CN103613741A - Preparation method of PLGA (Polylacticcoglycollic Acid) microparticle for changing monomer sequence - Google Patents
Preparation method of PLGA (Polylacticcoglycollic Acid) microparticle for changing monomer sequence Download PDFInfo
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- CN103613741A CN103613741A CN201310586181.6A CN201310586181A CN103613741A CN 103613741 A CN103613741 A CN 103613741A CN 201310586181 A CN201310586181 A CN 201310586181A CN 103613741 A CN103613741 A CN 103613741A
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Abstract
The invention relates to a preparation method of a PLGA (Polylacticcoglycollic Acid) microparticle for changing a monomer sequence. The preparation method is used for preparing a sequentially arranged PLGA copolymer by using a repetitive sequence PLGA copolymer through steps such as dissolving and precipitating, re-emulsifying and stirring, and washing. The sequentially arranged PLGA copolymer disclosed by the invention can affect degradation rate, so that the degradation rate is slower and more stable; and moreover, prospect in controlling drug release and a degradable surgical operation suture line is wide.
Description
Technical field
The present invention relates to the preparation of PLGA micron particle, relate in particular to a kind of preparation method who changes the PLGA micron particle of monomer sequence.
Background technology
The multipolymer of occurring in nature can be arranged and be realized controlled structure, catalytic performance and adjustable material property by the order of the monomer to relatively limited.In natural silk, crystalline part ((GlyAlaGlyAlaGlySer)
n) and the amorphous portion based on amino acid whose carrying side group be alternately to exist, thereby orderly order is to have interim crosslinked action to give the principal element that the antiparallel β of a mechanical property-sheet forms, and in prior art, by the method for simplifying sequence, prepares synthetic analogue.
The not synthetic multipolymer with pin-point accuracy sequential control in prior art, protein be a kind of aspect three (composition, tacticity and structural order) can realize the complex body that microstructure is controlled.And most synthetic polymer is relatively simple, even microstructure that can fine control, as a rule poly(lactic acid), still can not show high structural complexity, because it only contains a kind of monomer, although high structural complexity can obtain, from same system, the example of acquisition order-property relationship but lacks very much, except the material based on peptide, the research major part of order and property relationship all obtains from oligomeric folded formation.
PLGA is that a class can obtain by sequential control the polymkeric substance of useful performance.PLGA is prototype biodegradability polymkeric substance, and it can obtain from recyclability resource, and degraded do not need special enzyme, be that itself or hydrolysate are all nontoxic.At random, the PLGA of lack of alignment is for controlling the important component part of the implanted device that drug release and degradable surgical sewing thread and human body can absorb.In these application, be the absorption of graft or the degradation rate that drug release rate all depends on PLGA.Controlling the degradation rate of PLGA normally realizes by changing the ratio of ratio, control molecular weight or racemize and the three-dimensional poly(lactic acid) unit of lactic acid-glycol acid, the monomer sequence that changes multipolymer makes it from becoming at random in order, can control its degradation rate, the application of this respect is considerably less at present.
Summary of the invention
The present invention relates to a kind of for studying the preparation of monomer sequence on the PLGA micron particle of the impact of biodegradability poly(lactic acid)-ethylene glycol tumor-necrosis factor glycoproteins segmented copolymer hydrolysis.
Preparation process is as follows:
(1) PLGA's is synthetic: the analogue (R-SAP50) synthetic and random alignment of tumor-necrosis factor glycoproteins PLGA multipolymer is all used the preparation of SAP method, then the monomer of equivalent and 4-dimethylamino pyridine-p-tosylate (DPTS) combination are dissolved in methylene dichloride, make the solution of 15wt%, solution is cooled to after 0 ℃, 1,3-di-isopropyl carbodiimide (DIC, 17.1g, 136mmol) dropwise join in solution and at room temperature stir 2h, with methanol extraction out, filtration final vacuum is dried and obtains white sample the product obtaining.
