纳米羟基磷灰石/壳聚糖复合微球的原位仿生制备及表征

doi:10.15541/jim20140167

无机材料学报 ›› 2014, Vol. 29 ›› Issue (12): 1327-1332.DOI: 10.15541/jim20140167 CSTR: 32189.14.10.15541/jim20140167

纳米羟基磷灰石/壳聚糖复合微球的原位仿生制备及表征

李健¹, 韩志军¹, 魏延¹, 牛璐璐¹, 刘宇¹, 路国运², 黄棣¹

(太原理工大学 1. 力学学院, 材料强度与结构冲击山西省重点实验室; 2. 应用力学与生物医学工程研究所, 太原 030024)

收稿日期:2014-04-03 修回日期:2014-06-12 出版日期:2014-12-20 网络出版日期:2014-11-20
作者简介:李健(1989–), 女, 硕士研究生. E-mail: 18503512013@163.com
基金资助:
国家自然科学基金(11372209, 51203028);山西省青年科技基金(2013021014-2);山西省高等学校科技创新项目(2013111)

In situ Biomimetic Fabrication and Characterization of Nano-hydroxyapatite/ Chitosan Composite Microspheres

LI Jian¹, HAN Zhi-Jun¹, WEI Yan¹, NIU Lu-Lu¹, LIU Yu¹, LU Guo-Yun², HUANG Di¹

(1. College of Mechanics, Shanxi Key Laboratory of Material Strength & Structural Impact, Taiyuan University of Technology, Taiyuan 030024, China; 2. Institute of Applied Mechanics & Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030024, China)

Received:2014-04-03 Revised:2014-06-12 Published:2014-12-20 Online:2014-11-20
About author:LI Jian. E-mail: 18503512013@163.com
Supported by:
National Natural Science Foundation of China (11372209, 51203028);Natural Science Foundation of Shanxi Province (2013021014-2);Scientific and Technological Innovation Programs of Higher Education Institutions in Shanxi (2013111)

摘要/Abstract

摘要：

为解决纳米羟基磷灰石/壳聚糖(nHA/CS)复合微球中nHA团聚及分散不均的问题, 本研究在油包水的乳液体系中, 原位仿生制备了nHA/CS复合微球, 并与共混法制备的nHA/CS复合微球进行了对比研究。利用扫描电镜(SEM)、X射线能谱(EDS)、X射线衍射(XRD)、红外(FTIR)和激光粒度仪等手段对不同微球的理化性能进行表征。结果表明: 相比共混法, 原位仿生制备的nHA/CS复合微球形态圆整均匀, 分散性好, 粒径分布较窄, 平均粒径为8.62 μm, nHA晶体均匀分布在微球内部及表面, 并与CS基质以化学键结合。该复合微球有望用于骨组织工程及药物控制释放。

关键词: 原位仿生, 纳米羟基磷灰石, 壳聚糖, 复合微球

Abstract:

To solve the problem that nano-hydroxyapatite (nHA) crystals aggregation and non-uniformly distribution in nano-hydroxyapatite/chitosan (CS) composite microspheres, nHA/CS microspheres were prepared through in situ biomimetic method in water-in-oil (W/O) emulsions. The physical and chemical properties of the composite microspheres were investigated by scanning electronic microscopy (SEM), X-ray energy-dispersive spectroscope (EDS), X-ray diffraction (XRD), fourier transform infrared spectroscope (FTIR) and laser particle size analyzer. The results indicate that the composite microspheres are spherical with average size of 8.62 μm and disperse uniformly. Moreover, the nHA crystals are dispersed uniformly within composite microspheres and bonded with CS matrix. The composite microspheres have great potential in bone tissue engineering and drug delivery system.

Key words: in situ biomimetic, nano-hydroxyapatite, chitosan, composite microspheres

中图分类号:

TB33

李健, 韩志军, 魏延, 牛璐璐, 刘宇, 路国运, 黄棣. 纳米羟基磷灰石/壳聚糖复合微球的原位仿生制备及表征[J]. 无机材料学报, 2014, 29(12): 1327-1332.

LI Jian, HAN Zhi-Jun, WEI Yan, NIU Lu-Lu, LIU Yu, LU Guo-Yun, HUANG Di. In situ Biomimetic Fabrication and Characterization of Nano-hydroxyapatite/ Chitosan Composite Microspheres[J]. Journal of Inorganic Materials, 2014, 29(12): 1327-1332.

图/表 7

图 1 纯CS微球(a)、原位仿生(b)和共混法(c)制备的nHA/CS复合微球的XRD图谱

Fig. 1 XRD patterns of pure CS microspheres (a), nHA/CS composite microspheres fabricated by in situ biomimetic method (b) and co-mixing method (c)

图 2 纯CS微球(a)、原位仿生(b)和共混法(c)制备的nHA/CS复合微球红外光图谱

Fig. 2 FTIR spectra of pure CS microspheres (a), nHA/CS composite microspheres fabricated by in situ biomimetic method (b) and co-mixing method (c)

图 3 纯CS微球(a)、共混法制备的nHA/CS复合微球SEM照片(b); 复合微球放大照片(c); Ca(d)和P(e)元素面扫描图

Fig. 3 SEM images of CS microspheres (a) and nHA/CS composite microspheres fabricated by co-mixing method: in the low mag-nification (b) and in the high magnification (c); EDS map-scanning analysis of Ca and P element (d, e) corresponding to (c)

图 4 原位仿生制备的nHA/CS复合微球SEM照片(a), 复合微球放大照片(b), Ca (c)和P (d)元素面扫描图

Fig. 4 SEM images and EDS map-scanning analysis of nHA/CS composite microspheres fabricated by in situ biomimetic method: low magnification of the sample (a); higher magnification of the sample (b) and map-scanning analysis of Ca and P element (c, d) corresponding to the bottom rectangle region in (a)

图 5 原位仿生制备的nHA/CS复合微球断面SEM照片(a), 复合微球断面放大图(b), Ca (c)和P (d)元素面扫描

Fig. 5 SEM images and EDS map-scanning analysis of the fracture surface of nHA/CS composite microspheres fabricated by in situ biomineralization method: low magnification of the sample (a); higher magnification of the sample (b) and map-scanning analysis of Ca and P element (c, d) corresponding to the pink rectangle region in (a)

图 6 纯CS微球(a)、原位仿生(b)和共混法(c)制备的nHA/CS复合微球的粒径分布图

Fig. 6 Size distribution of CS microspheres (a), nHA/CS composite microspheres fabricated by in situ biomimetic method (b) and co-mixing method (c)

图 7 原位仿生nHA/CS复合微球形成机理图

Fig. 7 The growth process of nHA/CS composite microsphe-res fabricated in situ biomimetic method

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纳米羟基磷灰石/壳聚糖复合微球的原位仿生制备及表征

In situ Biomimetic Fabrication and Characterization of Nano-hydroxyapatite/ Chitosan Composite Microspheres

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