Skip to main content
SpringerLink
Log in

Fabrication and characterization of hydroxyapatite-strontium/polylactic acid composite for potential applications in bone regeneration

  • Original Paper
  • Published:
Polymer Bulletin Aims and scope Submit manuscript

Abstract

In this study, polylactic acid (PLA) was reinforced with hydroxyapatite (HAp) microparticles and strontium (Sr) powder via the melt extrusion/hot pressing manufacturing process to produce scaffolding materials with bone regeneration potentials. After the fabrication of the materials, the physico-chemical and mechanical characteristics were investigated. The morphology of the precursors for scaffold fabrication and the resulting composites was investigated. The structural characterization showed the semicrystalline nature of the PLA polymer and the characteristic reflections of HAp loading in the polymer matrix. The functional groups of the PLA matrix and the loaded variants showed the characteristic bands of HAp and Sr for the PLA-HAp and PLA-HAp-Sr scaffolding materials, respectively. Moreover, the physical property evaluation showed that with the addition of HAp, the porosity of the PLA-HAp scaffolds was reduced. However, the addition of Sr increased the porosity of the scaffolds, and this can possibly be ascribed to the grain refinement ability of strontium. The mechanical measurement data showed that the inclusion of Sr produced the maximum average Vickers hardness value of 49.1 HV. The composite scaffolds showed bioactivity potentials, thus, they can serve as suitable bone regeneration materials.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. Improta G, Balato G, Romano M, Ponsiglione AM, Raiola E, Russo MA, Cesarelli M (2017) Improving performances of the knee replacement surgery process by applying DMAIC principles. J Eval Clin Pract 23(6):1401–1407

    Article  PubMed  PubMed Central  Google Scholar 

  2. Donate R, Monzón M, Alemán-Domínguez ME (2020) Additive manufacturing of PLA-based scaffolds intended for bone regeneration and strategies to improve their biological properties. E-Polymers 20(1):571–599

    Article  CAS  Google Scholar 

  3. Gritsch L, Conoscenti G, La Carrubba V, Nooeaid P, Boccaccini AR (2019) Polylactide-based materials science strategies to improve tissue-material interface without the use of growth factors or other biological molecules. Mater Sci Eng, C 94:1083–1101

    Article  CAS  Google Scholar 

  4. Akindoyo JO, Beg MD, Ghazali S, Heim HP, Feldmann M (2017) Effects of surface modification on dispersion, mechanical, thermal, and dynamic mechanical properties of injection-moulded PLA-hydroxyapatite composites. Compos A Appl Sci Manuf 103:96–105

    Article  CAS  Google Scholar 

  5. Singhvi MS, Zinjarde SS, Gokhale DV (2019) Polylactic acid: synthesis and biomedical applications. J Appl Microbiol 127(6):1612–1626

    Article  CAS  PubMed  Google Scholar 

  6. Farah S, Anderson DG, Langer R (2016) Physical and mechanical properties of PLA, and their functions in widespread applications—A comprehensive review. Adv Drug Deliv Rev 107:367–392

    Article  CAS  PubMed  Google Scholar 

  7. Reddy M, Ponnamma D, Choudhary R, Sadasivuni KK (2021) A comparative review of natural and synthetic biopolymer composite scaffolds. Polymers 13(7):1105

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  8. Maniruzzaman M, Douroumis D, Joshua S, Martin J (2012) Hot-melt extrusion (HME): from process to pharmaceutical applications. In: Sezer A D (ed) Recent Advances in Novel Drug Carrier Systems. InTech. https://doi.org/10.5772/51582

    Chapter  Google Scholar 

  9. Manavitehrani I, Fathi A, Badr H, Daly S, Negahi Shirazi A, Dehghani F (2016) Biomedical applications of biodegradable polyesters. Polymers 8(1):20

    Article  PubMed  PubMed Central  Google Scholar 

  10. Zheng Y, Pokorski JK (2021) Hot-melt extrusion: an emerging manufacturing method for slow and sustained protein delivery. Wiley Interdiscipl Rev: Nanomed Nanobiotechnol 13(5):e1712

    CAS  Google Scholar 

  11. Ouyang Q, Feng X, Kuang S, Panwar N, Song P, Yang C, Wang ZL (2019) Self-powered, on-demand transdermal drug delivery system driven by triboelectric nanogenerator. Nano Energy 62:610–619

    Article  CAS  Google Scholar 

  12. Shen P, Moriya A, Rajabzadeh S, Maruyama T, Matsuyama H (2013) Improvement of the antifouling properties of poly (lactic acid) hollow fibre membranes with poly (lactic acid)–polyethylene glycol–poly (lactic acid) copolymers. Desalination 325:37–39

