摘要
通过碳化二亚胺(EDC)改性、二次冻干制备多孔胶原-β-磷酸三钙-硫酸软骨素复合膜材料。通过扫描电镜(SEM)、X射线衍射分析仪(XRD)与原子力显微镜(AFM)考察了组分变化与制备过程中复合材料的微观形貌变化,并进一步利用红外、孔隙率、MTT细胞毒性实验等分析手段对复合材料的结构与性能进行了表征。实验结果表明,当胶原盐酸溶解液pH=2,胶原与β-磷酸三钙质量比为1∶2(m(Col)∶m(β-TCP)=1∶2)时,复合材料中β-TCP晶相保持较好,其与胶原之间的排列结合最为均匀紧密。经EDC改性后,SEM与AFM实验均显示了交联后的胶原束明显变大变粗,以一定的方向紧密地排列在一起。XRD图谱显示复合材料中β-TCP特征衍射峰明显。复合材料的孔径为80~90μm,三元膜孔隙率为(90.76±1.28)%,大于纯胶原冻干膜(85.88±0.92)%;红外光谱证实β-TCP中的钙离子与Col上的羧基发生了化学键合,AFM显示β-TCP颗粒能与胶原发生直接联结。复合材料的MTT实验结果为1级,是一种潜在的口腔修复膜材料。
The porous collagen-β-tricalcium phosphate-chondroitin sulfate composite membrane was prepared by EDC modifi- cation and twice freeze-dried method. The effect of variation of material proportion, pH value and method in materials preparation process on the structure and properties of composite materials were investigated by scanning electron microscope (SEM), X-ray dif- fraction analyzer (XRD) and atomic force microscope (AFM), P-β-IR, porosity measurer, MTT cytotoxicity tester. The results indicated that when the pH value of collagen/HCl solution was 2, the mass ratio of collagen and β-tricalcium phosphate was 1 : 2 (m(Col) : m(β-TCP)= 1 : 2), the β-TCprs crystalline phase maintained, the composition was uniform and compact. After EDC modification, the SEM and AFM results showed that the collagen bundles after crosslinking got bigger and thicker obviously, ar- ranged closely in a certain direction. XRD spectrum showed that the characteristic diffraction peaks of β-TCP in composite materials were obvious. The pore size of composite material was about 80--90μm, the porosity of ternary membrane was (90. 76±1.28)%, larger than that of collagen membrane (85.88±0. 91)%. Infrared spectra confirmed that Ca2+ of β-TCP and carboxyl of Col were chemically bonded. AFM showed that β-TCP particles had a direct connection with collagen. The MTT eytotoxicity levels of compo- site materials were 1, which was a kind of potential dental restorative material.
出处
《材料导报》
EI
CAS
CSCD
北大核心
2017年第2期8-12,19,共6页
Materials Reports
基金
国家自然科学基金(51473001)
关键词
胶原
Β-磷酸三钙
硫酸软骨素
多孔复合膜
微观形貌
collagen, β-tricalcium phosphate, chondroitin sulfate, porous composite membrane, mierostructure