This is an unedited manuscript accepted for publication and provided as an Article in Press for early access at the author’s request. The article will undergo copyediting, typesetting, and galley proof review before final publication. Please be aware that errors may be identified during production that could affect the content. All legal disclaimers of the journal apply.
Subhasis Nath,
Sujan Krishna Samanta,
Sourav Debnath,
Soumya Mukherjee,
- Principal, Department of Mechanical Engineering, Central Tool Room and Training Center, Kolkata, West Bengal, India
- Associate Professor, Department of Biomedical Engineering, Netaji Subhash Engineering College, Kolkata, West Bengal, India
- Assistant Professor, Department of Electrical Engineering, Brainware University, Barasat, Kolkata, West Bengal, India
- Assistant Professor, Department of Metallurgical Engineering, Kazi Nazrul University, Asansol, Paschim Bardhaman, West Bengal, India
Abstract
Hydroxyapatite is widely used as a bioceramic material in orthopedic and dental field because of its exceptional biocompatibility and bioactivity. Hydroxyapatite (HAp) doped with several mineral ions has been frequently reported to further enhance its bioactive nature. Several studies indicate that biological waste materials can serve as calcium sources for hydroxyapatite synthesis, with eggshells being one such promising source. In the present work, two types of hydroxyapatite were synthesized: pure hydroxyapatite and 5% magnesium-doped hydroxyapatite (based on weight percentage). Laboratory-grade calcium hydroxide was used for synthetic HAp, while eggshell powder was employed for eggshell-derived HAp. The activity of the developed materials in biological environment was assessed using in vitro methods. Porous ceramic blocks were fabricated by compacting the powders using a hydraulic press and sintering them at 950°C. Powder samples calcined at 800°C were analysed by X-ray diffraction (XRD) to assess the lattice parameters and functional groups identification was done by Fourier transform infrared spectroscopy (FTIR) to identify. Apparent porosity was determined using Archimedes’ principle, confirming the presence of pores in the pellets. Hemolysis studies demonstrated that the synthesized materials are hemocompatible. Simulated body fluid (SBF) studies confirmed the appearance of apatite layer on the sintered pellets, establishing the bioactive and interactive nature of the developed materials.
Keywords: Hydroxyapatite, Eggshell waste, Lattice parameter, Surface morphology, In vitro biocompatibility.
Subhasis Nath, Sujan Krishna Samanta, Sourav Debnath, Soumya Mukherjee. Fabrication and Comparative Study of Synthetic and Eggshell Waste Derived Hydroxyapatite-Based Composites for Biomedical Applications. Journal of Polymer & Composites. 2026; 14(03):-.
Subhasis Nath, Sujan Krishna Samanta, Sourav Debnath, Soumya Mukherjee. Fabrication and Comparative Study of Synthetic and Eggshell Waste Derived Hydroxyapatite-Based Composites for Biomedical Applications. Journal of Polymer & Composites. 2026; 14(03):-. Available from: https://journals.stmjournals.com/jopc/article=2026/view=242961
References
[1] Ayrilmis N, Kanat G, Yildiz Avsar E, Palanisamy S, Ashori A. Utilizing waste manhole covers and fibreboard as reinforcing fillers for thermoplastic composites. Journal of Reinforced Plastics and Composites. 2025;44(17-18):1108-1118. doi:10.1177/07316844241238507
[2] Bhuvaneshwaran Mylsamy, Karthik Aruchamy, Senthil Kumar Marudhamuthu Shanmugam, Sivasubramanian Palanisamy, Nadir Ayrilmis, “Improving performance of composites: Natural and synthetic fibre hybridisation techniques in composite materials – A review,” Materials Chemistry and Physics, Volume 334, 1 April 2025, 130439. https://doi.org/10.1016/j.matchemphys.2025.130439
