Yokogawa Y, Paz Reyes J, Mucalo M R, Toriyama M, Kawamoto Y, Suzuki T, Nishizawa K, Nagata F, Kamayama T
Bioceramics Laboratory, National Industrial Research Institute of Nagoya, Japan.
J Mater Sci Mater Med. 1997 Jul;8(7):407-12. doi: 10.1023/a:1018549404092.
Calcium phosphate growth on chitin phosphorylated fibres was studied using scanning electron microscopy and energy dispersive X-ray analysis (SEM, EDX), micro-Fourier transform infrared spectroscopy (FTIR), and solid state magic angle spinning nuclear magnetic resonance (MAS NMR) techniques. The C6 chemical shift positions of 13C MAS NMR in the chitin fibres phosphorylated using urea and H3PO4 are obvious indicating that phosphorylation takes place not in the C1 but in the C6 region. Micro-FTIR and 31P MAS NMR suggested that ammonium hydrogen phosphate formed during the phosphorylation procedure. Chitin fibres phosphorylated using urea and H3PO4 and then soaked in saturated Ca(OH)2 solution at ambient temperature, which lead to the formation of thin coatings formed by partial hydrolysis of the PO4 functionalities, were found to stimulate the growth of a calcium phosphate coating on their surfaces after soaking in 1.5xSBF solution for as little as one day. The thin layer after Ca(OH)2 treatment functioned as a nucleation layer for further calcium phosphate deposition after soaking in 1.5xSBF solution. EDX-measured Ca : P ratios of the coatings of Ca(OH)2-treated phosphorylated chitin in 1.5xSBF solution suggested that calcium-deficient apatite was formed.
利用扫描电子显微镜和能量色散X射线分析(SEM、EDX)、微傅里叶变换红外光谱(FTIR)以及固态魔角旋转核磁共振(MAS NMR)技术,研究了磷酸钙在磷酸化几丁质纤维上的生长情况。使用尿素和H3PO4磷酸化的几丁质纤维中,13C MAS NMR的C6化学位移位置明显,表明磷酸化并非发生在C1区域,而是在C6区域。微FTIR和31P MAS NMR表明,磷酸化过程中形成了磷酸氢铵。发现使用尿素和H3PO4磷酸化的几丁质纤维,然后在室温下浸泡在饱和Ca(OH)2溶液中,这导致由PO4官能团部分水解形成薄涂层,在1.5x模拟体液(SBF)溶液中浸泡仅一天后,其表面就会刺激磷酸钙涂层的生长。Ca(OH)2处理后的薄层在浸泡于1.5x SBF溶液后,起到了进一步磷酸钙沉积的成核层作用。EDX测量的在1.5x SBF溶液中Ca(OH)2处理的磷酸化几丁质涂层的Ca:P比表明,形成了缺钙磷灰石。