Diametral Tensile Strength Evaluation of Carbonate Apatite Cement Reinforced by Genipin Cross-Linked Gelatin

2019 ◽  
Vol 829 ◽  
pp. 28-33
Author(s):  
Zatira Avriyanti ◽  
Zulia Hasratiningsih ◽  
Arief Cahyanto

Carbonate apatite is one of the most widely studied bioceramic material for its use as bone cement. On the previous study, it has already stated that CO3Ap cement has good osteoconductivity which makes this cement could be replaced by bone. However, the mechanical strength of CO3Ap cement is still low. This low mechanical strength is estimated due to the high porosity and absence of organic components. The aim of this study is to improve the mechanical strength of the CO3Ap cement reinforced by gelatin as an organic component with genipin as a cross-linking agent (Gelapin). The powder phase of vaterite and DCPA at weight ratio 40:60 were mixed with 0.2 mol/L Na2HPO4, 5% (w/v) gelatin, and 20% (v/v) genipin using 0.5 liquid to powder (L/P) ratio. The liquid phase ratios of Na2HPO4 and Gelapin were 50:50, 70:30, and 90:10. For control group, Gelapin were didn’t mixed in the liquid. Diametral tensile strength was improving and statistically significant (p<0.05) on set cement with 50:50 liquid ratio, the average value was 6.02 ± 0.14 MPa whereas the average value of the control group was only 3.10 ± 0.15 MPa. For this instance, gelatin serves a polymer matrix so the carbonate apatite crystallites could be well distributed within it which then gives more flexibility and resistance for the cement. On the other hand, genipin was also successfully cross-linked the gelatin. This study showed that by reinforcing CO3Ap cement using genipin cross-linked gelatin might be a good candidate for a bone substitute material.

2017 ◽  
Vol 758 ◽  
pp. 56-60 ◽  
Author(s):  
Arief Cahyanto ◽  
Atina Ghina Imaniyyah ◽  
Myrna Nurlatifah Zakaria ◽  
Zulia Hasratiningsih

Mechanical strength is one of the key factors for clinical application of injectable carbonate apatite (CO3Ap) cement. Incorporation of polymeric additives into the mixing liquid of injectable bone cement has been known to improve cement injectability. The aim of this study is to determine whether incorporation of sodium carboxymethyl cellulose (Na CMC) into the mixing liquid would affect the diametral tensile strength (DTS) of injectable CO3Ap cement. In the present study, Na CMC, a polymeric additive and a cellulose derivative, was used to promote the injectability of CO3Ap cement. Three groups of CO3Ap cement samples consist of CaCO3 and CaHPO4 powder in each group were mixed with 0.5 %, 1%, and 2% Na CMC solution incorporated to 0.2 mol/L Na2HPO4 solution. As a control, powder mixed with 0.2 mol/L Na2HPO4 solution was used. Samples were kept in an incubator (37°C, 100% relative humidity, 24 hours). The mechanical strength properties were evaluated by diametral tensile strength (DTS). The average DTS of samples containing 0.5%, 1%, and 2% Na CMC were 3.19 MPa, 3.57 MPa, and 3.06 MPa, respectively. While the average DTS of the control group was 3.29 MPa. The groups containing Na CMC in all concentrations showed no statistical difference (p>0.05) on DTS compared to the control group. The injectability improved as the concentration of Na CMC increased. In conclusion, revealed that Na CMC does not affect the mechanical strength of CO3Ap cement. Therefore, it may be considered as an effective material to promote cement injectability. Further study of additives that can be used to promote the injectability of CO3Ap cement and enhance the mechanical strength awaits based on this initial finding.


2012 ◽  
Vol 529-530 ◽  
pp. 192-196 ◽  
Author(s):  
Arief Cahyanto ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Shigeki Matsuya ◽  
Ishikawa Kunio

The aim of the present study is to fabricate bone cement that could transform to carbonate apatite (CO3Ap) completely at body temperature. The powder phase of vaterite and dicalcium phosphate anhydrous (DCPA) was mixed with 0.8 mol/L of NaH2PO4, Na2HPO4, and Na3PO4 aqueous solution, respectively, with liquid to powder ratio (L/P ratio) of 0.45, 0.55, and 0.65. The paste was packed into split stainless steel mold, covered with the glass slide and kept at 37°C and 100% relative humidity for up to 96 hours (h). XRD analysis revealed that the cement became pure CO3Ap within 24 h for Na3PO4, 72 h for Na2HPO4, and 96 h for NaH2PO4, respectively. FT-IR results showed that all of the obtained specimens could be assigned to B-type CO3Ap. CHN analysis showed the carbonate content of the specimen were 10.4 ± 0.3% for NaH2PO4, 11.3 ± 0.7% for Na2HPO4, and 11.8 ± 0.4% for Na3PO4, respectively. Diametral tensile strength of the set CO3Ap cement was 1.95 ± 0.42 MPa for NaH2PO4, 2.53 ± 0.53 MPa for Na2HPO4, and 3.45 ± 1.53 MPa for Na3PO4, respectively. The set CO3Ap cement had low crystallinity similar to bone apatite since it was synthesized at body temperature. We concluded, therefore, that CO3Ap cement prepared from the present method has higher possibility to be used as an ideal bone replacement.


