CN107022039A - A kind of new method that liquaemin is prepared by raw material of chitterlings - Google Patents
A kind of new method that liquaemin is prepared by raw material of chitterlings Download PDFInfo
- Publication number
- CN107022039A CN107022039A CN201710452495.5A CN201710452495A CN107022039A CN 107022039 A CN107022039 A CN 107022039A CN 201710452495 A CN201710452495 A CN 201710452495A CN 107022039 A CN107022039 A CN 107022039A
- Authority
- CN
- China
- Prior art keywords
- resin
- liquaemin
- filtrate
- butane
- time
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08B37/0063—Glycosaminoglycans or mucopolysaccharides, e.g. keratan sulfate; Derivatives thereof, e.g. fucoidan
- C08B37/0075—Heparin; Heparan sulfate; Derivatives thereof, e.g. heparosan; Purification or extraction methods thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is using chitterlings as raw material, pass through the collection of pig intestinal mucosa liquid, digest (salt solution), filter residue, resin adsorption, butane equipment extraction element under liquid gas biphase equilibrium state is passed through to the resin for having adsorbed liquaemin, using butane as solvent, principle using liquaemin insoluble in butane, washing, which is removed, is attached to lipid material and impurity that the liquaemin being adsorbed in resin surface layer and resin is wrapped, ensure liquaemin from the elution in resin, the consummate degree of liquaemin is improved, the yield of liquaemin is improved.
Description
Technical field
The invention belongs to biology extraction, purification preparation technology field, and in particular to one kind is passed through using chitterlings for raw material
Butane under enzymolysis or salt solution, extraction and application liquid gas biphase equilibrium state carries out extraction cleaning and degreasing class and impurity and enters to advance again
Refined heparin sodium is made in the purifying of one step.
Background technology
The current main source of heparin is chitterlings, and international market is very powerful to the demand of heparin bulk drug, its medicine
Function is mainly：The sowing property intravascular coagulation early stage of various diseases concurrently, prevention artery and vein thrombus and pulmonary embolism are treated, is
The maximum anticoagulation medicine of most effective in the world and quantity.Traditional heparin sodium is main from the extraction preparation method in chitterlings
It is：The technical process such as chitterlings knifing, mucous membrane collection, enzymolysis, filter residue, resin adsorption, dry elution, alcohol precipitation, dry is deposited
Its top layer makes liquaemin be difficult to elute by lipid or impurity parcel after because of resin adsorption liquaemin, and contains a certain amount of lipid
Material and impurity, have impact on quality and efficiency.This technology carries out degreasing class and miscellaneous using the butane under liquid gas biphase equilibrium state
The preparation method of matter improves the consummate degree of liquaemin, improves the yield of liquaemin.
The content of the invention
Pass through enzymolysis or salt solution, extraction and application liquid gas two using chitterlings for raw material it is an object of the invention to provide one kind
Butane under the state that balances each other carries out extraction cleaning and degreasing class and impurity and obtained refined heparin sodium is further purified again
Method.
The present invention preparation method be：Under certain condition, make butane equal in liquid gas two by the control to pressure, temperature
Weighing apparatus state；And lipid and impurity are removed as extraction, cleaning solvent, specific method is as follows：Using chitterlings as raw material, pass through pig
The collection of mucous membrane of small intestine liquid, enzymolysis (salt solution), filter residue, resin adsorption are equal by liquid gas two to the resin that has adsorbed liquaemin
Butane equipment extraction element under weighing apparatus state, using butane as solvent, the principle using liquaemin insoluble in butane, washing removes attached
Lipid material and impurity that the liquaemin being adsorbed in resin surface layer and resin is wrapped, have ensured liquaemin from washing in resin
It is de-, the consummate degree of liquaemin is improved, the yield of liquaemin is improved.
The preparation method of the present invention follows these steps what is carried out：
(1), the mucous membrane of fresh chitterlings is scraped, pig intestinal mucosa liquid is collected, this pig intestinal mucosa liquid is transferred to enzyme
Solve in tank and to adjust pH value to 8.5--9.5 with sodium hydroxide solution, then add into pig intestinal mucosa liquid protease, and will enzymolysis
Tank is warming up to 45-50 DEG C, is incubated 3 hours, and insulation is finished adjusts pH value 9- by intestinal mucosa liquid sodium hydroxide solution in enzymatic vessel
9.5,60 DEG C are warming up to, 1 hour is incubated.Wherein, the dosage of protease is mucous membrane obtained by every chitterlings plus protease is 2-3
Gram.
