Preparation method of nano starch particle reinforced aldehyde-hydrazine crosslinking type injectable poly(N-isopropylacrylamide) (PNIPAM) hydrogel
A cross-linked, hydrogel technology, which is applied in the direction of medical preparations with non-active ingredients, medical preparations containing active ingredients, and pharmaceutical formulations, can solve the problems of poor gel strength, stability, and poor degradation performance. Achieve the effect of strength improvement and good application prospect
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[0026] The preparation method of the precursor is:
[0027] (1) Using AIBN as the initiator and ethanol as the solvent, the poly-(NIPAM-co-AA) copolymer was prepared by free radical polymerization, and then ADH was used to react with -COOH in the poly-(NIPAM-co-AA) copolymer Introducing -NHNH in the side chain 2 Preparation of poly-(NIPAM-co-AA)-hdz copolymer precursor.
[0028] (2) Utilizing the oxidizing property of sodium periodate on the vicinal hydroxyl group to oxidize the vicinal hydroxyl group on the polysaccharide into the vicinal aldehyde group to prepare the precursor of the aldylated polysaccharide. The polysaccharide is dextrin, carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, alginate or hyaluronic acid.
[0029] (3) The preparation method of SNPs quotes the method of the inverse microemulsion in the reference document [1] of background technology part, is oil phase with toluene and chloroform, and 10wt% starch aqueous solution is water p...
Embodiment 1
[0031](1) Preparation of Poly(NIPAM-co-AA) copolymer: A copolymer of NIPAM and AA was synthesized by free radical polymerization. The reactants NIPAM (8.0g), AA (2.0g) and initiator AIBN (0.45g) were added to 80mL of absolute ethanol, nitrogen gas was passed for 2h, and the reaction was carried out at 55±1°C for 12h. Then the reaction product was diluted with deionized water, and then the diluted polymer solution was dialyzed six times with a 12-14KDa MWCO dialysis membrane for a total duration of not less than three days. The dialyzed solution was freeze-dried. A poly(NIPAM-co-AA) copolymer is obtained. GPC measurement results showed that the molecular weight was 19100 g / mol, and the molecular weight distribution was 2.0.
[0032] (2) Preparation of Poly(NIPAM-co-AA)-hdz copolymer: by adding adipic acid dihydrazide (1.87g) into the poly(NIPAM-co-AA) copolymer aqueous solution of 0.65wt% / vol , adding 1.0mol / L of HCl to adjust the pH of the solution to 4.75. Then EDC coupli...
Embodiment 2
[0037] Steps (1) to (4) are identical with embodiment 1;
[0038] (5) Preparation of SNPs reinforced 9.0wt% hydrogel: formaldehyde dextrin into 9.0wt% polymer aqueous solution, add SNPs into the formaldehyde dextrin solution to prepare SNPs content of 0.5-4.0wt% suspension. The poly-(NIPAM-co-AA)-hdz copolymer was formulated as an aqueous polymer solution with a polymer content of 9.0 wt%. Then, an equal volume of hydrazide solution, aldehyddextrin and SNPs suspension were mixed and extruded to obtain a 9.0 wt% hydrazine cross-linked injectable PNIPAM hydrogel reinforced by SNPs. It can be seen from the scanning electron microscope that the hydrogel dried by supercritical carbon dioxide has a porous three-dimensional network structure with an average pore size of 38.40 nm, and the hydrogel starch nanoparticles reinforced by SNPs are uniformly dispersed in the hydrogel. in the network structure.
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