2016 ◽  
Vol 696 ◽  
pp. 23-26
Author(s):  
Nguyen Xuan Thanh Tram ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Shigeki Matsuya ◽  
Kunio Ishikawa

We have established a processing method to fabricate three - dimensional porous carbonate apatite (CO3Ap) with interconnected porous structure and improved mechanical strength. Briefly, porous CO3Ap materials were produced via phosphorization of porous calcite precursor in hydrothermal condition. In order to make porous calcite precursor, negative replication of modified polyurethane foam template was conducted. In this study, an in vivo behavior of that porous CO3Ap was evaluated. The interconnected porous CO3Ap material was implanted in the tibia of Japanese male rabbits and removed after a period of 6 months. Micro-computed tomography (μ-CT) scanner and histological analysis were used to characterize the bone formation response of the porous CO3Ap. The results suggest that porous CO3Ap with enhanced mechanical strength was not only osteoconductive but also bioresorbable therefore it could be used as bone substitute material.


2012 ◽  
Vol 529-530 ◽  
pp. 153-156 ◽  
Author(s):  
Tram Nguyen Xuan Thanh ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Alireza Valanezhad ◽  
Shigeki Matsuya ◽  
...  

We have previously reported that calcite foam that had interconnected porous structure could be prepared by ceramic foam method and it transformed to carbonate apatite (CO3Ap). In the ceramic foam method, polyurethane sponge was used as a template. The polyurethane sponge was immersed in the ceramics slurry, and the strut of the polyurethane foam was covered by ceramic powder. After that it was dried and sintered at high temperature. Calcite foams produced by this approach were comprised of a three-dimensional (3D) interconnected porous structure that facilitated cell penetration. However, all foams have a common limitation: the inherent lack of mechanical strength associated with high porosity. Therefore, in this study, an inverse ceramic foam method was studied; multi polyurethane coating method using polyurethane foam as a template. In this study, the compressive strength was improved by an inverse replication allowed for decreasing porosity while at the same time maintaining the interconnectivity. The burnable synthetic resin coating layer was introduced onto struts of polyurethane foam to make the triangular struts become more round and thick, consequently producing large round capillary within the foam structure fulfilling the requirement for osteoblast colonization. In particular, polyurethane foam was dipped orderly into two monomers, followed by centrifugation to remove excess liquids inside foam. After resin curing, a layer of synthetic resin was coated strut of foam. Calcium hydroxide Ca (OH)2 slurry was then infiltrated into resin coated-polyurethane foam. By firing at 600°C in O2-CO2 stream, polyurethane template was burnt off and Ca (OH)2 was converted into calcite. Negative replicated calcite foam was fabricated and characterized micro-structurally with interconnectivity and improved mechanical strength. The results obtained in this study suggested that this method dramatically improved the mechanical strength of the calcite foam without sacrificing the interconnected structure, and this means that the calcite foam obtained in this method could be precursors for the 3D interconnected porous CO3Ap foam.


2016 ◽  
Vol 720 ◽  
pp. 167-172 ◽  
Author(s):  
Arief Cahyanto ◽  
Kanji Tsuru ◽  
Kunio Ishikawa ◽  
Masanori Kikuchi

The combination of tetracalcium phosphate (TTCP; Ca4(PO4)2O) and dicalcium phosphate anhydrous (DCPA; CaHPO4) which are known as one system of apatite cements already used in the medical and dental application. In spite of several advantages of apatite cements, such as self-setting ability and biocompatibility, their mechanical strengths are still low. The aim of this study is to improve the mechanical strength of the TTCP-DCPA apatite cement using the hydroxyapatite/collagen nanocomposite (HAp/Col). The apatite cement powder was prepared using an equimolar TTCP and DCPA with addition of 10% and 20% of the HAp/Col. That without the HAp/Col was used as a control group. Each group was mixed with 1 mol/L Na1.8H1.2PO4 aqueous solution at powder/liquid ratio of 0.5 and hardened at 37°C and 100 % of relative humidity for 24 hours. A setting time of the cement was evaluated using Vicat needle according to ISO 1566 for dental zinc phosphate cements. Morphology of the cements set were observed by the scanning electron microscopy (SEM), and crystalline phases were identified by the powder X-Ray diffractometry (XRD). The mechanical strength of the cement set was evaluated by the diametral tensile strength (DTS). The setting times of cements were the shortest for the cement with HAp/Col and the longest for the control. XRD patterns of the cement at 24 hours after mixing revealed that all cements changed into apatite from the mixture of TTCP and DCPA. The DTSs of cements were the highest for the cement with 20% HAp/Col and the lowest for the control with significant differences between the cement with 20 % HAp/Col and respective other two cements. The scanning electron micrographs of the surface and fracture surface of the cements suggested that the cement with HAp/Col showed denser structure in comparison to the control and the HAp/Col fibers and/or sheets covered the fracture surface. The HAp/Col would act as reinforcement fibers as well as an adhesive of apatite granules formed by the reaction between TTCP and DCPA. The setting time and mechanical strength of apatite cement was statistically significant improved by adding 20% HAp/Col.


