The electrospun poly(ε‐caprolactone)/fluoridated hydroxyapatite nanocomposite for bone tissue engineering

Biodegradable cell‐incorporated scaffolds can guide the regeneration process of bone defects such as physiological resorption, tooth loss, and trauma which medically, socially, and economically hurt patients. Here, 0, 5, 10, and 15 wt% fluoridated hydroxyapatite (FHA) nanoparticles containing 25 wt% F^? and 75 wt% OH^? were incorporated into poly(ε‐caprolactone) (PCL) matrix to produce PCL/FHA nanocomposite scaffolds using electrospinning method. Then, scanning electron microscopy (SEM), X‐ray diffraction (XRD) pattern, and Fourier transform infrared spectroscopy (FTIR) were used to evaluate the morphology, phase structure, and functional groups of prepared electrospun scaffolds, respectively. Furthermore, the tensile strength and elastic modulus of electrospun scaffolds were investigated using the tensile test. Moreover, the biodegradation behavior of electrospun PCL/FHA scaffolds was studied by the evaluation of weight loss of mats and the alternation of pH in phosphate buffer saline (PBS) up to 30 days of incubation. Then, the biocompatibility of prepared mats was investigated by culturing MG‐63 osteoblast cell line and performing MTT assay. In addition, the adhesion of osteoblast cells on prepared electrospun scaffolds was studied using their SEM images. Results revealed that the fiber diameter of prepared electrospun PCL/FHA scaffolds alters between 700 and 900 nm. The mechanical assay illustrated the mat with 10 wt% FHA nanoparticles revealed the highest tensile strength and elastic modulus. The weight loss alternation of mats determined around 1% to 8% after 30 days of incubation. The biocompatibility and cell adhesion of mats improved by increasing the amounts of FHA nanoparticles.     

Raman Spectroscopy of Natural Bone and Synthetic Apatites

Abstract

Raman spectroscopy of natural bones and hydroxyapatites is described. In addition, how Raman spectroscopy has proved crucial in providing baseline data for the modification of synthetic apatite powders that are routinely used now as bone replacement materials is explained. It is important to understand the chemical structural properties of natural bone. Bone consists of two primary components: an inorganic or mineral phase, which is mainly a carbonated form of a nanoscale crystalline calcium phosphate, closely resembling hydroxyapatite, and an organic phase, which is composed largely of type I collagen fibers. Other constituents of bone tissue include water and organic molecules such as glycosaminoglycans, glycoproteins, lipids, and peptides. Ions such as sodium, magnesium, fluoride, and citrate are also present, as well as hydrogenophosphate. Hence, the mineral phase in bone may be characterized essentially as nonstoichiometric substituted apatite. Such a distinction is important in the development of synthetic calcium phosphates for application as skeletal implants. An understanding of bone function and its interfacial relationship to an implant clearly depends on the associated structure and composition. Therefore, it is essential to fully understand the chemical composition of bone, and Raman spectroscopy is an excellent technique for such an analysis.     

Composites of Hydroxyapatite Whiskers/poly(L-lactide-co-glycolide) with High Tensile Plasticity

Hydroxyapatite whiskers (HAW) with a maximum aspect ratio of 20 were employed to improve the toughness of poly(L-lactide-co-glycolide) (PLGA). 3-Aminopropyltriethoxysilane (AMEO) was grafted on the surface of the hydroxyapatite whiskers (g-HAW) to improve its wetting in the PLGA matrix. Composites based on HAW, g-HAW, and PLGA were prepared. The structure and properties of the composites were subsequently investigated by powder X-ray diffraction (XRD), scanning electron microscopy, differential scanning calorimetry, and tensile testing. The g-HAW were distributed homogenously in the PLGA matrix because of improved wetting of g-HAW while the HAW were aggregated. The stronger interfacial bonding also gave rise to improved mechanical properties of the g-HAW/PLGA composites. The HAW/PLGA and g-HAW/PLGA composites failed in a tough manner with intensive plastic deformation. The g-HAW/PLGA composite (5 wt% g-HAW) failed at a maximum elongation of 366%, although the tensile strength dropped slightly. The g-HAW/PLGA composite (1 wt% g-HAW) maintained the initial tensile strength of neat PLGA but failed at an equally high elongation of 347%, whereas PLGA failed at an elongation of 11%.     

Properties of Polyamide-6 Composites Reinforced with Hydroxyapatite Nanospheres

Hydroxyapatite nanospheres (nHA) were first synthesized from (NH₄)₂HPO₄ and CaCl₂ precursors in the presence of poly(vinyl alcohol) templates. The structure and morphology of as-synthesized products were examined by materials characterization techniques. X-ray diffraction patterns and Fourier transform infrared spectra showed that the nHA (50–70 nm) exhibit the crystalline structure and vibration bands of HA. The Ca/P molar ratio of nHA approached the stoichiometric value of 1.67. The nHA were then melt blended with polyamide-6 (PA6), followed by injection molding. Tensile and flexural measurements showed that the tensile and bending strengths of injection molded PA6–10 wt% nHA composite were close to those of human cortical bone. A simulated body fluid immersion test revealed that apatite crystals can be readily deposited on the PA6–10 wt% nHA composite surface after immersion for 30 days.     