    Article  CAS  Google Scholar 

  13. Guvendiren M, Molde J, Soares RM, Kohn J (2016) Designing biomaterials for 3D printing. ACS Biomater Sci Eng 2(10):1679–1693

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  14. Obada DO, Salami KA, Oyedeji AN, Fasanya OO, Suleiman MU, Ibisola BA, Dauda ET (2021) Solution combustion synthesis of strontium-doped hydroxyapatite: effect of sintering and low compaction pressure on the mechanical properties and physiological stability. Mater Lett 304:130613

    Article  CAS  Google Scholar 

  15. Obada DO, Dauda ET, Abifarin JK, Dodoo-Arhin D, Bansod ND (2020) Mechanical properties of natural hydroxyapatite using low cold compaction pressure: effect of sintering temperature. Mater Chem Phys 239:122099

    Article  CAS  Google Scholar 

  16. Bose S, Das C (2013) Preparation and characterization of low-cost tubular ceramic support membranes using sawdust as a pore-former. Mater Lett 110:152–155

    Article  CAS  Google Scholar 

  17. Leyva-Verduzco AA, Castillo-Ortega MM, Chan-Chan LH, Silva-Campa E, Galaz-Méndez R, Vera-Graziano R, Santos-Sauceda I (2020) Electrospun tubes based on PLA, gelatin, and genipin in different arrangements for blood vessel tissue engineering. Polym Bull 77(11):5985–6003

    Article  CAS  Google Scholar 

  18. Zhang Z, Li S, Wang J (2019) Measurement of micro-hardness of the human lower cervical vertebrae in vitro. Chin J Anat Clin 24(5):425–429

    Google Scholar 

  19. Poskus LT, Latempa AMA, Chagas MA, Silva EMD, Leal MPDS, Guimarães JGA (2009) Influence of post-cure treatments on hardness and marginal adaptation of composite resin inlay restorations: an in vitro study. J Appl Oral Sci 17:617–622

    Article  PubMed  PubMed Central  Google Scholar 

  20. Şevik H, Kurnaz SC (2014) The effect of strontium on the microstructure and mechanical properties of Mg–6Al–0.3 Mn–03 Ti–1Sn. J Magnes Alloys 2(3):214–219

    Article  Google Scholar 

  21. Pandithevan P, Saravana Kumar G (2009) Personalized bone tissue engineering scaffold with controlled architecture using fractal tool paths in layered manufacturing. Virtual Phys Prototyp 4(3):165–180

    Article  Google Scholar 

  22. Chu L, Gao H, Cheng T, Zhang Y, Liu J, Huang F, Liu J (2016) A charge-adaptive nanosystem for prolonged and enhanced in vivo antibiotic delivery. Chem Commun 52(37):6265–6268

    Article  CAS  Google Scholar 

  23. Chang C, Peng N, He M, Teramoto Y, Nishio Y, Zhang L (2013) Fabrication and properties of chitin/hydroxyapatite hybrid hydrogels as scaffold nano-materials. Carbohyd Polym 91(1):7–13

    Article  CAS  Google Scholar 

  24. Maji S, Agarwal T, Das J, Maiti TK (2018) Development of gelatin/carboxymethyl chitosan/nano-hydroxyapatite composite 3D macroporous scaffold for bone tissue engineering applications. Carbohyd Polym 189:115–125

    Article  CAS  Google Scholar 

  25. Wüst S, Godla ME, Müller R, Hofmann S (2014) Tunable hydrogel composite with two-step processing in combination with innovative hardware upgrade for cell-based three-dimensional bioprinting. Acta Biomater 10(2):630–640

    Article  PubMed  Google Scholar 

  26. Huang Y, Zhang X, Wu A, Xu H (2016) An injectable nano-hydroxyapatite (n-HA)/glycol chitosan (G-CS)/hyaluronic acid (HyA) composite hydrogel for bone tissue engineering. RSC Adv 6(40):33529–33536

    Article  CAS  Google Scholar 

  27. Saravanan S, Chawla A, Vairamani M, Sastry TP, Subramanian KS, Selvamurugan N (2017) Scaffolds containing chitosan, gelatin and graphene oxide for bone tissue regeneration in vitro and in vivo. Int J Biol Macromol 104:1975–1985

    Article  CAS  PubMed  Google Scholar 

  28. Tripathi A, Saravanan S, Pattnaik S, Moorthi A, Partridge NC, Selvamurugan N (2012) Bio-composite scaffolds containing chitosan/nano-hydroxyapatite/nano-copper–zinc for bone tissue engineering. Int J Biol Macromol 50(1):294–299