2017 ◽  
Vol 758 ◽  
pp. 52-55 ◽  
Author(s):  
Nina Djustiana ◽  
Mitha Amaranila ◽  
Nadia Greviana ◽  
Myrna Nurlatifah Zakaria ◽  
Sunarso ◽  
...  

Carbonate Apatite (CO3Ap) cement is considered as an ideal bone substitute due to its biocompatibility and osteoconductivity. Also, CO3Ap cement has the chemical composition that closes to natural bone. During cement preparation, precursors play an important role that affects the properties of CO3Ap cement. Cement hardness is one of the important properties that need to be evaluated before the obtained cement can be applied as a bone substitute. Therefore, the purpose of this study is to determine the effect of precursor ratio of CaCO3 and CaHPO4 on the hardness level of CO3Ap cement. In the present study, the CO3Ap cement was prepared from CaCO3 and CaHPO4. Both Commercial and synthesized CaCO3 were used. The CO3Ap cement obtained from commercial CaCO3 was used as a control group. Synthesized CaCO3 was obtained from Indonesian natural limestone. Three different CaCO3:CaHPO4 ratios, 40:60, 30:70 and 20:80 were mixed with 1 mol/L Na2HPO4. Samples were kept at 37°C with 100% relative humidity for 24 hours then tested using micro Vickers hardness testing machine. The micro Vickers hardness of the control group with CaCO3:CaHPO4 ratio of 40:60, 30:70 and 20:80 were 5.09 VHN, 6.34 VHN, and 6.73 VHN, respectively. Meanwhile, the micro Vickers hardness of the CO3Ap cement obtained from synthesized CaCO3 were 6.22 VHN, 7.50 VHN, and 10.37 VHN for the CaCO3:CaHPO4 ratio of 40:60, 30:70 and 20:80, respectively. The micro Vickers hardness level of CO3Ap cement precursor ratio from the lowest to the highest was 40:60 < 30:70 < 20:80. In conclusion, the precursor ratio significantly affects the hardness level of the CO3Ap cement. The hardness level of CO3Ap cement obtained from synthesized CaCO3 was higher compared with that obtained from commercial CaCO3.


2016 ◽  
Vol 720 ◽  
pp. 147-152 ◽  
Author(s):  
Myrna Nurlatifah Zakaria ◽  
Arief Cahyanto ◽  
Ahmed El-Ghannam

Silica-calcium phosphate composite (SCPC) and carbonate apatite (CO3Ap) are resorbable bioactive materials with the ability to adapt to bone structure and to induce bone regeneration. Considering the similarity between bone and dental structure, where both are mainly composed of calcium deficient carbonate containing hydroxyapatite, we hypothesize that a SCPC-CO3Ap bone cement might also be favorable for the regeneration of dentin and pulp tissue. Therefore, in the present study we report on the effect of composition and structure of SCPC-CO3Ap cement on the morphology, setting and mechanical properties of the material. The novel bioceramics cement composed of vaterite, dicalcium phosphate anhydrous (DCPA) and SCPC. The powder cement ratio divided into 5 groups: group 1 (60% DCPA : 40% vaterite : 0% SCPC) as a control, group 2 (60% DCPA : 10% vaterite : 30% SCPC), group 3 (60% DCPA : 20% vaterite : 20% SCPC), group 4 (60% DCPA : 30% vaterite : 10% SCPC), and group 5 (60% DCPA : 0% vaterite : 40% SCPC). Each group was mixed by 1M Na2HPO4 aqueous solution at liquid to powder ratio of 0.5 and hardened at 37°C and 100 % of relative humidity for 72 hours. Set cement was examined by X-Ray diffraction (XRD), scanning electron microscopy (SEM) and the mechanical strength was evaluated by diametral tensile strength. XRD patterns revealed that the apatite formation was formed after 72 hours, however the intensity of apatite varied based on the SCPC content. The DTS evaluation indicated that group 3 has the highest mechanical strength compared to others. This was supported by SEM analysis of set cement showing more compact surface microstructure of group 2 and 3 compared to other different ratio and control group. The novel bioceramics cement was successfully made using vaterite, DCPA and SCPC. This new cement is currently being investigated for dental application to induce dentinogenesis.


