US 12,005,156 B2
Berberine/mineralized collagen-based composite membrane and preparation method and application thereof
Weifen Zhang, Shandong (CN); Jian Zhang, Shandong (CN); Jingjing Zhang, Shandong (CN); Dejun Ding, Shandong (CN); Xiuwen Guan, Shandong (CN); Linlin Hu, Shandong (CN); and Yuhan Zhang, Shandong (CN)
Assigned to WEIFANG MEDICAL UNIVERSITY, Shandong (CN)
Appl. No. 17/413,390
Filed by WEIFANG MEDICAL UNIVERSITY, Shandong (CN)
PCT Filed Apr. 2, 2021, PCT No. PCT/CN2021/085258
§ 371(c)(1), (2) Date Jun. 11, 2021,
PCT Pub. No. WO2022/105091, PCT Pub. Date May 27, 2022.
Claims priority of application No. 202011317356 (CN), filed on Nov. 23, 2020.
Prior Publication US 2023/0355837 A1, Nov. 9, 2023
Int. Cl. A61L 27/26 (2006.01); A61F 2/30 (2006.01); A61L 27/20 (2006.01); A61L 27/24 (2006.01); A61L 27/48 (2006.01); A61L 27/58 (2006.01); D01D 5/00 (2006.01); D04H 1/4282 (2012.01); D04H 1/435 (2012.01); D04H 1/728 (2012.01); D04H 3/007 (2012.01); D04H 3/011 (2012.01); D04H 3/16 (2006.01); D06M 15/03 (2006.01); D06M 23/10 (2006.01); D06M 101/18 (2006.01); D06M 101/32 (2006.01)
CPC A61L 27/26 (2013.01) [A61F 2/30965 (2013.01); A61L 27/20 (2013.01); A61L 27/24 (2013.01); A61L 27/48 (2013.01); A61L 27/58 (2013.01); D01D 5/0038 (2013.01); D01D 5/0084 (2013.01); D04H 1/4282 (2013.01); D04H 1/435 (2013.01); D04H 1/728 (2013.01); D04H 3/007 (2013.01); D04H 3/011 (2013.01); D04H 3/16 (2013.01); D06M 15/03 (2013.01); D06M 23/10 (2013.01); A61L 2400/12 (2013.01); A61L 2430/02 (2013.01); D06M 2101/18 (2013.01); D06M 2101/32 (2013.01); D10B 2321/12 (2013.01); D10B 2331/041 (2013.01); D10B 2509/00 (2013.01)] 8 Claims
 
1. A preparation method of a berberine/mineralized collagen-based composite membrane comprising the following steps:
(1) mixing chitosan and mineralized collagen with a glacial acetic acid solution to obtain a resulting mineralized collagen suspension;
(2) mixing polycaprolactone, water-soluble compounds, and berberine with a solvent to obtain an electrospinning solution; and
(3) casting the resulting mineralized collagen suspension obtained in step (1) into a film to obtain a mineralized collagen membrane, and electrospinning the electrospinning solution obtained in step (2) and receiving resulting electrospun fibers on the mineralized collagen membrane to obtain the berberine/mineralized collagen-based composite membrane;
or electrospinning the electrospinning solution obtained in step (2) to obtain a berberine nanofiber membrane, coating the resulting mineralized collagen suspension obtained in step (1) on the berberine nanofiber membrane, and drying the coated berberine nanofiber membrane to obtain the berberine/mineralized collagen-based composite membrane;
wherein in the berberine/mineralized collagen-based composite membrane, the berberine nanofiber membrane comprises components of the following mass fractions: 20-65 wt % of polycaprolactone, 18-80 wt % of water-soluble compounds, and berberine≤0.1 wt % based on the mass of the berberine nanofiber membrane; and the mineralized collagen membrane comprises components of the following mass fractions: 15-90 wt % of chitosan, and 10-85 wt % of mineralized collagen based on the mass of the mineralized collagen membrane;
the mixing processes in step (2) are as below: berberine is dissolved in the solvent to get a berberine solution, then polycaprolactone and the water-soluble compounds are respectively dissolved in the berberine solution to get a polycaprolactone-berberine solution and a water-soluble compound-berberine solution; the polycaprolactone-berberine solution and the water-soluble compound-berberine solution are mixed to get the electrospinning solution; and
wherein the mass concentration of polycaprolactone in the polycaprolactone-berberine solution is 5-15%; the mass concentration of the water-soluble compounds in the water-soluble compound-berberine solution is 10-30%; the volume ratio of the polycaprolactone-berberine solution to the water-soluble compound-berberine solution is 7:(2-4); the concentration of berberine in the electrospinning solution is 5-50 μmol/L; the solvent is a mixed solvent of trichloromethane and methanol.