Polylactic acid-polyethylene glycol block copolymer-based magnetic microsphere preparation method

A technology of block copolymer and polyethylene glycol, which is applied in the field of preparation of magnetic microspheres, can solve the problems of weak magnetic response, low coating rate of magnetic polymer microspheres, uneven particle size distribution, etc., and achieve reduction Agglomeration, wide application range, smooth surface effect

Active Publication Date: 2014-08-13
磐升瑞祥(山东)生物工程股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the main technical problems of the prior art, such as low coating rate, weak magnetic response, uneven particl

Method used

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  • Polylactic acid-polyethylene glycol block copolymer-based magnetic microsphere preparation method
  • Polylactic acid-polyethylene glycol block copolymer-based magnetic microsphere preparation method
  • Polylactic acid-polyethylene glycol block copolymer-based magnetic microsphere preparation method

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Implementation example 1:

[0024] 1. Modification of magnetic ferroferric oxide

[0025] (1) Disperse 1.0 g of ferroferric oxide ultrasonically in 100 mL of deionized water, then transfer the ferroferric oxide suspension to a 250 mL three-necked flask, and use 10% hydrochloric acid solution (about 9-10 drops) Adjust the pH value of the ferroferric oxide suspension to 5.5-6.0, put it in a constant temperature water bath at 80°C while stirring (500r / min) while adding 0.15g sodium oleate, stirring for 1-1.5h, and then adding 0.05g Polyethylene glycol, continue to stir and react for 1 hour and then cool to room temperature, and then adjust the pH of the solution to 7 with 10% NaOH solution (about 5-6 drops).

[0026] (2) Put the solution on a multi-purpose magnetic analyzer for rapid solid-liquid separation, wash it with deionized water and absolute ethanol for 2 to 3 times to wash off excess oleic acid on the surface, filter with suction, and dry for later use.

[0027] 2. Prepa...

Example Embodiment

[0033] Implementation example 2:

[0034] 1. Modification of magnetic ferroferric oxide: same as above

[0035] 2. Preparation of oil-in-water emulsion

[0036] (1) Dissolve 1.0 g of polylactic acid-polyethylene glycol block copolymer (PLA-PEG-PLA) with a molecular weight of 10,000 in 15 mL of dichloromethane and acetone (V acetone / V CH2Cl2 = 1:2) In the mixed solution, add 0.1g modified ferroferric oxide, and ultrasonically disperse to obtain the oil phase;

[0037] (2) 1.0g of polyvinyl alcohol is heated at 95°C and stirred at 500r / min for 1 hour and dissolved in 100mL of deionized water to obtain an aqueous phase;

[0038] (3) Slowly add the organic phase to the water phase with stirring at room temperature. When the temperature is 60℃, use a high-speed dispersing homogenizer 12000r / min to emulsify and disperse for 3-5min to obtain an oil-in-water (O / W) emulsion. The ratio of emulsified oil to water is 1:5-1:10.

[0039] 3. Emulsification solvent volatilization process: Same as ab...

Example Embodiment

[0040] Implementation example 3:

[0041] 1. Modification of magnetic ferroferric oxide: Same as above

[0042] 2. Preparation of oil-in-water emulsion

[0043] (1) Dissolve 1.0 g of polylactic acid-polyethylene glycol block copolymer (PLA-PEG-PLA) with a molecular weight of 30000 in 20 mL of dichloromethane and acetone (V acetone / V CH2Cl2 = 1:4) the mixed solution, add 0.15 g modified ferroferric oxide, and ultrasonically disperse to obtain the oil phase;

[0044] (2) 1.0g of polyvinyl alcohol is heated at 95°C and stirred at 500r / min for 1 hour and dissolved in 100mL of deionized water to obtain an aqueous phase;

[0045] (3) Slowly add the organic phase to the water phase with stirring at room temperature. When the temperature is 60℃, use a high-speed dispersing homogenizer 12000r / min to emulsify and disperse for 3-5min to obtain an oil-in-water (O / W) emulsion. The ratio of emulsified oil to water is 1:5-1:10.

[0046] 3. Emulsification solvent volatilization process: Same as abov...

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Abstract

The invention relates to a polylactic acid-polyethylene glycol block copolymer (PLA-PEG-PLA)-based magnetic microsphere preparation method. Magnetic microspheres are prepared by adopting ferriferrous oxide (Fe3O4) as a core material and the PLA-PEG-PLA as a wall material through an emulsion solvent evaporation process. The preparation method comprises the following steps: modifying Fe3O4; dissolving the PLA-PEG-PLA in an organic solvent, adding modified Fe3O4, carrying out ultrasonic dispersion to obtain an oil phase, dissolving polyvinyl alcohol in deionized water to obtain a water phase, mixing the water phase with the oil phase, and carrying out emulsion dispersion by using a high speed dispersion homogenizer to obtain an oil-in-water O/W emulsion; and transferring the O/W emulsion to a beaker, carrying out low speed stirring until the organic solvent completely volatilizes, centrifuging, washing, carrying out pumping filtration, and carrying out vacuum drying. The preparation process is simple; and the prepared magnetic microspheres have the particle sizes of 6-8mum, and has the advantages of structured surface morphology, high entrapment rate and good magnetic responsibility; and the prepared magnetic microspheres can be used as a target administration carrier.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and specifically relates to a method for preparing magnetic microspheres based on polylactic acid-polyethylene glycol block copolymers. The obtained magnetic polymer microspheres can be used in medicine, bioengineering, and the environment , food and other fields. technical background [0002] Magnetic polymer microspheres are widely used in magnetic composite materials. It refers to the combination of polymer materials and magnetic inorganic substances by appropriate methods to form microspheres with certain magnetic properties and core-shell structure. Magnetic polymer microspheres, as a new type of functional polymer material, began in the 1970s, and the research has become more active in recent decades, and has become a research hotspot at home and abroad. Magnetic polymer microspheres have many excellent characteristics, such as small particle size, strong magnetic response, bioc...

Claims

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Application Information

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IPC IPC(8): C08J3/12C08L67/00C08K9/04C08K3/22
Inventor 詹世平张楠陈淑花陈理
Owner 磐升瑞祥(山东)生物工程股份有限公司
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