Rapid water-phase synthesis method of multifunctional cyclodextrin polymerized microspheres

A technology for polymerizing microspheres and cyclodextrins, which can be applied to inactive components of polymer compounds, microcapsules, nanocapsules, etc. The preparation method is simple, the product morphology and size are regular and uniform, and the synthesis reaction is mild.

Active Publication Date: 2021-03-19
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a rapid aqueous phase synthesis method of multifunctional cyclodextrin polymerized microspheres, wh

Method used

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  • Rapid water-phase synthesis method of multifunctional cyclodextrin polymerized microspheres
  • Rapid water-phase synthesis method of multifunctional cyclodextrin polymerized microspheres
  • Rapid water-phase synthesis method of multifunctional cyclodextrin polymerized microspheres

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preparation example Construction

[0048] A rapid aqueous phase synthesis method of multifunctional cyclodextrin polymerized microspheres, comprising the following steps:

[0049]1) Preparation of aldehyde-cyclodextrin: Dissolve and disperse 30g of β-cyclodextrin in 200mL of deionized water, then add sodium periodate (6-18g) of different quality, stir at 40°C at constant speed and avoid light for 4h , and then filtered with a 220nm filter membrane, and the filtrate was precipitated with 800mL of excess absolute ethanol to obtain aldehyde cyclodextrins with different aldehyde content with a dialdehyde structure;

[0050] 2) washing the aldehyde cyclodextrin with a mixed solvent of ethanol / water (V / V=80 / 20), and then freeze-drying to obtain aldehyde cyclodextrin freeze-dried powders with different modification ratios;

[0051] 3) Dissolve aldehyde cyclodextrin freeze-dried powder in deionized water to prepare an aqueous solution and heat it in a water bath to 60-80°C;

[0052] 4) Add the cross-linking agent 4-am...

Embodiment 1

[0069] A rapid aqueous phase synthesis method of multifunctional cyclodextrin polymerized microspheres, comprising the following steps:

[0070] 1) Dissolve and disperse 30g of β-cyclodextrin in 200mL of deionized water, add 12g of sodium periodate, and react in the dark at 40°C for 4 hours, then filter with a 220nm filter membrane, and use 800mL of excess ethanol to filter the filtrate Precipitate and separate out, obtain aldehyde group cyclodextrin;

[0071] 2) washing the aldehyde cyclodextrin with a mixed solvent of ethanol / water (V / V=80 / 20), and then freeze-drying to obtain the aldehyde cyclodextrin freeze-dried powder;

[0072] 3) Dissolve 0.34g of aldehyde cyclodextrin freeze-dried powder in 20mL of deionized water, and heat to 60°C in a water bath;

[0073] 4) Add 0.17g of 4-amino-6-hydroxy-2-mercaptopyrimidine, the pH of the system is about 7.0 at this time, then continue to heat and stir for 5 minutes;

[0074] 5) After the product is washed and vacuum-dried, cyclo...

Embodiment 2

[0078] In step 4) of this example, after adding 4-amino-6-hydroxy-2-mercaptopyrimidine, adjust the pH to 7.0, 7.5, 8.0, and 8.5 respectively, and then conduct the heating reaction, and the rest are the same as in Example 1. The SEM figure and TEM figure of gained cyclodextrin polymer microsphere are as follows Figure 5 shown

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Abstract

The invention relates to a rapid water-phase synthesis method of multifunctional cyclodextrin polymerized microspheres. The rapid water-phase synthesis method comprises the following steps of: pre-oxidizing beta-cyclodextrin by using sodium periodate to obtain aldehyde cyclodextrin at first; then, preparing an aldehyde cyclodextrin aqueous solution and performing heating; and then adding a cross-linking agent 4-amino-6-hydroxyl-2-mercaptopyrimidine, performing stirring for reaction, and carrying out post-treatment to obtain cyclodextrin polymerized microspheres; meanwhile, before the cross-linking agent is added, an active drug or a modifier can be introduced into a reaction system, so that the loading of the active drug and the preparation of the modified cyclodextrin polymerized microspheres can be realized. Compared with the prior art, the preparation method disclosed by the invention is simple, mild and green, and can quickly react in an open water-phase system under a low-temperature condition; the product has a good alkaline response function and can be used for various oral intestinal drug delivery systems; and in addition, the boron-modified cyclodextrin polymerized microspheres show an excellent rapid adsorption effect on fluoroquinolone antibiotics, and have a better application prospect in the field of waste drug treatment.

Description

technical field [0001] The invention belongs to the technical field of responsiveness and porous polymer materials, and relates to a method for rapid aqueous phase synthesis of multifunctional cyclodextrin polymerized microspheres, in particular to a rapid aqueous phase synthesis method for multifunctional cyclodextrin polymerized microspheres. And the application of this method in the field of synthesizing nano drug carriers with alkaline response and in the field of synthesizing quinolone antibiotics fast adsorption materials. Background technique [0002] Cyclodextrin (CD) is an inexpensive, natural, and cavity-containing oligomeric macromolecule capable of trapping organic molecules with appropriate size, shape, and hydrophobicity to form well-defined host-guest complexes. In addition, cyclodextrin-based insoluble polymers have been extensively studied in the fields of adsorptive removal of various micro-pollutants, membrane separation, and as carrier materials. So far,...

Claims

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Application Information

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IPC IPC(8): A61K9/51A61K47/40A61K31/496A61P31/04
CPCA61K9/5161A61K31/496A61P31/04
Inventor 毛舜李秋菊王丹丹
Owner TONGJI UNIV
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