Effect of Sterilization on Bone Implants Based on Biodegradable Polylactide and Hydroxyapatite
Abstract
:1. Introduction
2. Materials and Methods
2.1. Research Object
2.1.1. Materials
2.1.2. Preparation Implants for Study
2.2. Organoleptic Evaluation
2.3. Fourier-Transform Infrared Study
2.4. Gel Permeation Chromatography
2.5. Thermal Properties
- Xc—degree of crystallinity;
- ΔHm—enthalpy connected with the melting process of the crystalline phase;
- —enthalpy connected with the melting process of the crystalline phase PLA; completely crystalline ( = 109 J/g) [26].
2.6. Test of Sterility
3. Results and Discussion
3.1. Change in the Shape of the Implants
3.2. The Structural Properties of the Implant Material
3.2.1. Fourier-Transform Infrared Study (FTIR)
- ca. 3550 cm−1 coming from stretching vibrations of –O–H bonds;
- 2996; 2946 cm−1 coming from stretching vibrations of –CH– bonds;
- 1755 cm−1 coming from vibrations stretching the –C=O bonds;
- 1455 cm−1 coming from deformation vibrations of the –CH3 group;
- 1383; 1361 cm−1 originating from symmetric and asymmetric –CH– bond vibrations;
- ca. 1264 cm−1 coming from deformation vibrations of the –C=O bond;
- 1184; 1131; 1087 cm−1 coming from vibrations stretching the –C–O– bonds;
- 1043 cm−1 coming from vibrations stretching the –OH bonds;
- ca. 950 cm−1 derived from –CH in the PLA ring;
- 870 cm−1 coming from deformation vibrations of –C–C– bonds.
3.2.2. Molecular Weight and Polydispersity
3.3. Thermal Analysis
3.4. Sterility Tests
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Implants Group | Characteristics of the Sterile Barrier System | Characteristics of the Sterilization Process | |||
---|---|---|---|---|---|
Packaging | Heat Sealing Parameters | Sterilization Type | Parameters of the Sterilization Process | Sterilization Unit | |
A | flat paper–foil bag, TZMO_OM-191-FPPA-126 | downforce: 700–850 N without the air remove T = 180 °C t = 2 s | steam | T = 121 °C t = 16 min | CitoNet-Łódź Sp. z o. o. Lodz, Poland |
T = 134 °C t = 5.5 min | |||||
B | flat paper–foil bag, TZMO_OM-191-FPPR-033 | downforce: 700–850 N without the air remove T = 180 °C t = 2 s | ethylene oxide | amount of gas used 48.2 kg, including 5.1 kg of ethylene oxide | Yavo Sp. z o.o. Belchatow, Poland |
C | flat foil bag WIPAK_ ESE 1250–ESE 1250 Medi Peel | downforce: 700–850 N tAR = 2 s T = 135 °C t = 0.8 s | electron beam radiation | irradiation dose 25 kGy ± 0.99% transportation speed 0.459 m/min ± 1.12% | Radiation Sterilization Plant of Medical Devices and Allografts Warsaw, Poland |
Sample Characteristics | Molecular Weight (g/mol) | Polydispersity | |
---|---|---|---|
Mw | Mn | Mw/Mn | |
bone implant sample after steam sterilization (T = 121 °C; t = 16 min) | 5.628 × 104 (±16.850%) | 2.198 × 104 (±19.830%) | 2.561 (±26.022%) |
bone implant sample after steam sterilization (T = 134 °C; t = 5.5 min) | 4.146 × 104 (±35.801%) | 3.697 × 104 (±35.110%) | 1.122 (±50.143%) |
bone implant sample after sterilization with ethylene oxide | 10.35 × 104 (±18.882%) | 5.896 × 104 (±22.611%) | 1.756 (±29.458%) |
bone implant sample after radiation sterilization with electrons | 7.789 × 104 (±19.554%) | 3.922 × 104 (±22.033%) | 1.986 (±29.459%) |
bone implant sample before sterilization process | 10.57 × 104 (±16.227%) | 4.014 × 104 (±20.597%) | 2.633 (±26.221%) |
Sample Characteristics | I SEGMENT Heating | II SEGMENT Cooling | III SEGMENT Reheating | |||||
---|---|---|---|---|---|---|---|---|
Tg [°C] | Tm [°C] | ΔHm [J/g] | Tg [°C] | Tc [°C] | Tg [°C] | Tm [°C] | ΔHm [J/g] | |
bone implant sample before sterilization process | 60.0 ± 2.7 | 137.0 ± 1.8 | −8.5 ± 0.7 | 55.0 ± 2.6 | - | 56.0 ± 2.7 | 139.5 ± 2.7 | −2.2 ± 0.2 |
bone implant sample after steam sterilization (T = 121 °C; t = 16 min) | 61.0 ± 2.8 | 138.0 ± 1.7 | −14.0 ± 0.9 | 54.0 ± 1.9 | - | 57.0 ± 2.1 | 142.0 ± 2.8 | −0.5 ± 0.2 |
bone implant sample after steam sterilization (T = 134 °C; t = 5.5 min) | 56.0 ± 2.7 | 139.0 ± 2.3 | −17.5 ± 0.7 | - | - | 56.0 ± 1.9 | 140.0 ± 2.1 | −6.6 ± 0.4 |
bone implant sample after sterilization with ethylene oxide | 56.0 ± 2.4 | 138.0 ± 2.1 | −6.3 ± 0.8 | 59.0 ± 1.8 | - | 55.0 ± 2.4 | 139.0 ± 2.3 | −1.3 ± 0.7 |
bone implant sample after radiation sterilization with electrons | 63.0 ± 2.7 | 138.0 ± 1.7 | −7.4 ± 1.1 | 59.0 ± 1.6 | - | 57.0 ± 2.2 | - | - |
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Kucharska-Jastrząbek, A.; Chmal-Fudali, E.; Rudnicka, D.; Kosińska, B. Effect of Sterilization on Bone Implants Based on Biodegradable Polylactide and Hydroxyapatite. Materials 2023, 16, 5389. https://doi.org/10.3390/ma16155389
Kucharska-Jastrząbek A, Chmal-Fudali E, Rudnicka D, Kosińska B. Effect of Sterilization on Bone Implants Based on Biodegradable Polylactide and Hydroxyapatite. Materials. 2023; 16(15):5389. https://doi.org/10.3390/ma16155389
Chicago/Turabian StyleKucharska-Jastrząbek, Agnieszka, Edyta Chmal-Fudali, Daria Rudnicka, and Barbara Kosińska. 2023. "Effect of Sterilization on Bone Implants Based on Biodegradable Polylactide and Hydroxyapatite" Materials 16, no. 15: 5389. https://doi.org/10.3390/ma16155389