(2), insulation finishes the pig intestinal mucosa liquid 90-100 mesh nylon bag filtrations after enzymolysis.(it can use and be centrifuged at a high speed
One kind in the diversified forms such as filtering, suction filtration, press filtration) collect filtrate filtrate is transferred in resin adsorption tank, add it is processed
Good liquaemin absorption is resin dedicated, (resin dosage is the 20% of filtrate), turn on agitator, mixing speed be 60-70 turn/
When, absorption overall process about 6-7 hours filters out resin with 90-100 mesh nylon leaching nets, resin is drained, is transferred to liquid gas two-phase
In degreasing class device, the butane for being passed through liquefied is washed to resin, is 1-1.5 hours to the control of resin wash time.
(3) after washing is finished, the butane degreasing class device under liquid gas biphase equilibrium state is in the state of butane is drained
Resin is taken out, resin is washed with 1.2 times of 5% dilute sodium chloride aqueous solution, about 10-20 minutes time, drained after washing.Will
Resin after scrubbed is eluted with the sodium-chloride water solution of 18%-20% concentration, and elution is carried out in three times：For the first time to set
1.2-2 times of fat volume measures submergence resin, about 4 hours time；Submergence resin is measured for 1.2-1.5 times with resin volume for the second time,
About 2 hours time；Third time is with 1.2 times of amount submergence resins of resin volume, about 1 hour time.
(4) three eluents in combining step (3), adjust pH value to 10-12 eluent, stand 10- with sodium hydrate aqueous solution
24 hours, eluent is filtered, remove filtrate after impurity and be transferred in settling tank, PH is adjusted with hydrochloric acid solution in settling tank
It is worth to 7-7.5,
(5) it is 45%-50% (about with filtrate into 1 containing concentration of alcohol that 95% alcohol is added in the filtrate of settling tank to filtrate：1
Dosage), stirring stands closing precipitation after 5-10 minutes, staticly settle suction after 24 hours and remove top ethanol solution, collect precipitation
Thing, is refined heparin sodium after drying.
Preparation method proposed by the present invention is after resin adsorption liquaemin to select resin with traditional preparation methods difference
Butane is cleaned, and eliminates the lipid material and impurity of resin surface and inside, while also having eluted adsorbed heparin
The lipid material and impurity of sodium institute adhesive tape, have ensured that finishing operations are not washed caused by resin is by lipids blocking from resin
The difficulty of de- liquaemin.Purity to the liquaemin after elution is further improved.
Butane in the present invention under liquid gas biphase equilibrium state, which removes the application of lipid and debris during liquaemin is prepared, to be added
The fast speed eluted from resin, lifts the yield unit of liquaemin, improves the quality purity of heparin sodium product.
Fig. 1 is a kind of flow chart that liquaemin technique is prepared by raw material of chitterlings
Fig. 2 is the butane washing degreasing removal of impurity process schematic under liquid gas biphase equilibrium state
Embodiment
The mucous membrane of fresh chitterlings is scraped, pig intestinal mucosa liquid is collected.
The pig intestinal mucosa liquid being collected into is transferred in enzymatic vessel and adjusts pH value to 8.5. with sodium hydroxide solution
Protease is added in [0005] pig intestinal mucosa liquid, and enzymatic vessel is warming up to 45-50 DEG C, 3 hours are incubated.
The dosage of protease adds 2000-3000 grams of protease by every 1000 intestinal mucosas scraped in [0006],
Mucous membrane obtained by every chitterlings adds protease to be 2-3 grams.
Insulation is finished adjusts pH value 9-9.5 by intestinal mucosa liquid sodium hydroxide solution in enzymatic vessel, is warming up to 60 DEG C, insulation 1
Individual hour.
The pig intestinal mucosa liquid 90-100 mesh nylon bag filtrations after enzymolysis are finished by being incubated.(can be using high speed centrifugation point
From one kind in the diversified forms such as filtering, suction filtration, press filtration)
Collect filtrate filtrate is transferred in resin adsorption tank.
Processed good liquaemin is added in resin adsorption tank and adsorbs resin dedicated, resin dosage is the 20% of filtrate.
Turn on agitator, mixing speed be 60-70 turn/when.
Adsorb overall process about 6-7 hours.
Resin is filtered out with 90-100 mesh nylon leaching nets.
Resin is drained.
The resin drained is transferred in liquid gas two-phase degreasing class device, the butane for being passed through liquefied is washed to resin
Wash.
The dissolution of resin and debris is dissolved the lipid material and impurity that are attached to resin outer layer by butane,
The lipid material and impurity of the liquaemin entrained with that resin endoporus is adsorbed also have been eluted simultaneously.Improve liquaemin yield.
It it is 1-1.5 hours to resin wash time.
After washing is finished, butane degreasing class device under liquid gas biphase equilibrium state in butane drain in the state of take
Go out resin.
Resin will be taken out to be washed with 1.2 times of 5% dilute sodium chloride aqueous solution, about 10-20 minutes time, dripped after washing
It is dry.
