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Cyclodextrin-base comb polypseudorotaxane (CD-PPR) aquagel and preparation method thereof

A technology of polypseudorotaxanes and hydrogels, which is applied in the field of cyclodextrin-based comb polypseudorotaxane hydrogels, and can solve the problems of not using side chain cyclodextrin-based polypseudorotaxanes

Inactive Publication Date: 2015-07-22
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The inclusion of PEG and α-CD is the earliest proposed method for the preparation of a relatively classic main-chain cyclodextrin-based polyrotaxane, but it has not been applied to side-chain cyclodextrin-based polyrotaxanes so far. Examples of alkane

Method used

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  • Cyclodextrin-base comb polypseudorotaxane (CD-PPR) aquagel and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Step a: Weigh 15 g of APEG-1200 and dissolve it in 20 mL of redistilled DMF solvent, then add 0.3 g of AIBN, react under nitrogen protection at 65°C for 15 h, and distill off the solvent under reduced pressure at 80°C after the reaction , and finally dried under vacuum at 60°C to obtain APEG-1200 polymer. Weigh 5 g of APEG-1200 polymer and dissolve it in 50 mL of water, extract with 150 mL of chloroform, and repeat the operation three times.

[0022] Step b: Dissolve 0.1 g of the extracted polymer in 1 mL of water, add dropwise to the aqueous solution of 0.03 g / ml α-CD, sonicate for 15 min to make it evenly mixed, and then let the system stand for 12 h, A hydrogel is formed. At this time, the polyoxyethylene segment (CH 2 CH 2 O) to the molar ratio of α-CD (n(CH 2 CH 2 O) / n(α-CD)) is 6.

Embodiment 2

[0024] Step a: Weigh 15 g of APEG-1200 and dissolve it in 20 mL of redistilled DMF solvent, then add 0.6 g of AIBN, react under nitrogen protection at 70°C for 15 h, and distill off the solvent under reduced pressure at 80°C after the reaction , and finally dried under vacuum at 60°C to obtain APEG-1200 polymer. Weigh 5 g of APEG-1200 polymer and dissolve it in 50 mL of water, extract with 150 mL of chloroform, and repeat the operation three times.

[0025] Step b: Dissolve 0.1 g of the extracted polymer in 1 mL of water, add dropwise to the α-CD aqueous solution with a concentration of 0.05 g / ml, sonicate for 15 min to make it evenly mixed, and then let the system stand for 12 h. A hydrogel is formed. At this time, the polyoxyethylene segment (CH 2 CH 2 O) to the molar ratio of α-CD (n(CH 2 CH 2 O) / n(α-CD)) is 4.

Embodiment 3

[0027] Step a: Weigh 15 g APEG-1200 and dissolve it in 20 mL redistilled DMF solvent, then add 0.9 g AIBN, react under nitrogen protection at 75 °C for 15 h, and distill off the solvent under reduced pressure at 80 °C after the reaction , and finally dried under vacuum at 60°C to obtain APEG-1200 polymer. Weigh 5 g of APEG-1200 polymer and dissolve it in 50 mL of water, extract with 150 mL of chloroform, and repeat the operation three times.

[0028] Step b: Dissolve 0.1 g of the extracted polymer in 1 mL of water, add dropwise to the α-CD aqueous solution with a concentration of 0.09 g / ml, sonicate for 15 min to make it evenly mixed, and then let the system stand for 12 h. A hydrogel is formed. At this time, the polyoxyethylene segment (CH 2 CH 2 O) to the molar ratio of α-CD (n(CH 2 CH 2 O) / n(α-CD)) is 2.

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Abstract

The invention provides a cyclodextrin-base comb polypseudorotaxane (CD-PPR) aquagel and a preparation method thereof. The preparation method comprises the following steps: 1) carrying out free radical homopolymerization on monomer allyl polyethenoxy ether (APEG-200) by using azodiisobutyronitrile (AIBN) as an initiator to obtain a comb polymer; and 2) including the comb polymer prepared in the step 1) and alpha-CD in different inclusion ratios to obtain the CD-PPR aquagel. The formed comb polypseudorotaxane structure can be included with the alpha-CD under the condition of lower polymer molecular weight to form the aquagel with tubular crystal form. As the doping amount of the alpha-CD increases, the crosslinking density of the aquagel gradually increases, the gel-sol transition temperature of the aquagel becomes high, the swelling ratio becomes lower, and the thixotropy and yield stress are lower. The CD-PPR aquagel can be used as a drug carrier.

Description

technical field [0001] The invention relates to a cyclodextrin-based comb-like poly-pseudorotaxane hydrogel prepared by a free radical homopolymerization method, and also relates to a specific preparation method thereof. Background technique [0002] Cyclodextrins (CDs) are a general term for a group of oligosaccharides formed by ring-shaped arrangements of 6-12 D-glucopyranose units. characteristic. Common α-CD, β-CD and γ-CD are composed of 6-8 glucose units respectively. CD is an important class of host molecules in host-guest chemistry, and its inclusion with guest molecules is one of the important research contents of supramolecular chemistry. [0003] Macromolecules such as linear, tree, star, and hyperbranched can form cyclodextrin-based hydrogels by inclusion with cyclodextrin. Most cyclodextrin-based hydrogels have the remarkable characteristics of shear thinning and temperature sensitivity. In addition to the gel-sol transition, the temperature sensitivity also ...

Claims

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Application Information

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IPC IPC(8): C08J3/075C08J3/24C08L5/16C08L57/10C08F299/02
Inventor 关瑞芳陈其凤祝琳周传健
Owner UNIV OF JINAN
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