Method for synthesizing dextran-magnetic LDH-fluorouracil magnetic targeting sustained and controlled release tripolymer

A technology of fluorouracil and dextran, which is applied in the field of joint preparation of "nitrogen-protected co-precipitation intercalation-dextran compound-solvent conversion", which can solve the problems of unstable storage of magnetic LDH-Drugs, difficulty in slow-release and targeted fusion, and magnetic LDH is easy to oxidize and other problems, and achieves the effect of solving the problems of preparation and anti-oxidation protection, wide application range and high storage stability

Active Publication Date: 2009-12-23
NINGXIA MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the above-mentioned existing LDH-Drugs preparation technology and the complicated preparation process of the traditional magnetic targeting system, the difficulty of combining slow release and targeting, the easy oxidation and decomposition of magnetic

Method used

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  • Method for synthesizing dextran-magnetic LDH-fluorouracil magnetic targeting sustained and controlled release tripolymer
  • Method for synthesizing dextran-magnetic LDH-fluorouracil magnetic targeting sustained and controlled release tripolymer
  • Method for synthesizing dextran-magnetic LDH-fluorouracil magnetic targeting sustained and controlled release tripolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 7.5g FeCl 2 4H 2 O, 3.4 g FeCl 3 ·6H 2 O, 2.0g 5-Flu (fluorouracil), with 150mL H 2 O is dissolved under the conditions of 35-70°C, stirring speed 200rpm and nitrogen protection, and 2mol L is added dropwise over 15-30min. -1 NaOH solution to pH 6.0-8.0 at the end point of precipitation. After crystallizing the original slurry under the same conditions for 45-60 minutes, add 8.0-16.0 g of dextran to the reaction device, increase the stirring speed to 300 rpm, and react for 40-80 minutes at 35-70 ° C and nitrogen. Seal the reaction slurry and quickly transfer it to 500~1000mL of absolute ethanol that has been cryogenically treated at -10~-30°C for 2~4h, stir for 5~10min, then let it stand for 15~30min to complete the solvent conversion, and centrifuge (speed 5000rpm , 15min). Drying conditions: After the vacuum drying box is filled with nitrogen and emptied, transfer to the sample, set at 50-80°C, vacuum degree 0.085MPa, and dry for 24-48 hours.

[0026] The ferro...

Embodiment 2

[0028] 3.7g FeCl 2 4H 2 O, 1.7 g FeCl 3 ·6H 2 O with 150mL H 2 O is dissolved at 35-70°C, 200rpm and under nitrogen protection conditions, and 2mol L is driven dropwise by a constant flow of nitrogen -1 NaOH to the pH of the precipitation end point (6.0-8.0), maintain the reaction temperature of 35-70°C through the agitator and relay; crystallize the co-precipitation slurry under the same stirring speed, protective gas flow rate and 35-70°C for 45-60 minutes ; Then add 0.5-1.0g fluorouracil to the crystallization slurry, maintain the same conditions for ion exchange reaction for 1-4 hours, then add 4.0-8.0g dextran, increase the stirring speed to 300rpm, and perform compound reaction at 35-70°C and nitrogen protection conditions 40~80min. Seal the reaction slurry and quickly transfer it to 500~1000mL of absolute ethanol that has been cryogenically treated at -10~-30°C for 2~4 hours, complete the solvent conversion treatment under stirring conditions, and then centrifuge a...

Embodiment 3

[0030] Press Fe 2+ / Al 3+ Molar ratio 3 will 8mL 1.50mol L -1 FeCl 2 and 8mL 0.50mol·L -1 AlCl 3 The solution was driven into the synthesis device by high-purity nitrogen, and 0.5 g of fluorouracil was dissolved in the mixed salt solution under constant nitrogen protection and 200 rpm stirring conditions, and 2.0 mol L was added dropwise. -1 NaOH precipitant until the end point pH is 6.0-8.0, and maintain the reaction temperature of 35-70°C; the co-precipitation slurry is crystallized for 45-60 minutes under the same stirring speed, protective gas flow rate and 35-70°C; then add 4.0 to the synthesis device ~8.0g dextran, increase the stirring speed to 300rpm, compound reaction at 35~70℃ and nitrogen protection conditions for 40~80min; seal the reaction slurry, quickly transfer it to 500~1000mL, and undergo cryogenic treatment at -10~-30℃ for 2~ In 4 hours of absolute ethanol, stir to complete the solvent conversion treatment, let stand for about 15-30 minutes, and then ce...

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Abstract

The invention relates to a method for synthesizing dextran-magnetic LDH-fluorouracil magnetic targeting sustained and controlled release tripolymer, comprising the following steps of: finishing the synthesis of magnetic layered composite hydroxide and the intercalation assembly of fluorouracil to the magnetic layered composite hydroxide under the condition of nitrogen protection; performing the in-situ composite process of magnetic LDH-fluorouracil under the condition of nitrogen protection with the dextran as the wrapping material; and finally separating the product through the solvent conversion technology. The invention realizes the merging and unification of the targeting and the sustained release of a magnetic targeting drug, thereby solving the problems of the preparation of magnetic LDH-Drugs and protection against oxidation, and synthesizing a magnetic targeting sustained and controlled release drug delivery system which has good biocompatibility and high storage stability and fits for transport in vivo; and the invention is suitable for the chemical synthesis of various magnetic targeting sustained and controlled release drugs, and has the advantages of simple and rapid preparation technology, high product purity, energy consumption saving, no environment pollution, wide application range and the like.

Description

technical field [0001] The invention relates to the technical field of inorganic material composites, in particular to a joint preparation method of "nitrogen protection co-precipitation intercalation-dextran composite-solvent conversion" of a "dextran-magnetic LDH-fluorouracil" trimer type magnetic targeting slow-controlled release system , to solve the problems of oxidative decomposition of the magnetic LDH-fluorouracil dimer carrier and the reduction of slow and controlled release performance. Background technique [0002] Magnetically targeted drug delivery system is a new type of delivery system that has attracted much attention at home and abroad in recent years. The traditional chemical synthesis includes the main stages of organic grafting of magnetic particles, drug loading and preparation of dosage forms. Combining the interlayer controlled release effect of LDH layered structure with the paramagnetism of magnetic LDH laminates structurally is the best solution to ...

Claims

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Application Information

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IPC IPC(8): A61K47/48A61K47/36A61K47/02A61K31/513A61P35/00A61K47/52A61K47/61
Inventor 苟国敬鲍凤娟蒋袁絮
Owner NINGXIA MEDICAL UNIV
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