Resin after scrubbed drain is eluted with the sodium-chloride water solution of 18%-20% concentration, carried out in three times：
Submergence resin, about 4 hours time are measured with 1.2-2 times of resin volume for the first time；Measured for the second time for 1.2-1.5 times with resin volume
Submerge resin, about 2 hours time；Third time is with 1.2 times of amount submergence resins of resin volume, about 1 hour time.
Three eluents during merging is above-mentioned, adjust pH value to 10-12 eluent, stand 10- with sodium hydrate aqueous solution
24 hours.
Eluent is filtered (or being separated with supercentrifuge, 3600 revs/min -4000 revs/min, 20 minutes), removed
Filtrate is transferred in settling tank after impurity.PH value is adjusted to 7-7.5 with hydrochloric acid solution in settling tank.
It is 45%-50% (about with filtrate into 1 containing concentration of alcohol that 95% alcohol is added in the filtrate of settling tank to filtrate：1
Dosage), stirring stands closing precipitation after 5-10 minutes.
Staticly settle suction after 24 hours and remove top ethanol solution, collect sediment, be refined heparin sodium after drying.
Claims (2)
1. a kind of new method that liquaemin is prepared by raw material of chitterlings, it is characterised in that：Using the tree to having adsorbed liquaemin
Fat is by the butane equipment extracting method under liquid gas biphase equilibrium state, and its preparation method follows these steps what is carried out：
(1), the mucous membrane of fresh chitterlings is scraped, pig intestinal mucosa liquid is collected, this pig intestinal mucosa liquid is transferred to enzyme
Solve in tank and to adjust pH value to 8.5--9.5 with sodium hydroxide solution, then add into pig intestinal mucosa liquid protease, and will enzymolysis
Tank is warming up to 45-50 DEG C, is incubated 3 hours, and insulation is finished adjusts pH value 9- by intestinal mucosa liquid sodium hydroxide solution in enzymatic vessel
9.5,60 DEG C are warming up to, 1 hour is incubated.
(2), insulation finishes the pig intestinal mucosa liquid 90-100 mesh nylon bag filtrations after enzymolysis.(it can use and be centrifuged at a high speed
One kind in the diversified forms such as filtering, suction filtration, press filtration) collect filtrate filtrate is transferred in resin adsorption tank, add it is processed
Good liquaemin adsorbs resin dedicated, turn on agitator, mixing speed be 60-70 turn/when, absorption overall process about 6-7 hour, use
90-100 mesh nylon leaching nets filter out resin, and resin is drained, and are transferred in liquid gas two-phase degreasing class device, are passed through liquefied
Butane is washed to resin, is 1-1.5 hours to the control of resin wash time.
(3) after washing is finished, the butane degreasing class device under liquid gas biphase equilibrium state is in the state of butane is drained
Resin is taken out, resin is washed with 1.2 times of 5% dilute sodium chloride aqueous solution, about 10-20 minutes time, drained after washing, will
Resin after scrubbed is eluted with the sodium-chloride water solution of 18%-20% concentration, and elution is carried out in three times：For the first time to set
1.2-2 times of fat volume measures submergence resin, about 4 hours time；Submergence resin is measured for 1.2-1.5 times with resin volume for the second time,
About 2 hours time；Third time is with 1.2 times of amount submergence resins of resin volume, about 1 hour time
(4) three eluents in combining step (3), adjust pH value to 10-12 eluent, stand 10- with sodium hydrate aqueous solution
24 hours, eluent is filtered, remove filtrate after impurity and be transferred in settling tank, PH is adjusted with hydrochloric acid solution in settling tank
It is worth to 7-7.5,
(5) it is 45%-50% (about with filtrate into 1 containing concentration of alcohol that 95% alcohol is added in the filtrate of settling tank to filtrate：1
Dosage), stirring stands closing precipitation after 5-10 minutes, staticly settle suction after 24 hours and remove top ethanol solution, collect precipitation
Thing, is refined heparin sodium after drying.