(2) methylene dichloride (4mL) high speed agitator for solution (8000~10000rpm) of the preparation of PLGA micron particle: PLGA (200mg) is at polyvinyl alcohol (PVA, 50~80mL, 2~5%w/v) in solution, emulsification forms emulsion, emulsion joins in 80~120mLPVA solution (1~3%w/v) and stirs 3~10h to evaporate methylene dichloride, the centrifugal deionized water wash of out then using three times of microparticle, lyophilize 36~72h is to remove remaining solvent again, and the micron particle preparing is stored in moisture eliminator.
Order PLGA multipolymer prepared by the present invention, compares with random alignment multipolymer, can affect degradation rate, obtains more slowly and discharges.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with specific embodiment, the present invention is described in further detail.
(1) PLGA's is synthetic: the synthetic of tumor-necrosis factor glycoproteins PLGA multipolymer prepared by SAP method.The analogue of random alignment (R-SAP50) is also with the preparation of SAP method: by the monomer (0.34g of equivalent, 2.26mol) then combination is dissolved in methylene dichloride with 4-dimethylamino pyridine-p-tosylate (DPTS), makes the solution of 15wt%; Solution is cooled to after 0 ℃, and 1,3-di-isopropyl carbodiimide (DIC, 17.1g, 136mmol) dropwise joins in solution and at room temperature stirs 2h, and with methanol extraction out, filtration final vacuum is dried and obtains white sample the product obtaining.
(2) methylene dichloride (4mL) high speed agitator for solution (10000rpm) of the preparation of PLGA micron particle: PLGA (200mg) is at polyvinyl alcohol (PVA, 60mL, 2%w/v) in solution, emulsification forms emulsion, then emulsion joins in 80mLPVA solution (1%w/v) and stirs 3h to evaporate methylene dichloride, the centrifugal deionized water wash of out then using three times of microparticle, lyophilize 36h is to remove remaining solvent again, and the micron particle preparing is stored in moisture eliminator.
Claims (2)
1. change the preparation method of the PLGA micron particle of monomer sequence, its step is as follows:
(1) PLGA's is synthetic:
The analogue (R-SAP50) synthetic and random alignment of tumor-necrosis factor glycoproteins PLGA multipolymer is all used the preparation of SAP method, then the monomer of equivalent and 4-dimethylamino pyridine-p-tosylate (DPTS) combination are dissolved in methylene dichloride, make the solution of 15wt%, solution is cooled to after 0 ℃, 1,3-di-isopropyl carbodiimide (DIC, 17.1g, 136mmol) dropwise join in solution and at room temperature stir 2h, with methanol extraction out, filtration final vacuum is dried and obtains white sample the product obtaining;
(2) preparation of PLGA micron particle:
Methylene dichloride (4mL) high speed agitator for solution (8000~10000rpm) of PLGA (200mg) is at polyvinyl alcohol (PVA, 50~80mL, 2~5%w/v) emulsification in solution, emulsion joins in 80~120mLPVA solution (1~3%w/v) and stirs 3~10h to evaporate methylene dichloride, the centrifugal deionized water wash of out then using three times of microparticle, lyophilize 36~72h is to remove remaining solvent again, and the micron particle preparing is stored in moisture eliminator.
2. micron particle preparation method as claimed in claim 1, is characterized in that: the stir speed (S.S.) of described high speed agitator is 10000rpm.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102295765A (en) * | 2011-06-30 | 2011-12-28 | 南京大学 | Copolycondensation synthesized polylactic acid-glycollic acid catalyzed by biomass creatinine |
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102295765A (en) * | 2011-06-30 | 2011-12-28 | 南京大学 | Copolycondensation synthesized polylactic acid-glycollic acid catalyzed by biomass creatinine |
Non-Patent Citations (1)
Title |
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LI J.: "THE DEPENDENCE OF DEGRADATION AND RELEASE BEHAVIOR OF POLYESTERS ON MONOMER SEQUENCE", 《DISSERTATION&THESES》 * |
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Application publication date: 20140305 |