    Article  CAS  PubMed  Google Scholar 

  29. Nam J, Huang Y, Agarwal S, Lannutti J (2007) Improved cellular infiltration in electrospun fiber via engineered porosity. Tissue Eng 13(9):2249–2257

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  30. Dhand C, Ong ST, Dwivedi N, Diaz SM, Venugopal JR, Navaneethan B, Lakshminarayanan R (2016) Bio-inspired in situ crosslinking and mineralization of electrospun collagen scaffolds for bone tissue engineering. Biomaterials 104:323–338

    Article  CAS  PubMed  Google Scholar 

  31. Ooi CY, Hamdi M, Ramesh S (2007) Properties of hydroxyapatite produced by annealing of bovine bone. Ceram Int 33(7):1171–1177

    Article  CAS  Google Scholar 

  32. Lowe B, Venkatesan J, Anil S, Shim MS, Kim SK (2016) Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering. Int J Biol Macromol 93:1479–1487

    Article  CAS  PubMed  Google Scholar 

  33. Zhang X, Chen L, Mulholland T, Osswald TA (2019) Characterization of mechanical properties and fracture mode of PLA and copper/PLA composite part manufactured by fused deposition modeling. SN Appl Sci 1(6):1–12

    Article  Google Scholar 

  34. Leroux L, Lacout JL (2001) Preparation of calcium strontium hydroxyapatites by a new route involving calcium phosphate cements. J Mater Res 16(1):171–178

    Article  CAS  Google Scholar 

  35. Tadier S, Bareille R, Siadous R, Marsan O, Charvillat C, Cazalbou S, Combes C (2012) Strontium-loaded mineral bone cements as sustained release systems: compositions, release properties, and effects on human osteoprogenitor cells. J Biomed Mater Res B Appl Biomater 100(2):378–390

    Article  PubMed  Google Scholar 

  36. Wu T, Yang S, Lu T, He F, Zhang J, Shi H, Ye J (2019) Strontium ranelate simultaneously improves the radiopacity and osteogenesis of calcium phosphate cement. Biomed Mater 14(3):035005

    Article  CAS  PubMed  Google Scholar 

  37. No YJ, Xin X, Ramaswamy Y, Li Y, Roohaniesfahani S, Mustaffa S, Zreiqat H (2019) Novel injectable strontium-hardystonite phosphate cement for cancellous bone filling applications. Mater Sci Eng C 97:103–115

    Article  CAS  Google Scholar 

  38. Lode A, Heiss C, Knapp G, Thomas J, Nies B, Gelinsky M, Schumacher M (2018) Strontium-modified premixed calcium phosphate cements for the therapy of osteoporotic bone defects. Acta Biomater 65:475–485

    Article  CAS  PubMed  Google Scholar 

  39. Kaygili O, Keser S, Kom M, Eroksuz Y, Dorozhkin SV, Ates T, Yakuphanoglu F (2015) Strontium substituted hydroxyapatites: synthesis and determination of their structural properties, in vitro and in vivo performance. Mater Sci Eng C 55:538–546

    Article  CAS  Google Scholar 

  40. Sun L, Li T, Yu S, Mao M, Guo D (2021) A novel fast-setting strontium-containing hydroxyapatite bone cement with a simple binary powder system. Front Bioeng Biotechnol 9:168

    Article  Google Scholar 

  41. Xue W, Hosick HL, Bandyopadhyay A, Bose S, Ding C, Luk KDK, Lu WW (2007) Preparation and cell–materials interactions of plasma sprayed strontium-containing hydroxyapatite coating. Surf Coat Technol 201(8):4685–4693

    Article  CAS  Google Scholar 

  42. Li ZY, Lam WM, Yang C, Xu B, Ni GX, Abbah SA, Lu WW (2007) Chemical composition, crystal size and lattice structural changes after incorporation of strontium into biomimetic apatite. Biomaterials 28(7):1452–1460

    Article  CAS  PubMed  Google Scholar 

  43. Li Y, Li Q, Zhu S, Luo E, Li J, Feng G, Hu J (2010) The effect of strontium-substituted hydroxyapatite coating on implant fixation in ovariectomized rats. Biomaterials 31(34):9006–9014

    Article  CAS  PubMed  Google Scholar 

  44. Ge M, Ge K, Gao F, Yan W, Liu H, Xue L, Zhang J (2018) Biomimetic mineralized strontium-doped hydroxyapatite on porous poly (l-lactic acid) scaffolds for bone defect repair. Int J Nanomed 13:1707

