Method for preparing heparinoid polysaccharide
A technology of heparin and polysaccharides, applied in the field of medical polymers, can solve the problems of difficulty, influence, and comparison of anticoagulant activity
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Embodiment 1
[0018] Disperse 20g of chitin powder (usually commercially available chitin is sufficient, in the embodiment of the present invention, 60 mesh chitin with a degree of deacetylation of 9%) is dispersed into 200ml of phosphoric acid with a concentration of 85%, and stirred until the chitin After all is dissolved, add this solution to 4000ml of distilled water, stir quickly while adding, precipitate white gelatinous chitin, centrifuge to remove water, wash with distilled water to neutrality, and obtain acid-treated product. Disperse the acid-treated product in 1000ml of distilled water, stir under ice-water bath conditions, add 240mg Tempo and 8g NaBr to completely dissolve Tempo and NaBr, then add 480ml of 4% NaClO solution, continue to add 0.5M NaOH solution dropwise to make the reaction During the process, the pH value of the solution was stabilized at 10.8, reacted for 1 hour, then 50ml ethanol was added, the pH value was adjusted to neutral with 2M acetic acid, the solution wa...
Embodiment 2
[0021] Disperse 5g chitin powder (60 mesh, deacetylation degree 15%) in 90ml 65% phosphoric acid, stir until all the chitin is dissolved, add this solution to 300ml distilled water, stir quickly while adding, and precipitate white gum After the chitin is formed, the water is removed by centrifugal separation, and the precipitate is washed with distilled water to neutrality to obtain the acid-treated product. Disperse the acid-treated product in 150ml distilled water, stir under ice-water bath conditions, add 75mg Tempo and 1.5g NaBr to completely dissolve Tempo and NaBr, then add 40ml 10% NaClO solution, and continue to add 2M KOH solution dropwise to make During the reaction, the pH value of the solution stabilized at 9.6, reacted for 0.5h, and then added 10ml of methanol, adjusted the pH value to neutral with 4M HCl, the solution was purified by ultrafiltration, concentrated by distillation under reduced pressure, precipitated with acetone, and dried in vacuum to obtain 6-posi...
Embodiment 3
[0024] Disperse 2g of chitin powder (60 mesh, deacetylation degree 15%) in 38ml of 70wt% phosphoric acid, stir until all the chitin is dissolved, add this solution to 200ml of distilled water, stir quickly while adding, and precipitate white gum After the shape of chitin is centrifuged to remove water, it is washed with distilled water to neutrality to obtain an acid-treated product. Disperse the acid-treated product in 50ml of distilled water, stir under ice-water bath conditions, add 16mg Tempo and 0.8g NaBr to completely dissolve Tempo and NaBr, then add 16ml of 8% NaClO solution, and continue to add 2M Na 2 CO 3 The solution makes the pH of the solution 10.0 during the reaction, react for 0.5h, add 4.5ml of ethanol, adjust the pH to neutral with 3M phosphoric acid, dialyze the solution against distilled water for 72h, concentrate by distillation under reduced pressure, precipitate with anhydrous methanol, and dry in vacuum The 6-position selective oxidation reaction product ...
PUM
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