纳米羟基磷灰石-聚(己内酯-丙交酯)共聚物复合材料

通过纳米羟基磷灰石(HA)的羟基引发ε-已内酯(ε-CL)开环聚合,再接枝不同量的丙交酯(LA),制备了HA-P(CL-LA)复合材料.采用TEM、FT-IR、~1H-NMR、~(13)C-NMR等对复合物的结构进行了表征.结果表明:HA在复合物中的分散较均匀,并且保持了原来的针状或棒状形貌;共聚物中n(ε-CL)/n(LA)随着单体投料中n(ε-CL)/n(LA)的增加而增加;样品在制备过程中没有发生丙交酯与己内酯之间的酯交换,只发生了丙交酯自身的酯交换,共聚物中丙交酯链段主要以全同序列为主.     

Dissolution kinetic and structural behaviour of natural hydroxyapatite vs. thermal treatment Comparison to synthetic hydroxyapatite

The dissolution kinetic and structural behaviour of natural hydroxyapatite (N-HA) and synthetic hydroxyapatite (S-HA) was studied vs. sintering temperature and using ‘in vitro’ experiments. Obtained results highlight the chemical stability of N-HA. Any structural modification was observed until 1200°C. In the fact S-HA undergoes some modifications. XRD diagrams show the tricalcium phosphate (TCP) phase formation between 800 and 1100°C and tetracalcium phosphate (TetCP) phase formation at 1200°C. The ‘in vitro’ assay shows that the dissolution was occurred more in N-HA than in S-HA. The formed TCP activated the dissolution kinetic and then the precipitation phenomena when a continuous dissolution of TetCP leaded to slow down the kinetic precipitation.     

类牙釉状丝胶蛋白/羟基磷灰石复合材料的合成及表征

采用化学沉淀法合成了丝胶蛋白(SS)/羟基磷灰石(HAP)复合材料, 并研究了矿化时间对复合材料的影响. X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、透射电镜(TEM/HRTEM)和扫描电镜(SEM)表征结果表明: 在较短的矿化时间内, 合成的SS/HAP为直径约20 nm的复合颗粒; 随着矿化时间的延长, 这些复合颗粒能够沿轴方向组装并融合成类牙釉结构的较大晶体. 文章讨论了其可能的组装机制.     

羟基磷灰石/离子液体混合膜修饰电极的制备及其应用于水中痕量镉离子的高选择性测定

利用溴代十六烷基三甲基铵(CTAB)为模板, 合成制备了棒状羟基磷灰石颗粒, 并以SEM, XRD, IR等手段进行了表征. 用制备的羟基磷灰石与自制的离子液体([BMIM]PF6)充分混合涂覆在玻碳电极表面制备了羟基磷灰石/离子液体修饰电极, 研究了镉离子在该修饰电极上的富集和电化学行为. 结果发现, 羟基磷灰石对镉离子有较好的富集作用, 而离子液体则可以在开路条件下使镉离子还原为金属镉, 氧化扫描时可以得到镉的灵敏氧化溶出峰, 以此为基础建立了一种高选择性地测定痕量镉离子的新方法, 该方法可以较好地避免铅、汞、银等重金属离子的干扰, 对镉离子检出限可达2.0×10－8 mol•L－1, 在4.0×10－8～2.2×10－7 mol•L－1的浓度范围内, 氧化溶出峰电流与Cd(II)的浓度呈良好的线性关系. 该研究有望在环境检测和环境治理方面发挥重要作用.     

珊瑚水热转换羟基磷灰石中的影响因素

分别在不同的反应温度、不同的pH值、加矿化剂与否的条件下,将滨珊瑚水热转换为珊瑚羟基磷灰石。利用X射线衍射（XRD）、扫描电子显微镜（SEM）分别对产物和中间产物的物相和微结构进行了分析。发现不同条件下存在有不同的反应路径。考察了反应温度、pH值和矿化剂对珊瑚水热反应的影响。     

Porous Calcium Hydroxyapatite as an Efficient Catalyst for Synthesis of Pyrazolines via 1,3‐Dipolar Cycoloaddition Under Solvent‐Free Microwave Irradiation

Adsorbed on porous calcium hydroxyapatite, 1,3‐dipolar cycloaddition of diphenylnitrilimine on olefins is readily catalyzed under solvent‐free microwaves irradiation. The pyrazolines are obtained in few minutes with high yields. Specific surface of porous calcium hydroxyapatite and microwaves effects are discussed.