    Article  CAS  Google Scholar 

  45. Melo P, Naseem R, Corvaglia I, Montalbano G, Pontremoli C, Azevedo A, Fiorilli S (2020) Processing of Sr2+ containing Poly L-lactic acid-based hybrid composites for additive manufacturing of Bone Scaffolds. Front Mater 7:413

    Article  Google Scholar 

  46. Akpan ES, Dauda M, Kuburi LS, Obada DO (2021) Box-Behnken experimental design for the process optimization of catfish bones derived hydroxyapatite: a pedagogical approach. Mater Chem Phys 272:124916

    Article  CAS  Google Scholar 

  47. Osuchukwu OA, Salihi A, Abdullahi I, Obada DO (2022) Synthesis and characterization of sol–gel derived hydroxyapatite from a novel mix of two natural biowastes and their potentials for biomedical applications. Mater Today Proc. https://doi.org/10.1016/j.matpr.2022.04.696

    Article  Google Scholar 

  48. Osuchukwu OA, Salihi A, Abdullahi I, Obada DO (2022) Experimental data on the characterization of hydroxyapatite produced from a novel mixture of biowastes. Data Brief 42:108305

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  49. Akpan ES, Dauda M, Kuburi LS, Obada DO, Dodoo-Arhin D (2020) A comparative study of the mechanical integrity of natural hydroxyapatite scaffolds prepared from two biogenic sources using a low compaction method. Res Phys 17:103051

    Google Scholar 

  50. Akpan ES, Dauda M, Kuburi LS, Obada DO (2020) A facile synthesis method and fracture toughness evaluation of catfish bones-derived hydroxyapatite. MRS Adv 5(26):1357–1366. https://doi.org/10.1557/adv.2020.172

    Article  CAS  Google Scholar 

  51. Akpan ES, Dauda M, Kuburi LS, Obada DO, Bansod ND, Dodoo-Arhin D (2020) Hydroxyapatite ceramics prepared from two natural sources by direct thermal conversion: from material processing to mechanical measurements. Mater Today Proc 38:2291–4

    Article  Google Scholar 

  52. Obada DO, Dauda ET, Abifarin JK, Bansod ND, Dodoo-Arhin D (2020) Mechanical measurements of pure and kaolin reinforced hydroxyapatite-derived scaffolds: a comparative study. Mater Today Proc. 38:2295–300

    Article  Google Scholar 

  53. Obada DO, Osseni SA, Sina H, Salami KA, Oyedeji AN, Dodoo-Arhin D, Bansod ND et al (2021) Fabrication of novel kaolin-reinforced hydroxyapatite scaffolds with robust compressive strengths for bone regeneration. Appl Clay Sci 215:106298

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The authors wish to acknowledge the Tertiary Education Trust Fund (TETFund) in Nigeria for funding this research under grants with reference: NRF_SETI_HSW_00714, 2020, and NRF_SETI_HSW_00379, 2021 (provisional).

Author information

Authors and Affiliations

  1. Department of Mechanical Engineering, Ahmadu Bello University, Zaria, Nigeria

    Ayodeji Nathaniel Oyedeji, David Olubiyi Obada, Muhammad Dauda & Laminu Shettima Kuburi

  2. Multifunctional Materials Laboratory, Shell Office Complex, Department of Mechanical Engineering, Ahmadu Bello University, Zaria, Nigeria

    Ayodeji Nathaniel Oyedeji, David Olubiyi Obada & Laminu Shettima Kuburi

  3. Africa Centre of Excellence on New Pedagogies in Engineering Education, Ahmadu Bello University, Zaria, Nigeria

    David Olubiyi Obada

  4. Air Force Institute of Technology, Nigerian Air Force Base, Kaduna, Nigeria

    Muhammad Dauda

  5. Department of Physics, Constantine the Philosopher University in Nitra, Nitra, Slovakia

    Stefan Csaki

  6. Institute of Plasma Physics, The Czech Academy of Sciences, Prague, Czech Republic

    Jakub Veverka

Authors
  1. Ayodeji Nathaniel Oyedeji
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. David Olubiyi Obada
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Muhammad Dauda
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Laminu Shettima Kuburi
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Stefan Csaki
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Jakub Veverka
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to David Olubiyi Obada.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Oyedeji, A.N., Obada, D.O., Dauda, M. et al. Fabrication and characterization of hydroxyapatite-strontium/polylactic acid composite for potential applications in bone regeneration. Polym. Bull. 80, 10997–11014 (2023). https://doi.org/10.1007/s00289-022-04541-3

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00289-022-04541-3

Keywords

Search

Navigation