring insulation 50 minutes.
（6）After decolouring and adsorb, glue first carries out initial filter through closed flame filter press, then carries out through cardboard filter
Refined filtration, obtains clear liquid.
（7）The clear liquid that step 6 is obtained passes through Na type ion exchange resin, Adsorption heavy metal.
（8）Clear liquid after ion exchange, adds the sulfuric acid solution that percent concentration is 10% to be acidified into alginic acid, after draining,
Plus 100 kilograms of pure water stirring and washing, proceed to squeezer after draining, alginic acid squeezes dehydration moisture content 70%, obtains alginic acid 25
Kilogram.
（9）The pure water of 1 times of quality is added in the alginic acid that step 8 obtains, plus guluronic acid lyases, stir 2 little
Shi Hou, alginic acid dissolves 1/3.
（10）Alginic acid after enzymolysis is centrifuged, solid add in alkali and after obtain 16kg pharmaceutical grade algin, yield
For 16%, centrifugate is spray-dried to obtain 5kg algin oligosaccharide, and yield is 5%.
Through H-NMR analysis, in algin manufactured in the present embodiment, mannuronic acid-content is 91.8%；The ratio of M/G is
11.5/1, surveying content of beary metal in algin through Atomic absorption is 6ppm, and recording endotoxin value in algin with gel method is
100EU, surveying content of beary metal in algin oligosaccharide through Atomic absorption is 5ppm.
Embodiment 2
（1）100 kilograms of dry sea-tangle, soaks 3h with the water of 1.5m, so that sea-tangle is fully soaked swelling, is cut into 5 with vegetable-chopper after control water
Centimetre bar, wash three times.
（2）Sea-tangle after cleaning, puts in digestion pot, adds 300 kilograms of running water, the lower carbonic acid adding 15kg of stirring
Sodium, isothermal reaction 4h at 60 DEG C, with machinery, sea-tangle is broken into sticky state, obtains sea-tangle digestion glue.
（3）The water obtaining adding 10 m in sea-tangle digestive juice in step 2 dilutes, and using compressed air, glue is foamed, and sends out
Floating standing 2h after bubble.
（4）The glue that step 3 is obtained, after centrifuge coarse filtration, adds 20 kilograms of diatomite, uses plate and frame filter press press filtration,
Obtain clear liquid.
（5）50 kilograms of activated carbon is added in the clear liquid that step 4 obtains, at 50 DEG C, stirring insulation 60 minutes.
（6）After adsorbing after decolouring, glue first carries out initial filter through closed flame filter press, then carries out through cardboard filter
Refined filtration, obtains clear liquid, and adjusting glue pH using NaOH is 11.
（7）The clear liquid that step 6 is obtained passes through polystyrene schiff bases chelating resin Adsorption of Heavy Metals.
（8）The stillness of night after ion exchange, the sulfuric acid solution that percent concentration is 10% is added to be acidified into alginic acid, after draining,
Plus 100 kilograms of pure water stirring and washing, proceed to squeezer after draining, alginic acid squeezes dehydration moisture content 70%, obtains alginic acid 25
Kilogram.
（9）Alginic acid is added the pure water of 1 times of quality, plus guluronic acid lyases, after stirring 3 hours, alginic acid is molten
Take off 1/3.
（10）Alginic acid after enzymolysis after centrifugal dehydration, solid add in alkali and after obtain 15kg pharmaceutical grade algin, receive
Rate is 15%, and centrifugate is spray-dried to obtain 5.5kg algin oligosaccharide, and yield is 5.5%.
Through H-NMR analysis, in algin manufactured in the present embodiment, mannuronic acid-content is 92.3%；The ratio of M/G is
12/1, surveying content of beary metal in algin through Atomic absorption is 5ppm, and recording endotoxin value in algin with gel method is 50EU,
Surveying content of beary metal in algin oligosaccharide through Atomic absorption is 3ppm.
Above example is only several in the several preferred embodiment of the present invention it is noted that the invention is not restricted to
Above-described embodiment；For the person of ordinary skill of the art, still can be to the technical scheme described in previous embodiment
Modify, or equivalent is carried out to wherein some technical characteristics；And these modifications or replacement, do not make relevant art side
The essence of case departs from the spirit and scope of claimed technical solution of the invention.
Claims (10)
1. the technique of a kind of coproduction pharmaceutical grade algin and algin oligosaccharide is it is characterised in that step is：By dry brown alga through leaching
After bubble, digestion, dilution, foaming floating first time refined filtration, obtain clear liquid C, adjust pH using aqueous slkali, add in clear liquid C and live
Property charcoal carry out decolorization adsorption, then through closed flame filter press and cardboard filter two-stage refined filtration, filtrate pass through ion exchange
Resin carries out heavy metal adsorption, obtains clear liquid F, after clear liquid F being carried out be acidified, be dehydrated, washing, plus the cracking of lyases part, not
Cracking sour block be centrifuged, in solid with after obtain pharmaceutical grade algin, filtrate is spray-dried to obtain algin oligosaccharide.