2017 ◽  
Vol 758 ◽  
pp. 61-65 ◽  
Author(s):  
Arief Cahyanto ◽  
Elfira Megasari ◽  
Myrna Nurlatifah Zakaria ◽  
Nina Djustiana ◽  
Sunarso ◽  
...  

Carbonate Apatite (CO3Ap) cement has been widely used for bone substitute. It is known that CO3Ap crystals have the close composition to natural bone. It is expected that CO3Ap cement may play an essential role in endodontics treatment, particularly as an endodontic sealer due to its potential to obturate root canal system to a more hermetic and stable environment. Therefore, the aim of this study is to fabricate CO3Ap cement as a new material for endodontic sealer. The CO3Ap cement sealer was prepared by mixing dicalcium phosphate anhydrous (DCPA), vaterite and calcium hydroxide [Ca(OH)2] with 0.2 mol/L Na2HPO4 containing 1% sodium carboxymethyl cellulose (NaCMC) and 32 µg thymoquinone, with liquid to powder ratio of 0.6. The set cement was incubated at 37°C under 100% relative humidity for 72 h. In this study, five compositions of powder ratio were prepared. The diametral tensile strength (DTS) evaluation indicated that CO3Ap cement made of 60% DCPA, 30% Vaterite and 10% Ca(OH)2 has the highest mechanical strength compared with the other compositions. X-ray diffraction (XRD) analysis of the set cement with the highest DTS value indicated that CO3Ap crystals were successfully formed. The set cement with the highest DTS value showed the highest density compared with the other compositions evidenced from scanning electron microscope (SEM) images. In conclusion, the CO3Ap cement was successfully fabricated by mixing DCPA, vaterite and Ca(OH)2. The CO3Ap cement prepared from 60% DCPA, 30% Vaterite and 10% Ca(OH)2 demonstrated the highest DTS value compared with the other compositions.


2019 ◽  
Vol 829 ◽  
pp. 40-45
Author(s):  
Ira Artilia ◽  
Myrna Nurlatifah Zakaria ◽  
Arief Cahyanto

Apatite cement is ideal self-setting cement for bone substitute material, however its use is limited only to areas that receive minimum load bearing because mechanical strength of apatite cement is low. Silica-calcium phosphate nanocomposite (SCPC50) is material having good mechanical strength and has an important role in bone remodeling (bone metabolism), mineralization, synthesis of cartilage, collagen production, proliferation and differentiation of bone cells. However, the unsetting and granule’s physical shape of SCPC50 limits the application. The purpose of this study is to determine the effect of various mixtures of SCPC50 and apatite cement to manipulative index (setting time and handling property), and mechanical properties. The experimental results show that the setting time of apatite cement mixture with 5% and 10% SCPC50 was 40% higher (p<0.05). The mechanical strength evaluated by Diametral Tensile Strength showed that the addition of both 5% silica and 10% SCPC50 composition to apatite cement mixture increased the mechanical strength of apatite cement mixture (p<0.1). The handling property of cement paste was significantly increased between the apatite cement without SCPC50 and apatite cement with both 5% SCPC50 and 10% SCPC50 (p<0.05). It is concluded that the addition of SCPC50 to apatite cement mixture could improve the mechanical properties and it is expected to improve its bioactivity.


2012 ◽  
Vol 583 ◽  
pp. 32-35 ◽  
Author(s):  
Wen Yong Liu ◽  
Kai Tan ◽  
Yu Gang Huang ◽  
Yi Chen ◽  
Xiang Gang Li ◽  
...  

The thermoplastic processing and mechanical properties of starch and polyvinyl alcohol (PVA) composites reinforced with microcrystal cellulose (MCC) were investigated. Glycerol with 30 wt% was chosen as the plasticizer for starch and PVA, respectively. MCC with 2 wt% was used to reinforce the starch/PVA composite. The results showed that the mechanical properties of the obtained starch/PVA blend were best when the glycerol content was 30% of starch and 20% of PVA, and the weight ratio of PVA and starch was 4/6 (wPVA/wstarch). After the addition of MCC, the mechanical properties of the starch/PVA blends were improved, and the tensile strength was increased by 52%. Moreover, it was confirmed by rheological measurements that MCC could interact with the composite materials, which results in the improvement of the mechanical strength of the starch/PVA composites.


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