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Preparation method of novel nanometer micelle medicinal material

A nanomicelle, a new type of technology, applied in the field of biopolymer material synthesis, can solve the problems of inability to achieve scale and industrialization, and achieve the effect of convenient operation, strong controllability, and industrialization

Active Publication Date: 2015-10-07
SHANXI KANGBAO BIOLOGICAL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problem of the inability to achieve large-scale and industrialization in the preparation of polyethylene glycol-b-polylactic acid diblock copolymer micelles with small particle size (<30nm) and small molecular weight (3000-3400)) problem, and provides a new preparation method of nano-micelle medicinal material

Method used

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  • Preparation method of novel nanometer micelle medicinal material
  • Preparation method of novel nanometer micelle medicinal material
  • Preparation method of novel nanometer micelle medicinal material

Examples

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Effect test

Embodiment 1

[0031] A preparation method of a novel nano-micelle medicinal material:

[0032] (1) Add 700 g of polyethylene glycol monomethyl ether (1800-2200) into a dry 2L three-neck round bottom flask (equipped with a ground three-way valve), install mechanical stirring, and seal the stirring and bottle stopper well. One end of the three-way valve is connected to a safety bottle and then connected to a vacuum pump. The safety bottle must be in liquid nitrogen, and one end is connected to nitrogen gas; then put it in an oil bath, and the boundary of the oil bath should reach 2 / 3 of the neck of the flask; turn the three-way valve to the vacuum position , 110°C to remove water under reduced pressure for 6 hours, and the pressure is lower than -0.085MPa; under the protection of nitrogen, add the catalyst stannous octoate (2.072g dissolved in 1.1ml toluene), and vacuumize for 0.5h; under the protection of nitrogen, add D, L-propane Lactide 520g, under nitrogen protection, reacted at 135°...

Embodiment 2

[0040] A preparation method of a novel nano-micelle medicinal material:

[0041] (1) Put polyethylene glycol monomethyl ether with a molecular weight of 1800-2200 in an oil bath, heat to 110°C-115°C, vacuumize for 6 hours, and then add the catalyst stannous salt compound dissolved in toluene under nitrogen protection (Dissolve 1g of stannous salt with 0.4mL of toluene), then add D, L-lactide (the weight ratio of polyethylene glycol monomethyl ether to D, L-lactide is 44:56), the The amount of stannous salt compound is reactant D, 4‰-5‰ of the weight of L-lactide, heated under nitrogen protection, the reaction temperature is 130°C-135°C, the reaction time is 14h, and cooled;

[0042] (2) Dissolve the product of step (1) in dichloromethane (the volume of dichloromethane is 1 times the weight of D, L-lactide), and slowly add it dropwise to ether (the volume of anhydrous ether is D , 10 times the weight of L-lactide), stirred, precipitated at a temperature below 10°C, and filt...

Embodiment 3

[0046] A preparation method of a novel nano-micelle medicinal material:

[0047] (1) Put polyethylene glycol monomethyl ether with a molecular weight of 1800-2200 in an oil bath, heat to 110°C-115°C, vacuumize for 8 hours, and then add the catalyst stannous salt compound dissolved in toluene under nitrogen protection (dissolve 1g of stannous salt with 0.5mL of toluene), then add D, L-lactide (the weight ratio of polyethylene glycol monomethyl ether to D, L-lactide is 58:56), the The amount of stannous salt compound is 4‰-5‰ of the weight of reactant D, L-lactide, and the reaction is carried out by heating under the protection of nitrogen. The reaction temperature is 130°C-135°C, the reaction time is 16h, and then cooled;

[0048] (2) Dissolve the product of step (1) in dichloromethane (the volume of dichloromethane is 1.2 times the weight of D, L-lactide), and slowly add it dropwise to ether (the volume of anhydrous ether is D , 15 times the weight of L-lactide), stirred, ...

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Abstract

The invention discloses a preparation method of novel nanometer micelle medicinal material, and belongs to the field of biomacromolecule material synthesis, and realizes large scale production and industrialization in preparation of polyethylene glycol-b-polylactic acid diblock copolymer micelle of small particle size and small molecular weight. The method provided by the invention comprises the following steps: (1) placing polyethylene glycol monomethyl ether whose molecular weight is between 1800 and 2200 in an oil bath, performing heating and vacuuming, adding a catalyst tin salt compound, adding D,L-lactide, carrying out a heating reaction, and performing cooling; (2) dissolving the resultants of the step (1) in dichloromethane, and slowly adding the mixture into ether, performing stirring and precipitating, carrying out a pumping filtration, obtaining a light yellow solid, and performing drying and obtaining a finished product polyethylene glycol monomethyl ether-polylactic acid mPEG-b-PDLLA diblock amphiphilic copolymer. According to the invention, routine reaction apparatuses are used for reaching to a pilot scale, thereby facilitating operation with controllability, meeting the requirements for medicinal preparation production of a large scale, and realizing industrialization.

Description

technical field [0001] The invention belongs to the field of synthesis of biopolymer materials, and relates to a novel nano-micelle medicinal material, in particular to a medium of polyethylene glycol monomethyl ether-polylactic acid (mPEG-b-PDLLA) diblock amphiphilic copolymer. Test-scale preparation method. Background technique [0002] In recent years, with the development of combinatorial chemistry and high-throughput screening technology, the newly discovered drug candidate compounds have increased dramatically, but 70% of them are insoluble in water; at the same time, most of the anti-tumor drugs in clinical application are hydrophobic drugs, therefore, How to improve the water solubility of insoluble drugs, further improve drug bioavailability, reduce toxic and side effects, and achieve clinical efficacy has always been the research focus of new drug delivery systems, especially the solubilization technology of amphiphilic block copolymers has attracted much atten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G65/332A61K47/34A61K9/107
Inventor 周满祥
Owner SHANXI KANGBAO BIOLOGICAL PROD
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