[3] Murugesan Palaniappan, Sivasubramanian Palanisamy, Thulasi mani Murugesan, Srinivas Tadepalli, Rashid Khan, Sabbah Ataya, Influence of Washing with Sodium Lauryl Sulphate (SLS) Surfactant on Different Properties of Ramie Fibres, BioResources, 19(2), 2609-2625, 2024. DOI: 10.15376/biores.19.2.2609-2625
[4] Karuppusamy Manickaraj, Ramakrishnan Thirumalaisamy, Sivasubramanian Palanisamy, Nadir Ayrilmis, Ehab El Sayed Massoud, Murugesan Palaniappan, S. Lakshmi Sankar, Value-added utilization of agricultural wastes in biocomposite production: Characteristics and applications, Ann NY Acad Sci., 1549, 72–91, 2025. https://doi.org/10.1111/nyas.15368
[5] Sivasubramanian Palanisamy, Mayandi Kalimuthu, Shanmugam Dharmalingam, Azeez Alavudeen, Rajini Nagarajan, Sikiru Oluwarotimi Ismail, Suchart Siengchin, Faruq Mohammad and Hamad A, Al-Lohedan6Effects of fiber loadings and lengths on mechanical properties of Sansevieria Cylindrica fiber reinforced natural rubber biocomposites, Materials Research Express, Mater. Res. Express 10 (2023) 085503, pp. 2-13, 2023. https://doi.org/10.1088/2053-1591/acefb0
[6] Rajkumar Ramasubbu, Arumugam Kayambu, Sivasubramanian Palanisamy, and Nadir Ayrilmis, Mechanical Properties of Epoxy Composites Reinforced with Areca catechu Fibers Containing Silicon Carbide, BioResources 19(2), 2353-2370, 2024. DOI: 10.15376/biores.19.2.2353-2370
[7] J. Henkel, M.A. Woodruff, D.R. Epari, R. Steck, V. Glatt, I.C. DIckinson, P.F.M. Choong, M.A. Schuetz, Di.W. Hutmacher, Bone Regeneration Based on Tissue Engineering Conceptions-A 21st Century Perspective, Bone Research. 1 (2013) 216–248. https://doi.org/10.4248/BR201303002.
[8] T.S.B. Narasaraju, D.E. Phebe, Some physico-chemical aspects of hydroxylapatite, Journal of Materials Science. 31 (1996) 1–21. https://doi.org/10.1007/BF00355120.
[9] J.F. Shackelford, Bioceramics – current status and future trends, Materials Science Forum. 293 (1999) 99–106. https://doi.org/10.4028/www.scientific.net/msf.293.99.
[10] M.H. Santos, M. de Oliveira, L.P. de F. Souza, H.S. Mansur, W.L. Vasconcelos, Synthesis control and characterization of hydroxyapatite prepared by wet precipitation process, Materials Research. 7 (2004) 625–630. https://doi.org/10.1590/s1516-14392004000400017.
[11] B. Nasiri-Tabrizi, P. Honarmandi, R. Ebrahimi-Kahrizsangi, P. Honarmandi, Synthesis of nanosize single-crystal hydroxyapatite via mechanochemical method, Materials Letters. 63 (2009) 543–546. https://doi.org/10.1016/j.matlet.2008.11.030.
[12] A. Borello, A. Deptuła, W. Łada, T. Olczak, C. Alvani, A. Di Bartolomeo, NON-CRYSTALLINE SOLIDS Preparation of spherical powders of hydroxyapatite, Journal of Non-Crystalline Solids. 148 (1992) 537–541.
[13] S. Pramanik, A.K. Agarwal, K.N. Rai, A. Garg, Development of high strength hydroxyapatite by solid-state-sintering process, Ceramics International. 33 (2007) 419–426. https://doi.org/10.1016/j.ceramint.2005.10.025.
[14] T.S. Sampath Kumar, I. Manjubala, J. Gunasekaran, Synthesis of carbonated calcium phosphate ceramics using microwave irradiation, Biomaterials. 21 (2000) 1623–1629. https://doi.org/10.1016/S0142-9612(00)00014-4.
[15] H.S. Liu, T.S. Chin, L.S. Lai, S.Y. Chiu, K.H. Chung, C.S. Chang, M.T. Lui, Hydroxyapatite synthesized by a simplified hydrothermal method, Ceramics International. 23 (1997) 19–25. https://doi.org/10.1016/0272-8842(95)00135-2.
[16] T.J. Webster, E.A. Massa-Schlueter, J.L. Smith, E.B. Slamovich, Osteoblast response to hydroxyapatite doped with divalent and trivalent cations, Biomaterials. 25 (2004) 2111–2121. https://doi.org/10.1016/j.biomaterials.2003.09.001.
[17] N. Murugan, C. Murugan, A.K. Sundramoorthy, In vitro and in vivo characterization of mineralized hydroxyapatite/polycaprolactone-graphene oxide based bioactive multifunctional coating on Ti alloy for bone implant applications, Arabian Journal of Chemistry. 11 (2018) 959–969. https://doi.org/10.1016/j.arabjc.2018.03.020.
