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Method for removing residual organic solvent in polymer microsphere solvent

A technology of organic solvents and polymers, applied in the medical field, can solve the problems of high residual organic solvents and the influence of microsphere shape, etc., and achieve the effect of reducing the residual amount, accelerating the transfer amount and transfer speed

Active Publication Date: 2022-06-07
CHANGZHOU INST OF MATERIA MEDICA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The technical problem to be solved in the present invention is: to overcome the deficiencies in the prior art, to provide a method for removing organic solvent residues in polymer microsphere solvents, and to solve the problem of residual organic solvents when using previous methods to remove organic solvents in polymer microspheres. Problems that are high and affect the morphology of the microspheres

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  • Method for removing residual organic solvent in polymer microsphere solvent

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Embodiment 1

[0031] A method for removing organic solvent residues from polymer microsphere solvents, comprising the following steps:

[0032] Step S01, using dichloromethane as an organic solvent, the raw materials are polylactic acid, polyglycolic acid, polycaprolactone, poly (lactate - hydroxyacetic acid) copolymer of any one; Organic solvents and raw materials are configured into a mixture of prepared polymer microspheres;

[0033] Step S02, microsphere pre-washing: Transfer the configured polymer microsphere mixture to a beaker of 5 L, add 4 L of purified water, stir at 500 rpm at 25 °C for 1 h to transfer the organic solvent in the solution to water, centrifuge and discard the supernatant after washing, collect the microspheres, repeat the water washing process 2 times;

[0034] Step S03, microsphere hot water washing: then add 4L of purified water to the pre-washed polymer microspheres, and then add a certain concentration of anti-aggregation agent solution, anti-aggregation agent using...

Embodiment 2

[0038] A method for removing organic solvent residues from polymer microsphere solvents, comprising the following steps:

[0039] Step S01, using dichloromethane as an organic solvent, the raw materials are polylactic acid, polyglycolic acid, polycaprolactone, poly (lactate - hydroxyacetic acid) copolymer of any one; Organic solvents and raw materials are configured into a mixture of prepared polymer microspheres;

[0040] Step S02, microsphere pre-washing: Transfer the emulsified polymer microsphere mixture to a beaker of 5 L, add 5 L of purified water, stir at 500 rpm at 25 °C for 2h to transfer the organic solvent in the solution to water, centrifuge and discard the supernatant after the end of the wash, collect the microspheres, and repeat the pre-wash process 5 times.

[0041] Step S03, microsphere hot water washing: add 5L of purified water to the washed polymer microspheres, and then add a certain concentration of anti-aggregation agent solution, anti-aggregation agent usin...

Embodiment 3

[0046] A method for removing organic solvent residues from polymer microsphere solvents, comprising the following steps:

[0047] Step S01, ethyl acetate is used as an organic solvent, and the raw material is a poly (lactate - hydroxyacetic acid) copolymer; Organic solvents and raw materials are configured into a mixture of prepared polymer microspheres;

[0048] Step S02, microsphere pre-washing: Transfer the emulsified polymer microsphere mixture to a beaker of 5 L, add 4 L of purified water, stir at 500 rpm at 25 °C for 1h to transfer the organic solvent in the solution to water, centrifuge and discard the supernatant after the end of the wash, collect the beads, and repeat the pre-wash process 3 times.

[0049] Step S03, microsphere hot water washing: then add 4L of purified water to the pre-washed polymer microspheres, and then add a certain concentration of anti-aggregation agent solution, anti-aggregation agent using polyvinyl alcohol, formulated into 1% polyvinyl alcohol sol...

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Abstract

The present invention relates to a method for removing residual organic solvents in polymer microsphere solvents, comprising the following steps: step S01, preparing a polymer microsphere mixed solution; step S02, pre-washing the microspheres, and repeating the washing process for 2 to 5 times, so that Most of the organic solvent in the polymer microspheres is transferred to water; step S03, after the hot water washing, the polymer microsphere mixture is cooled to 20-25°C, and then centrifuged, the supernatant is discarded, and the microspheres are collected; Step S03 is repeated 5 to 6 times; Step S04, wash the microspheres with cold water: stir for 1 to 2 h to wash away the polyvinyl alcohol in the polymer microsphere solution, and collect the microspheres; Step S04 is repeated 10 to 15 times; Step S05, the The polymer microspheres were freeze-dried and subpackaged. Through pre-washing, hot water washing and cold water washing, multiple washings work together to effectively remove the organic solvent residue in the microspheres.

Description

Technical field [0001] The present invention relates to the medical field, specifically to a method of removing organic solvent residues from polymer microsphere solvents. Background [0002] Polymer microspheres refer to polymer materials or polymer composites with a diameter of nano to microns and shaped as spherical or other geometric bodies. Compared with inorganic material microspheres, polymer microspheres have the advantages of easy purification and separation, low price, large specific surface area, good monodispersity, easy preparation and functionalization, and adjustable compatibility with living organisms, which is conducive to the study of the interaction of biological components. Therefore, it is widely used in the field of biomedical materials and has become an indispensable material in biochemistry, pharmacy and medicine. [0003] Microspheres prepared from synthetic degradable materials represented by polymers, polycaprolactones and polyglycolic acid have been wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K9/16A61K47/32A61K47/42A61J3/00
CPCA61K9/1682A61K47/32A61K47/42A61J3/00
Inventor 张谦朱莲葛佳佳管汉亮耿文鑫李立文
Owner CHANGZHOU INST OF MATERIA MEDICA
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