2. the technique of coproduction pharmaceutical grade algin according to claim 1 and algin oligosaccharide is it is characterised in that described disappear
Change is the brown alga after cleaning, and puts in digestion reactor, adds water, and stirring is lower to add salt to carry out digestion reaction, amount of water with
The mass ratio of dry brown alga is 2-5:1, salt is 10-20 with the mass ratio of dry brown alga:100, digestion reaction temperature is 50-70 DEG C, instead
It is 2.5-3.5h between seasonable, described salt is sodium carbonate or sodium fluoride.
3. the technique of coproduction pharmaceutical grade algin according to claim 1 and algin oligosaccharide is it is characterised in that described
One time refined filtration is first through centrifuge coarse filtration after foaming floating, adds diatomite, and diatomite is 10- with the mass ratio of dry brown alga
30:100, use plate and frame filter press press filtration.
4. the technique of coproduction pharmaceutical grade algin according to claim 1 and algin oligosaccharide is it is characterised in that described work
Property charcoal and dry brown alga mass ratio be 20-50:100, described granularity of activated carbon is less than 200 mesh.
5. the technique of coproduction pharmaceutical grade algin according to claim 4 and algin oligosaccharide is lived it is characterised in that adopting
Property charcoal absorption temperature be 40-70 DEG C, stirring insulation 40-60min.
6. the technique of coproduction pharmaceutical grade algin according to claim 1 and algin oligosaccharide is it is characterised in that described clear
It is 9-11 that liquid C uses NaOH solution to adjust pH.
7. the technique of the coproduction pharmaceutical grade algin according to any one of claim 1-6 and algin oligosaccharide, its feature exists
In described ion exchange resin is polystyrene schiff bases chelating resin or Na type ion exchange resin.
8. the technique of the coproduction pharmaceutical grade algin according to any one of claim 1-6 and algin oligosaccharide, its feature exists
In described lyases is guluronic acid lyases.
9. the technique of coproduction pharmaceutical grade algin according to claim 8 and algin oligosaccharide is it is characterised in that described Gu
The addition of Lip river uronic acid lyases is the 5%-20% of dry brown alga, and the enzyme activity of described guluronic acid lyases is 20unit/mL.
10. the technique of coproduction pharmaceutical grade algin according to claim 2 and algin oligosaccharide is it is characterised in that plus split
Solution enzymatic lysis alignic 1/3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488687A (en) * | 2017-09-13 | 2017-12-19 | 北京雷力海洋生物新产业股份有限公司 | Alginic acid oligosaccharides prepared by a kind of enzymatic isolation method and combinations thereof and preparation method |
| CN107573441A (en) * | 2017-09-08 | 2018-01-12 | 山东省食品发酵工业研究设计院 | A kind of preparation method and application suitable for industrialized production high-purity sodium alginate |
| CN110714046A (en) * | 2019-11-22 | 2020-01-21 | 浙江丰安生物制药有限公司 | Preparation method of polypeptide for hydrolyzing pork protein of suckling pig |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423854A (en) * | 2008-12-02 | 2009-05-06 | 中国海洋大学 | Method for preparing algin oligosacchride by using algin lyase |
| CN102643882A (en) * | 2012-04-17 | 2012-08-22 | 青岛聚大洋海藻工业有限公司 | Novel process for extracting alginate-derived oligosaccharide from sea tangles by enzyme hydrolysis method |
-
2016
- 2016-09-18 CN CN201610827477.6A patent/CN106432535B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423854A (en) * | 2008-12-02 | 2009-05-06 | 中国海洋大学 | Method for preparing algin oligosacchride by using algin lyase |
| CN102643882A (en) * | 2012-04-17 | 2012-08-22 | 青岛聚大洋海藻工业有限公司 | Novel process for extracting alginate-derived oligosaccharide from sea tangles by enzyme hydrolysis method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573441A (en) * | 2017-09-08 | 2018-01-12 | 山东省食品发酵工业研究设计院 | A kind of preparation method and application suitable for industrialized production high-purity sodium alginate |
| CN107488687A (en) * | 2017-09-13 | 2017-12-19 | 北京雷力海洋生物新产业股份有限公司 | Alginic acid oligosaccharides prepared by a kind of enzymatic isolation method and combinations thereof and preparation method |
| CN110714046A (en) * | 2019-11-22 | 2020-01-21 | 浙江丰安生物制药有限公司 | Preparation method of polypeptide for hydrolyzing pork protein of suckling pig |
| CN110714046B (en) * | 2019-11-22 | 2021-06-04 | 浙江丰安生物制药有限公司 | Preparation method of polypeptide for hydrolyzing pork protein of suckling pig |
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Effective date of registration: 20190827 Address after: 266000, Mingyue Road, Huangdao District, Shandong, Qingdao 777 Patentee after: Qingdao Bright Moon Seaweed Group Co., Ltd. Address before: 266000, Mingyue Road, Huangdao District, Shandong, Qingdao 777 Patentee before: Qingdao Yue Hai Pharmaceutical Technology Co., Ltd. |
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Inventor after: Wang Fahe Inventor after: Jiang Jinju Inventor after: Zhao Hongtao Inventor after: Wang Nuansheng Inventor after: Han Jun Inventor before: Wang Fahe Inventor before: Jiang Jinju Inventor before: Zhao Hongtao Inventor before: Wang Nuansheng Inventor before: Han Jun |
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| CB03 | Change of inventor or designer information |