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CN-122005918-A - Preparation method of hydroxyapatite/curcumin antibacterial composite material with ultrasonic response

CN122005918ACN 122005918 ACN122005918 ACN 122005918ACN-122005918-A

Abstract

The invention discloses a preparation method of a hydroxyapatite/curcumin antibacterial composite material with ultrasonic response, and relates to the technical field of biomedical composite materials. In order to solve the problems of postoperative infection risk and antibiotic resistance of the material, a preparation method of the composite material with biocompatibility and ultrasonic response antibacterial property is provided. Dissolving calcium nitrate tetrahydrate and curcumin in deionized water to obtain a mixed solution A, dissolving diammonium phosphate in deionized water to obtain a mixed solution B, slowly dripping the mixed solution B into the mixed solution A to enable the molar ratio of calcium to phosphorus to be 1.67, adjusting the pH value to 8-10 by ammonia water, stirring to obtain a reaction precursor, performing hydrothermal reaction for 10-24 hours at 110-140 ℃, centrifugally washing to be neutral by deionized water, and freeze-drying to obtain the material. The preparation method provided by the invention is simple, mild in condition and free from harmful gas, and the obtained material can effectively generate active oxygen under ultrasonic stimulation, has excellent antibacterial effect on escherichia coli and staphylococcus aureus, and is suitable for biomedical fields such as bone repair and implant material coating.

Inventors

  • RAN QIAN
  • WU SHUILIN
  • LIU XIANGMEI

Assignees

  • 湖北大学
  • 冉倩

Dates

Publication Date
20260512
Application Date
20260317

Claims (5)

  1. 1. The technical scheme of the invention is that the preparation method of the hydroxyapatite/curcumin antibacterial composite material with ultrasonic response is characterized by comprising the following steps: Dissolving 5.8-6.0 g tetrahydrate calcium nitrate in 25-30 ml deionized water, adding 0.1-1.0 g curcumin, stirring for 30-50 min to obtain a mixed solution A, dissolving 1.9-2.0 g diammonium phosphate in 25-30 ml deionized water, stirring for 30-50 min to obtain a mixed solution B, slowly dripping the mixed solution B into the mixed solution A to enable the molar ratio of calcium to phosphorus to be 1.67, regulating the pH value to 8-10 by using 10-30% ammonia water, continuing stirring for 30-60 min to obtain a reaction precursor, transferring the reaction precursor solution into a polytetrafluoroethylene lining reaction kettle, carrying out hydrothermal reaction at 110-140 ℃ for 10-14 h, taking out after natural cooling, centrifugally separating a reaction product, washing 3 times to neutrality by using deionized water, and freeze-drying at-50-60 ℃ for 20-30 h to obtain the hydroxyapatite/curcumin composite material with ultrasonic response.
  2. 2. The method for preparing an ultrasonic-responsive hydroxyapatite/curcumin antibacterial composite material according to claim 1, wherein the amount of curcumin used in the step is 0.7-1.0g.
  3. 3. The method for preparing an ultrasonic-responsive hydroxyapatite/curcumin antibacterial composite material according to claim 1, wherein ammonia water with a mass-volume ratio of 10% -30% is used for adjusting the pH value in the step, and the pH value of the solution is kept to be 8-10. The stirring time is 30-60 minutes after the adjustment.
  4. 4. The method for preparing an ultrasonic-responsive hydroxyapatite/curcumin antibacterial composite material according to claim 1, wherein the hydrothermal reaction temperature in the step is 110-140 ℃ and the reaction time is 10-14 hours.
  5. 5. The method for preparing an ultrasonic-responsive hydroxyapatite/curcumin antibacterial composite material according to claim 1, wherein the temperature of freeze drying in the fifth step is-50-60 ℃ and the drying time is 20-30 hours.

