Mesoporous Whitlockite: Synthesis, characterization, and in vitro biocompatibility for bone tissue engineering applications

Q1 Medicine

Journal of oral biology and craniofacial research Pub Date : 2025-09-03 DOI:10.1016/j.jobcr.2025.09.002

J.S. Sharukh , Sinduja Palati , Saravanan Sekaran , Dhanraj Ganapathy

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引用次数: 0

Abstract

Background

Whitlockite (WH) is a magnesium-containing calcium phosphate mineral that occurs naturally in bone and teeth. Its biological relevance lies in its ability to promote osteogenesis and provide mechanical stability, making it a strong candidate for bone repair applications. Introducing mesoporosity into Whitlockite is expected to further enhance its biological activity by increasing surface roughness and surface area, which improves protein adsorption and supports cell growth.

Objective

This work focused on preparing mesoporous Whitlockite (Meso-Wh) through a controlled acid treatment method, followed by detailed structural and surface characterization, and an in vitro evaluation of its cytocompatibility.

Methods

Whitlockite was synthesized using a precipitation–hydrothermal method with calcium nitrate, magnesium nitrate, and diammonium hydrogen phosphate precursors. Mesoporosity was induced by hydrochloric acid treatment (pH 4). The particles were characterized using scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption–desorption studies with BET and BJH analysis. Cytocompatibility was tested by an indirect MTT assay using MG-63 osteoblast-like cells.

Results

SEM images showed that Meso-Wh particles were smaller and rougher compared with untreated Whitlockite. EDS confirmed calcium, phosphorus, oxygen, and magnesium as the major elements. XRD patterns indicated reduced crystallinity in Meso-Wh, and FTIR spectra revealed broadening of phosphate bands, suggesting lattice disorder due to acid treatment. BET analysis gave a surface area of 63.07 m²/g, while BJH pore distribution confirmed mesopores mainly in the 2–5 nm range. MTT results showed good cytocompatibility, with high cell viability at 25–75 % extract dilutions and a slight decrease at 100 %. The positive control exhibited marked cytotoxicity.

Conclusion

Acid treatment effectively produced mesoporous Whitlockite with enhanced surface area and nanoscale porosity, without altering its chemical composition, indicating its suitability for further development as a bone tissue engineering scaffold.

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介孔惠特洛克石：骨组织工程应用的合成、表征和体外生物相容性

whitlockite （WH）是一种含镁的磷酸钙矿物，自然存在于骨骼和牙齿中。其生物学相关性在于其促进成骨和提供机械稳定性的能力，使其成为骨修复应用的强有力的候选者。将介孔引入Whitlockite有望通过增加表面粗糙度和表面积来进一步提高其生物活性，从而改善蛋白质吸附并支持细胞生长。目的采用可控酸处理法制备介孔惠特洛克石（Meso-Wh），对其进行详细的结构和表面表征，并对其体外细胞相容性进行评价。方法以硝酸钙、硝酸镁、磷酸氢二铵为前驱物，采用沉淀-水热法制备惠特洛克石。盐酸（pH = 4）诱导介孔。采用扫描电子显微镜（SEM）、能谱仪（EDS）、x射线衍射仪（XRD）、傅里叶变换红外光谱（FTIR）对颗粒进行了表征，并用BET和BJH分析进行了氮的吸附-脱附研究。采用MG-63成骨样细胞间接MTT法检测细胞相容性。结果sem图像显示，与未处理的Whitlockite相比，Meso-Wh颗粒更小，更粗糙。EDS证实钙、磷、氧和镁是主要元素。XRD谱图显示，介观- wh的结晶度降低，FTIR谱图显示磷酸盐谱带变宽，表明酸处理导致晶格紊乱。BET分析得到的比表面积为63.07 m2/g，而BJH孔分布证实中孔主要分布在2-5 nm范围内。MTT结果显示细胞相容性良好，25 - 75%浓度时细胞活力高，100%浓度时细胞活力略有下降。阳性对照表现出明显的细胞毒性。结论酸处理可有效制备介孔Whitlockite，在不改变其化学成分的情况下，增加了其表面积和纳米级孔隙度，表明其适合作为骨组织工程支架进一步发展。

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来源期刊

Journal of oral biology and craniofacial research Medicine-Otorhinolaryngology

CiteScore

4.90

自引率

0.00%

发文量

133

审稿时长

167 days

期刊介绍： Journal of Oral Biology and Craniofacial Research (JOBCR)is the official journal of the Craniofacial Research Foundation (CRF). The journal aims to provide a common platform for both clinical and translational research and to promote interdisciplinary sciences in craniofacial region. JOBCR publishes content that includes diseases, injuries and defects in the head, neck, face, jaws and the hard and soft tissues of the mouth and jaws and face region; diagnosis and medical management of diseases specific to the orofacial tissues and of oral manifestations of systemic diseases; studies on identifying populations at risk of oral disease or in need of specific care, and comparing regional, environmental, social, and access similarities and differences in dental care between populations; diseases of the mouth and related structures like salivary glands, temporomandibular joints, facial muscles and perioral skin; biomedical engineering, tissue engineering and stem cells. The journal publishes reviews, commentaries, peer-reviewed original research articles, short communication, and case reports.