Sains Malaysiana 55(7)(2026): 1198-1210

http://doi.org/10.17576/jsm-2026-5507-08

 

Physicochemical Characteristics of Hydroxyapatite/Beta-Tricalcium Phosphate from Pinctada maxima Shells for Resorbable Bone Matrix Candidate

(Ciri Fizikokimia Hidroksiapatit/Beta-Trikalsium Fosfat daripada Cangkerang Pinctada maxima untuk Calon Matriks Tulang Boleh Serap)

 

AHMAD TAUFIK S^1,*, SUSI RAHAYU^2,3, MOHAMMAD RIZKI¹, M. MUKADDAM ALAYDRUS¹, I GUSTI AYU SRI ANDAYANI¹, IRNAWATI² & MUHAMAD ALI⁴

 

¹Department of Medical Sciences, Faculty of Medicine and Health Sciences, University of Mataram, Mataram, 83125, West Nusa Tenggara, Indonesia 

²Department of Physics, Faculty of Mathematics and Natural Sciences, University of Mataram, Mataram, 83125, West Nusa Tenggara, Indonesia

³Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Brawijaya, Malang, 65145, East Java, Indonesia

⁴Department of Animal Sciences, Faculty of Animal Sciences, University of Mataram, Mataram, 83125, West Nusa Tenggara, Indonesia

 

Diserahkan: 26 September 2025/Diterima: 29 Jun 2026

 

Abstract

The valorization of Pinctada maxima shell waste as a calcium source offers a sustainable route for developing calcium phosphate bioceramics. This study evaluated the effect of post-synthesis calcination duration on the physicochemical properties of hydroxyapatite/β-tricalcium phosphate (HAp/β-TCP) powders derived from Pinctada maxima shells. Shell-derived CaO was used as the calcium precursor, followed by wet precipitation to obtain calcium phosphate precursors and post-synthesis calcination at 700 °C for 3, 6, 9, and 12 h. The resulting powders were characterized using EDX, proximate analysis, FTIR, XRD, PSA, and SEM. The Ca/P ratios varied with calcination duration, with values of 1.70, 1.61, 1.54, and 1.53 for Samples A, B, C, and D, respectively. Proximate analysis showed high inorganic purity, indicated by low moisture content (0.01-0.08%), high ash content (99.93-99.99%), and negligible fat residues (0.0236-0.0457%). FTIR confirmed the presence of PO₄³⁻ and OH⁻ functional groups, while XRD qualitatively confirmed the coexistence of HAp and β-TCP phases. Among the tested conditions, the 9 h calcination treatment (Sample C) showed the most promising overall physicochemical profile, with a Ca/P ratio of 1.54, distinct HAp/β-TCP diffraction features, favourable crystallographic parameters, and a coherent particle size distribution (mean = 96.61 µm; D50 = 101.10 µm). SEM observations supported the PSA results, showing granular aggregates and irregular agglomerates typical of wet-synthesized calcium phosphate powders. However, quantitative HAp:β-TCP phase fractions were not determined; therefore, Rietveld refinement or the RIR method is required to confirm phase optimization. Overall, Pinctada maxima shell waste shows potential as a sustainable precursor for HAp/β-TCP powder development, although biological, mechanical, and benchmark evaluations are still needed before clinical applicability can be established.

Keywords: Biphasic calcium phosphate; calcination duration; HAp/β-TCP; marine-derived biomaterial; particle agglomeration; Pinctada maxima shell

 

Abstrak

Valorisasi sisa cangkerang Pinctada maxima sebagai sumber kalsium menawarkan pendekatan mampan untuk membangunkan bioseramik kalsium fosfat. Kajian ini menilai kesan tempoh pengkalsinan pascasintesis terhadap sifat fizikokimia serbuk hidroksiapatit/β-trikalsium fosfat (HAp/β-TCP) yang diperoleh daripada cangkerang Pinctada maxima. CaO terbitan cangkerang digunakan sebagai prekursor kalsium, diikuti kaedah pemendakan basah untuk menghasilkan prekursor kalsium fosfat dan pengkalsinan pascasintesis pada suhu 700 °C selama 3, 6, 9 dan 12 jam. Serbuk yang terhasil dicirikan menggunakan EDX, analisis proksimat, FTIR, XRD, PSA dan SEM. Nisbah Ca/P berubah mengikut tempoh pengkalsinan dengan nilai 1.70, 1.61, 1.54 dan 1.53 masing-masing bagi Sampel A, B, C dan D. Analisis proksimat menunjukkan ketulenan tak organik yang tinggi, ditunjukkan oleh kandungan lembapan yang rendah (0.01-0.08%), kandungan abu yang tinggi (99.93-99.99%) dan sisa lemak yang boleh diabaikan (0.0236-0.0457%). FTIR mengesahkan kehadiran kumpulan berfungsi PO₄³⁻ dan OH⁻, manakala XRD secara kualitatif mengesahkan kewujudan bersama fasa HAp dan β-TCP. Antara keadaan yang diuji, rawatan pengkalsinan selama 9 jam (Sampel C) menunjukkan profil fizikokimia keseluruhan yang paling berpotensi dengan nisbah Ca/P 1.54, ciri pembelauan HAp/β-TCP yang jelas, parameter kristalografi yang baik dan taburan saiz zarah yang koheren (min = 96.61 µm; D50 = 101.10 µm). Pemerhatian SEM menyokong keputusan PSA dengan menunjukkan agregat bergranul dan aglomerat tidak sekata yang lazim bagi serbuk kalsium fosfat yang disintesis melalui kaedah basah. Walau bagaimanapun, pecahan kuantitatif fasa HAp:β-TCP belum ditentukan; oleh itu, penapisan Rietveld atau kaedah RIR diperlukan untuk mengesahkan pengoptimuman fasa. Secara keseluruhan, sisa cangkerang Pinctada maxima menunjukkan potensi sebagai prekursor mampan untuk pembangunan serbuk HAp/β-TCP, namun penilaian biologi, mekanikal dan perbandingan dengan bahan penanda aras masih diperlukan sebelum kebolehgunaan klinikal dapat dipastikan.

Kata kunci: Aglomerasi zarah; biobahan terbitan marin; cangkerang Pinctada maxima; HAp/β-TCP; kalsium fosfat dwifasa; tempoh kalsinasi

 

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*Pengarang untuk surat-menyurat; email: taufik.unram@gmail.com