Description

Preparation method of hydroxyapatite/curcumin antibacterial composite material with ultrasonic response Technical Field The invention relates to the technical field of biomedical composite materials, in particular to a preparation method of an ultrasonic response hydroxyapatite/curcumin antibacterial composite material. Background Biomedical materials are functional materials for diagnosing, treating, repairing or replacing human tissues or organs, and are widely applied to the fields of orthopaedics, dentistry, drug delivery and the like. Among them, hydroxyapatite has become one of the hot spots of research due to its excellent biocompatibility, bone conductivity and chemical stability. The nano hydroxyapatite powder has higher specific surface area and biological activity, can promote cell adhesion and bone tissue regeneration, and has wide application prospect in bone repair and implantation materials. However, implant materials often face the risk of post-operative infection during clinical application. Traditional antimicrobial strategies rely primarily on antibiotics, but abuse of antibiotics tends to lead to the production of resistant bacteria and local drug concentrations are difficult to maintain. In recent years, active oxygen-based antibacterial strategies have received attention because of their broad-spectrum bactericidal properties and their low susceptibility to developing drug resistance. Ultrasonic is used as a non-invasive and strong penetrating external stimulation means, and can excite certain materials to generate active oxygen, so as to realize non-invasive antibacterial treatment. Curcumin is a natural polyphenol compound and has good biocompatibility, anti-inflammatory, antioxidant and antibacterial activities. Under the action of ultrasound, curcumin can be activated and generate singlet oxygen and other active oxygen species, and excellent ultrasound response antibacterial performance is shown. Therefore, curcumin and hydroxyapatite are compounded to prepare the composite material with good biological activity and ultrasonic response antibacterial property, and the composite material has important research value and application prospect. Disclosure of Invention The invention aims to provide a preparation method of an ultrasonic-response hydroxyapatite/curcumin antibacterial composite material, and the prepared material has good biocompatibility and ultrasonic-response antibacterial property, can generate active oxygen under ultrasonic stimulation, and can effectively inhibit bacterial growth. The technical scheme of the invention is that the preparation method of the hydroxyapatite/curcumin antibacterial composite material with ultrasonic response is characterized by comprising the following steps: Dissolving 5.8-6.0 g tetrahydrate calcium nitrate in 25-30 ml deionized water, adding 0.1-1.0 g curcumin, stirring for 30-50 min to obtain a mixed solution A, dissolving 1.9-2.0 g diammonium phosphate in 25-30 ml deionized water, stirring for 30-50 min to obtain a mixed solution B, slowly dripping the mixed solution B into the mixed solution A to enable the molar ratio of calcium to phosphorus to be 1.67, regulating the pH value to 8-10 by using 10-30% ammonia water, continuing stirring for 30-60 min to obtain a reaction precursor, transferring the reaction precursor solution into a polytetrafluoroethylene lining reaction kettle, carrying out hydrothermal reaction at 110-140 ℃ for 10-14 h, taking out after natural cooling, centrifugally separating a reaction product, washing 3 times to neutrality by using deionized water, and freeze-drying at-50-60 ℃ for 20-30 h to obtain the hydroxyapatite/curcumin composite material with ultrasonic response. The molar ratio of calcium to phosphorus in the step was 1.67. The addition amount of curcumin in the step is 0.1-1.0 g. In the step, ammonia water with the volume ratio of 10-30% is used for regulating the pH value. The hydrothermal reaction temperature in the step is 110-140 ℃ and the reaction time is 10-14 hours. The freeze drying temperature in the step is-55-60 ℃ and the drying time is 20-30 hours. A preparation method of a hydroxyapatite/curcumin antibacterial composite material with ultrasonic response is characterized by comprising the following steps of dissolving 5.9 g calcium nitrate tetrahydrate in 25 mL deionized water, adding 0.736 g curcumin, stirring for 30 minutes to obtain a mixed solution A, dissolving 1.98 g diammonium phosphate in 25 mL deionized water, stirring for 30 minutes to obtain a mixed solution B, slowly dropwise adding the mixed solution B into the mixed solution A to enable the molar ratio of calcium to phosphorus to be 1.67, regulating the pH value to 8.7 by using 25% ammonia water, continuing stirring for 1 hour to obtain a reaction precursor, transferring the reaction precursor solution into a polytetrafluoroethylene lining reaction kettle, carrying out hydrothermal reaction at 130 ℃ for 12 hours, taking out aft