Abstract
Nano-hydroxyapatite (HA)/poly(l-lactide) (PLLA) composite microspheres with relatively uniform size distribution were prepared by a solid-in-oil-in-water (s/o/w) emusion solvent evaporation method. The encapsulation of the HA nanopaticles in microshperes was significantly improved by grafting PLLA on the surface of the HA nanoparticles (p-HA) during emulsion process. This procedure gave a possibility to obtain p-HA/PLLA composite microspheres with uniform morphology and the encapsulated p-HA nanoparticle loading reached up to 40 wt% (33 wt% of pure HA) in the p-HA/PLLA composite microspheres. The microstructure of composite microspheres from core-shell to single phase changed with the variation of p-HA to PLLA ratios. p-HA/PLLA composite microspheres with the diameter range of 2–3 μm were obtained. The entrapment efficiency of p-HA in microspheres could high up to 90 wt% and that of HA was only 13 wt%. Surface and bulk characterizations of the composite microspheres were performed by measurements such as wide angle X-ray diffraction (WAXD), thermal gravimetric analysis (TGA), environmental scanning electron microscope (ESEM) and transmission electron microscopy (TEM).
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References
Bonfield W. (1988) Materials characteristics versus in vivo behavior. New York Academy of Science, New York, 173
Chen C.N., Zhu C.L., Hao L.Y., Hu Y., Chen Z.Y. (2004) Preparation and characterization of the CdS/PSA core-shell “egg”. Inorg. Chem. Commun.7(3):322–326
Daniels A.U., Adriano K.P., Smuts W.P., Chang M.K.O., Keller J. (1994) Evaluation of absorbable poly(ortho esters) for use in surgical implants. J. Appl. Biomater. 5(1):51–64
He Y.J. (2005) Synthesis of polyaniline/nano-CeO2 composite microspheres via a solid-stabilized emulsion route. Mater. Chem. Phys. 92(1):134–137
Hong Z.K., Zhang P.B., He C.L., Qiu X.Y., Liu A.X., Chen L., Chen X.S., Jing X.B. (2005) Nano-composite of poly(l-lactide) and surface grafted hydroxyapatite: Mechanical properties and biocompatibility. Biomaterials. 26:6296–6304
Hu J.S., Gu Y.G.o, Liang H.P., Wan L.J., Bai C.L., Wang Y.G. (2004) Interface assembly synthesis of inorganic composite hollow spheres. J. Phys. Chem. B. 108(28):9734–9738
Kim J.W., Lee J.E., Kim S.J., Lee J.S., Ryu J.H., Kim J., Han S.H., Chang I.S., Suh K.K. (2004) Synthesis of silver/polymer colloidal composites from surface-functional porous polymer microspheres. Polymer 45(14):4741–4747
Koprinarov I., Hitchcock A.P., Li W.H., Heng Y.M., Stöver H.D.H. (2001) Quantitative compositional mapping of core-shell polymer microspheres by soft X-ray spectromicroscopy. Macromolecules. 34(13):4424–4429
Labella R., Braden M., Deb S. (1994) Novel hydroxyapatite-based dental composites. Biomaterials 15(15):1197–1200
Pich A., Bhattacharya S., Ghosh A., Adler H.J.P. (2005) Composite magnetic particles: 2. Encapsulation of iron oxide by surfactant-free emulsion polymerization. Polymer 46(13):4596–4603
Qiu Q.Q., Ducheyne P., Ayyaswamy P.S. (2000) New bioactive, degradable composite microspheres as tissue engineering substrates. J. Biomed. Mater. Res. 52(1):66–76
Qiu X.Y., Hong Z.K., Hu J.L., Chen L., Chen X.S., Jing X.B. (2005) Hydroxyapatite surface modified by l-lactic acid and its subsequent grafting polymerization of l-lactide. Biomacromolecules. 6(3):1193–1199
Rong Y., Chen H.Z., Li H.Y., Wang M. (2005) Encapsulation of titanium dioxide particles by polystyrene via radical polymerization. Colloids Surf. A Physicochem. Eng. Asp. 253(1–3):193–197
Shi X.Y., Briseno A.L., Sanedrin R.J., Zhou F.M. (2003) Formation of uniform polyaniline thin shells and hollow capsules using polyelectrolyte-coated microspheres as templates. Macromolecules 36(11):4093–4098
Shim J.W., Kim J.W., Han S.H., Chang I.S., Kim H.K., Kang H.H., Lee O.S., Suh K.D. (2002) Zinc oxide/polymethylmethacrylate composite microspheres by in situ suspension polymerization and their morphological study. Colloids Surf. A. Physicochem. Eng. Asp. 207(1–3):105–111
Tanner K.E., C. Doyle & W. Bonfield, 1990. Clinical Implant Materials; Advances in Biomaterials, Vol. 9, Elsevier Science Publication, Amsterdam, pp. 1, 49–54
Udi A., Shlomo M. (2005) Surface-modified hemispherical polystyrene/polybutyl methacrylate composite particles. J. Colloid Interf. Sci. 288(1):61–70
Verheyen C.C.P.M., de Wijn J.R., van Blitterswijk C.A., Rozing P.M., de Groot K. (1992) Bone-bonding biomaterials. Reed Healthcare Commun. 1:53–71
Yin J.L., Qian X.F., Yin J., Shi M.W., Zhou G.T. (2003) Preparation of ZnS/PS microspheres and ZnS hollow shells. Mater. Lett. 57(24–25):3859–3863
Zhang L.J., Wan M.X., Wei Y. (2005) Polyaniline/TiO2 microspheres prepared by a template-free method. Synth. Metals. 151(1):1–5
Zhang X.F., Hu J.L., Chen X.S., Jing X.B. (2005) Preparation and characterization of biodegradable insulin-loaded microspheres. Chem. J. Chin. Univ. 26:554–557
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This project was financially supported by the National Natural Science Foundation of China (20574066), the National Fund for Distinguished Young Scholars (50425309) and the International Cooperation fund of Science and Technology (Key project 2005DFA50290).
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Qiu, X., Han, Y., Zhuang, X. et al. Preparation of nano-hydroxyapatite/poly(l-lactide) biocomposite microspheres. J Nanopart Res 9, 901–908 (2007). https://doi.org/10.1007/s11051-006-9158-6
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DOI: https://doi.org/10.1007/s11051-006-9158-6