[18] I. Cacciotti, A. Bianco, M. Lombardi, L. Montanaro, Mg-substituted hydroxyapatite nanopowders: Synthesis, thermal stability and sintering behaviour, Journal of the European Ceramic Society. 29 (2009) 2969–2978. https://doi.org/10.1016/j.jeurceramsoc.2009.04.038.
[19] A. Bigi, G. Falini, E. Foresti, A. Ripamonti, M. Gazzano, N. Roveri, Magnesium influence on hydroxyapatite crystallization, Journal of Inorganic Biochemistry. 49 (1993) 69–78. https://doi.org/10.1016/0162-0134(93)80049-F.
[20] E. Landi, A. Tampieri, M. Mattioli-Belmonte, G. Celotti, M. Sandri, A. Gigante, P. Fava, G. Biagini, Biomimetic Mg- and Mg,CO3-substituted hydroxyapatites: synthesis characterization and in vitro behaviour, Journal of the European Ceramic Society. 26 (2006) 2593–2601. https://doi.org/10.1016/j.jeurceramsoc.2005.06.040.
[21] J. Kolmas, A. Jaklewicz, A. Zima, M. Bućko, Z. Paszkiewicz, J. Lis, A. Ślósarczyk, W. Kolodziejski, Incorporation of carbonate and magnesium ions into synthetic hydroxyapatite: The effect on physicochemical properties, Journal of Molecular Structure. 987 (2011) 40–50. https://doi.org/10.1016/j.molstruc.2010.11.058.
[22] E. Landi, A. Tampieri, G. Celotti, S. Sprio, Densification behaviour and mechanisms of synthetic hydroxyapatites, Journal of the European Ceramic Society. 20 (2000) 2377–2387. https://doi.org/10.1016/S0955-2219(00)00154-0.
[23] Y. Yajing, D. Qiongqiong, H. Yong, S. Han, X. Pang, Magnesium substituted hydroxyapatite coating on titanium with nanotublar TiO 2 intermediate layer via electrochemical deposition, Applied Surface Science. 305 (2014) 77–85. https://doi.org/10.1016/j.apsusc.2014.02.163.
[24] C.M. Serre, M. Papillard, P. Chavassieux, J.C. Voegel, G. Boivin, Influence of magnesium substitution on a collagen–apatite biomaterial on the production of a calcifying matrix by human osteoblasts., Journal of Biomedical Materials Research. 42 (1998) 626–633. https://doi.org/10.1002/(sici)1097-4636(19981215)42:43.3.co;2-j.
[25] M. Mehrjoo, J. Javadpour, M. Ali Shokrgozar, M. Farokhi, S. Javadian, S. Bonakdar, Effect of magnesium substitution on structural and biological properties of synthetic hydroxyapatite powder, Materials Express. 5 (2015) 41–48. https://doi.org/10.1166/mex.2015.1205.
[26] J.E. Jones, R. Schwartz, L. Krook, Calcium homeostasis and bone pathology in magnesium deficient rats, Calcified Tissue International. 31 (1980) 231–238. https://doi.org/10.1007/BF02407186.
[27] E. Landi, G. Logroscino, L. Proietti, A. Tampieri, M. Sandri, S. Sprio, Biomimetic Mg-substituted hydroxyapatite: From synthesis to in vivo behaviour, Journal of Materials Science: Materials in Medicine. 19 (2008) 239–247. https://doi.org/10.1007/s10856-006-0032-y.
[28] D. Milovac, T.C. Gamboa-Martínez, M. Ivankovic, G. Gallego Ferrer, H. Ivankovic, PCL-coated hydroxyapatite scaffold derived from cuttlefish bone: In vitro cell culture studies, Materials Science and Engineering C. 42 (2014) 264–272. https://doi.org/10.1016/j.msec.2014.05.034.
[29] M. Akram, R. Ahmed, I. Shakir, W.A.W. Ibrahim, R. Hussain, Extracting hydroxyapatite and its precursors from natural resources, Journal of Materials Science. 49 (2014) 1461–1475. https://doi.org/10.1007/s10853-013-7864-x.
[30] A. Ruksudjarit, K. Pengpat, G. Rujijanagul, T. Tunkasiri, Synthesis and characterization of nanocrystalline hydroxyapatite from natural bovine bone, Current Applied Physics. 8 (2008) 270–272. https://doi.org/10.1016/j.cap.2007.10.076.
