Investigation of Antibacterial Properties of Ion-Doped β-Tri-calcium Phosphate Powders Produced via Microwave-Assisted Synthesis Technique

Year 2023, Volume: 23 Issue: 6, 1488 - 1496, 28.12.2023

Azade Yelten Coşkun , Yağmur Göçtü , Batur Ercan

https://doi.org/10.35414/akufemubid.1250275

Abstract

CaP-based bioceramic materials are widely used in orthopedic applications. β-tri-calcium phosphate (β-TCP) is a bioresorbable member of the CaP-based compounds and can be implemented as putty, coating, powders, granules, etc. depending on the implantation area. β-TCP is usually produced with wet chemical synthesis systems. However, long synthesis durations, processes with multiple steps, and difficulties in controlling the process parameters yield the researches to develop novel production methods. Recently, the microwave-assisted synthesis technique has drawn attention due to its advantages such as being a shorter and more practical experimental procedure. In this study, β-TCP powders were fabricated via the microwave-assisted synthesis method. Ca and P source solutions were prepared, and following their reaction microwave radiation was applied. The obtained product was centrifuged to separate the precipitate, and then this wet part was dried, and finally calcined at 900°C. In this way, Ce3+ and SeO3-2 doped β-TCP powders, which may show antibacterial properties and induce bone regeneration were achieved. Chemical phase analysis with X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Energy Dispersive Spectroscopy (EDS) observations to investigate the microstructure and elemental mapping, immersion in the Simulated Body Fluid (SBF) for 14 days at 37°C to determine the bioactivity behavior, and bacteria interaction studies by using Staphylococcus aureus (S. aureus, ATCC 25923) to evaluate the antibacterial activity of the synthesized powders were done within characterization. Formation of the CaP-based precipitates on the surfaces of the powders depending on immersion in 1X SBF solution showed the bioactive character of the products. Moreover, a reduction in the number of bacterial colonies proved that the ion-doped powders exhibited antibacterial properties.

Keywords

β-Tri-calcium phosphate powders, Microwave-assisted synthesis, Ion-doping, Bioactivity behavior, Antibacterial properties

Project Number

FBA-2021-34751

İyon Katkılı β-Trikalsiyum Fosfat Tozlarının Mikrodalga Destekli Sentez Tekniği ile Üretimi ve Antibakteriyellik Özelliklerinin İncelenmesi

Abstract

β-trikalsiyum fosfat (β-TCP), ortopedi uygulamalarında sıklıkla kullanılmakta olan kalsiyum fosfat (CaP) esaslı biyoseramik malzemelerden biri olup biyoemilebilir karakterdedir ve implantasyon alanına bağlı olarak macun, kaplama, toz, granül vb. formlarda uygulanabilmektedir. β-TCP üretimi için genellikle tercih edilen yaş kimyasal yöntemlerde, üretim sürelerinin uzun ve çok adımlı olması ve proses parametrelerinin kontrol edilmesinde güçlükler yaşanması nedeniyle farklı sentez yollarının geliştirilmesi yönünde araştırmalar ağırlık kazanmıştır. Bu çalışmada, β-TCP tozları deneysel sürecin çok daha kısa ve pratik olması yönleriyle ön plana çıkan mikrodalga destekli sentez tekniği ile elde edilmiştir. Hazırlanan Ca ve P kaynak çözeltileri reaksiyona sokulduktan sonra mikrodalga ışımasına tabi tutulmuş, ışıma sonrası ürünün santrifüj edilmesiyle açığa çıkan yaş çökelti kurutulmuş ve nihai olarak 900°C’de ısıl işlem görmesi sağlanmıştır. Böylelikle antibakteriyellik ve kemik gelişimini destekleme özellikleri sergilemesi beklenen Ce+3 ve SeO3-2 katkılı β-TCP tozları üretilmiştir. Tozların karakterizasyonu kapsamında; X-Işını Difraksiyonu (XRD) ile kimyasal faz analizi, Taramalı Elektron Mikroskobu (SEM) ve Enerji Dağılım Spektrometresi (EDS) ile mikroyapı ve elementel haritalama incelemeleri, vücut benzeri sıvı (Simulated Body Fluid, SBF) içerisinde 37°C’de 14 gün tutma suretiyle biyoaktivite davranışının belirlenmesi ve Staphylococcus aureus (S. aureus, ATCC 25923) kullanılarak yapılan bakteri etkileşim testleri doğrultusunda antibakteriyellik özelliklerinin tayin edilmesi gerçekleştirilmiştir. Sentezlenen tozlar, yüzeylerinde 1X SBF çözeltisinde 14 gün bekletilme sonucunda CaP esaslı birikintiler oluşturmuştur ve bu durum örneklerin biyoaktif karakterde olduğunu göstermektedir. Ayrıca, iyon katkısına bağlı olarak bakteri koloni sayısında azalma tespit edilmesi de tozların antibakteriyellik özelliğine işaret etmektedir.

Keywords

β-Trikalsiyum fosfat tozu, Mikrodalga destekli sentez, İyon katkılama, Biyoaktivite davranışı, Antibakteriyel özellikler

Supporting Institution

İstanbul Üniversitesi-Cerrahpaşa Bilimsel Araştırma Projeleri Koordinasyon Birimi

Project Number

FBA-2021-34751

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