2. the new method of liquaemin according to claim 1, it is characterised in that：The dosage of protease is every chitterlings institute
Obtaining mucous membrane adds protease to be 2-3 grams；Resin dosage is the 20% of filtrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710452495.5A CN107022039A (en) | 2017-06-15 | 2017-06-15 | A kind of new method that liquaemin is prepared by raw material of chitterlings |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710452495.5A CN107022039A (en) | 2017-06-15 | 2017-06-15 | A kind of new method that liquaemin is prepared by raw material of chitterlings |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107022039A true CN107022039A (en) | 2017-08-08 |
Family
ID=59531609
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710452495.5A Pending CN107022039A (en) | 2017-06-15 | 2017-06-15 | A kind of new method that liquaemin is prepared by raw material of chitterlings |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107022039A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293801A (en) * | 2018-09-19 | 2019-02-01 | 浙江土畜凯兴畜产有限公司 | A method of heparin sodium is prepared by raw material of chitterlings |
| CN110229252A (en) * | 2019-06-25 | 2019-09-13 | 广元市海天实业有限责任公司 | A kind of processing technology improving refined heparin sodium yield |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229681A (en) * | 2011-06-22 | 2011-11-02 | 郓城绅联生物科技有限公司 | Preparation method for producing heparin sodium by using porcine small intestines |
| CN103755837A (en) * | 2013-11-25 | 2014-04-30 | 青岛九龙生物医药有限公司 | Method for preparing heparin sodium by utilizing small intestines of pigs |
| CN103834470A (en) * | 2014-03-04 | 2014-06-04 | 秦广雍 | Method for extracting macadamia nut oil by adopting subcritical extraction technology |
| KR101447123B1 (en) * | 2014-02-27 | 2014-10-06 | 박상협 | Extraction Method of Heparin |
| CN104945539A (en) * | 2015-07-17 | 2015-09-30 | 大英县添峰生物制品有限公司 | Energy-saving low-temperature heparin sodium extraction technology |
-
2017
- 2017-06-15 CN CN201710452495.5A patent/CN107022039A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229681A (en) * | 2011-06-22 | 2011-11-02 | 郓城绅联生物科技有限公司 | Preparation method for producing heparin sodium by using porcine small intestines |
| CN103755837A (en) * | 2013-11-25 | 2014-04-30 | 青岛九龙生物医药有限公司 | Method for preparing heparin sodium by utilizing small intestines of pigs |
| KR101447123B1 (en) * | 2014-02-27 | 2014-10-06 | 박상협 | Extraction Method of Heparin |
| CN103834470A (en) * | 2014-03-04 | 2014-06-04 | 秦广雍 | Method for extracting macadamia nut oil by adopting subcritical extraction technology |
| CN104945539A (en) * | 2015-07-17 | 2015-09-30 | 大英县添峰生物制品有限公司 | Energy-saving low-temperature heparin sodium extraction technology |
Non-Patent Citations (1)
| Title |
|---|
| 杨公明，程玉来 主编: "《食品机械与设备》", 31 May 2015, 中国农业大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293801A (en) * | 2018-09-19 | 2019-02-01 | 浙江土畜凯兴畜产有限公司 | A method of heparin sodium is prepared by raw material of chitterlings |
| CN110229252A (en) * | 2019-06-25 | 2019-09-13 | 广元市海天实业有限责任公司 | A kind of processing technology improving refined heparin sodium yield |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102212149B (en) | Preparation process for extracting crude sodium heparin from pig lungs | |
| CN102351956B (en) | Extraction method of morindea officinalis polysaccharide | |
| CN110437197B (en) | Method for extracting anthocyanin from sphenoidea | |
| CN103214595B (en) | The preparation method of Sodium chondroitin sulfate A | |
| CN107022039A (en) | A kind of new method that liquaemin is prepared by raw material of chitterlings | |
| CN101230106B (en) | Preparation method of banana polysaccharide | |
| CN107056966A (en) | A kind of process for purification of liquaemin | |
| JP6353522B2 (en) | Method for separating and purifying recombinant human lactoferrin from rice seed | |
| CN108610391A (en) | A method of extracting polysaccharide and adenosine from Phellinus fructification | |
| CN108864224B (en) | Separation and purification method of malvidin-3-O-arabinoside and application thereof | |
| CN102180985A (en) | Method for extracting and purifying mugwort polysaccharides | |
| CN103936846B (en) | A kind of purification process of protamine sulfate | |
| CN101817884A (en) | Method for extracting narrow-leaved oleaster polysaccharide | |
| CN104045725A (en) | Method for refining inonotus obliquus crude polysaccharide by adopting D301G anion resin | |
| CN109293801A (en) | A method of heparin sodium is prepared by raw material of chitterlings | |
| CN101792394B (en) | Extraction separation method of L-synephrine | |
| CN109384861A (en) | A kind of method of heparin sodium pulp thickening dermatan sulfate | |
| CN107641161A (en) | A kind of optimal reparation technology of casing accessory substance liquaemin | |
| CN105266075B (en) | method for extracting Stichopus japonicus saponins from Stichopus japonicus blanching liquid | |
| CN108042569A (en) | A kind of method of impurity in separation gel class Chinese medicine | |
| CN113599405A (en) | Method for comprehensively extracting multiple effective components from acanthopanax sessiliflorus fruits and application thereof | |
| CN102382152A (en) | Method for preparing salidroside | |
| CN105777922A (en) | Pilose asiabell root polysaccharide extraction method | |
| CN104031159A (en) | Method for refining inonotus obliquus crude polysaccharide by use of 732 cationic resin | |
| CN109053830A (en) | A kind of separation purifying technique extracting gentiamarin from gentianae macrophyllae |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170808 |
|
| WD01 | Invention patent application deemed withdrawn after publication |