[31] J. Sang Cho, S.H. Um, D. Su Yoo, Y.C. Chung, S. Hye Chung, J.C. Lee, S.H. Rhee, Enhanced osteoconductivity of sodium-substituted hydroxyapatite by system instability, Journal of Biomedical Materials Research – Part B Applied Biomaterials. 102 (2014) 1046–1062. https://doi.org/10.1002/jbm.b.33087.
[32] S.S. Rahavi, O. Ghaderi, A. Monshi, M.H. Fathi, A comparative study on physicochemical properties of hydroxyapatite powders derived from natural and synthetic sources, Russian Journal of Non-Ferrous Metals. 58 (2017) 276–286. https://doi.org/10.3103/S1067821217030178.
[33] H.L. Jaber, A.S. Hammood, N. Parvin, Synthesis and characterization of hydroxyapatite powder from natural Camelus bone, Journal of the Australian Ceramic Society. 54 (2018) 1–10. https://doi.org/10.1007/s41779-017-0120-0.
[34] A.M. Janus, M. Faryna, K. Haberko, A. Rakowska, T. Panz, Chemical and microstructural characterization of natural hydroxyapatite derived from pig bones, Microchimica Acta. 161 (2008) 349–353. https://doi.org/10.1007/s00604-007-0864-2.
[35] E.A. Ofudje, A. Rajendran, A.I. Adeogun, M.A. Idowu, S.O. Kareem, D.K. Pattanayak, Synthesis of organic derived hydroxyapatite scaffold from pig bone waste for tissue engineering applications, Advanced Powder Technology. 29 (2018) 1–8. https://doi.org/10.1016/j.apt.2017.09.008.
[36] A. Pal, S. Paul, A.R. Choudhury, V.K. Balla, M. Das, A. Sinha, Synthesis of hydroxyapatite from Lates calcarifer fish bone for biomedical applications, Materials Letters. 203 (2017) 89–92. https://doi.org/10.1016/j.matlet.2017.05.103.
[37] R. Murugan, S. Ramakrishna, Crystallographic study of hydroxyapatite bioceramics derived from various sources, Crystal Growth and Design. 5 (2005) 111–112. https://doi.org/10.1021/cg034227s.
[38] W.F. Ho, H.C. Hsu, S.K. Hsu, C.W. Hung, S.C. Wu, Calcium phosphate bioceramics synthesized from eggshell powders through a solid state reaction, Ceramics International. 39 (2013) 6467–6473. https://doi.org/10.1016/j.ceramint.2013.01.076.
[39] Y. Shi, H. Ke, J. Xie, H. Tan, G. Luo, B. Xu, G. Abakari, Jo u pr oo f, Geoderma Regional. (2020) e00484. https://doi.org/10.1016/j.algal.2023.103165.
[40] L. Dupoirieux, D. Pourquier, F. Souyris, Powdered eggshell: a pilot study on a new bone substitute for use in maxillofacial surgery, Journal of Cranio-Maxillofacial Surgery. 23 (1995) 187–194. https://doi.org/10.1016/S1010-5182(05)80009-5.
[41] S. Sasikumar, R. Vijayaraghavan, Low temperature synthesis of nanocrystalline hydroxyapatite from egg shells by combustion method, Trends in Biomaterials and Artificial Organs. 19 (2006) 70–73.
[42] Anushika, P. Sharma, A. Trivedi, H. Begam, Synthesis and characterization of pure and titania doped hydroxyapatite, Materials Today: Proceedings. 16 (2019) 302–307. https://doi.org/10.1016/j.matpr.2019.05.094.
[43] T. Kokubo, H. Takadama, How useful is SBF in predicting in vivo bone bioactivity?, Biomaterials. 27 (2006) 2907–2915. https://doi.org/10.1016/j.biomaterials.2006.01.017.
[44] ASTM F 756-00, Standard practice for assessment of hemolytic properties of materials. Philadelphia, American Society for Testing and Materials. (2000) 5. https://doi.org/10.1520/F0756-13.

Journal of Polymer & Composites
| Volume | 14 |
| 03 | |
| Received | 15/03/2026 |
| Accepted | 31/03/2026 |
| Published | 05/05/2026 |
| Publication Time | 51 Days |
Login
PlumX Metrics