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制备羟基磷灰石的贝壳种类优选及方法比较
田璐琦1,2, 杨皓月1,3, 邢荣娥1,4,3, 刘松1,4,3, 李克成1,4,3, 于华华1,4,3, 李鹏程1,4,3
1.中国科学院海洋研究所 实验海洋生物学重点实验室, 山东 青岛 266071;2.中国科学院大学, 北京 100049;3.中国科学院海洋大科学研究中心, 山东 青岛 266071;4.青岛海洋科学与技术国家实验室 海洋药物与生物制品功能实验室, 山东 青岛 266237
摘要:
本研究以CaO、煅烧后的牡蛎壳、蛤蜊壳、扇贝壳和脉红螺壳为原料, 分别采用反相微乳液法和聚乙二醇(PEG)辅助微波加热法制备了纳米羟基磷灰石(HA), 并从产物的物理化学特性以及形态学参数方面进行比较。利用傅里叶变换红外光谱、X射线衍射对各组产物进行了化学表征, 扫描电子显微镜观察样品的表面形貌, Zeta电位仪测定样品表面的电势差。结果表明, 反相微乳液法制备的HA尺寸在(104.10±1.95) nm至(207.90±3.75) nm范围内, 为近球形颗粒; 而PEG辅助微波加热法制备得到的HA尺寸在(61.17±3.11) nm与(182.70±1.05) nm范围内, 倾向于形成椭圆及棒状的颗粒, 稳定性更高, 且各组样品均表现出完全的亲水性。此外, 对比于CaO制备的HA, 以贝壳为原料制备的HA具有更好的纳米结构, 其中利用脉红螺壳制备的HA在粒径大小、稳定性以及亲水性等方面均具有优势, 并且具有更接近天然骨的钙磷比。因此脉红螺壳可以作为PEG辅助微波加热法制备羟基磷灰石的主要原料。
关键词:  贝壳  反相微乳液法  微波加热  聚乙二醇  羟基磷灰石
DOI:10.11759/hykx20230303001
分类号:TS209
基金项目:国家重点研发计划项目(2019YFD0902105); 福建省科技计划项目-STS计划(2021T3013); 中国科学院海洋大科学研究中心重点部署项目(技术研发类)(COMS2020J04)
Comparison of raw materials and preparation methods for seashell hydroxyapatite
TIAN Luqi1,2, YANG Haoyue1,3, XING Ronge1,4,3, LIU Song1,4,3, LI Kecheng1,4,3, YU Huahua1,4,3, LI Pengcheng1,4,3
1.Key Laboratory of Experimental Marine Biology, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China;2.University of Chinese Academy of Sciences, Beijing 100049, China;3.Marine Research Center, Chinese Academy of Sciences, Qingdao 266071, China;4.National Laboratory of Marine Science and Technology, Qingdao 266237, China
Abstract:
In the present study, we used CaO and calcined oyster, clam, scallop, and snail shells as raw materials to synthesize nanohydroxyapatite (HA) using the reverse-phase microemulsion method and polyethylene glycol (PEG)-assisted microwave heating and compared the physicochemical characteristics and morphological parameters of HA. Fourier transform infrared spectroscopy and X-ray powder diffraction were used to characterize the product, scanning electron microscopy was employed to observe the surface morphology, and a Zeta potential analyzer was utilized for potential determination. The results showed that HA fabricated using the reverse-phase microemulsion method had a particle size between (104.10 ±1.95) and (207.90 ±3.75) nm and a sphere-like morphology; however, HA prepared using the PEG-assisted microwave method presented a smaller particle size that varied from (61.17 ±3.11) to (182.70 ±1.05) nm and tended to have an oval-like and rod-like shape, while showing better stability and hydrophilicity. In addition, compared with chemically synthesized HA, HA derived from seashells had a better nanostructure, and HA derived from snail shells outperformed others in terms of particle size, stability, and wettability. Furthermore, the Ca/P ratio of snail-shell HA was closer to that of the natural bone. Therefore, snail shells can be used as the main raw material for synthesizing HA using the PEG-assisted microwave method.
Key words:  sea shells  microemulsion method  microwave heating  polyethylene glycol  hydroxyapatite
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