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Organic/inorganic bioactive materials part IV: In vitro assessment of bioactivity of gelatin-calcium phosphate silicate/wollastonite hybrids

100%
Radev L., Hristov V., Fernandes M., Salvado I.
Open Chemistry
|
2010
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vol. 8
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issue 2
278-284
EN
Biohybrids consisting of gelatin (G) and calcium phosphate silicate/wollastonite (CPS/W) have not been prepared so far. In this work our results are focused on the possibility of obtaining G-CPS/W bioactive hybrids in vitro. XRD, FTIR, SEM/EDS techniques were employed to characterize the synthesized hybrid materials. FTIR shows that before immersion in 1.5 SBF the “red shift” of COO- band for pure G is observed. The presence of this bond could be attributed to the formation of COO-Ca2+ via non-biomimetic route. After immersion in 1.5 SBF, FTIR shows the presence of A- and B-type carbonate containing hydroxyapatite (A/B-CO3HA). ESD and FTIR show that small amount of calcite (CaCO3) are present after in vitro test in 1.5 SBF for 3 days. XRD reveals that CO3HA and small amounts of CaCO3 can be detected after in vitro test. SEM results obtained for immersed samples show that hydroxyapatite (HA) particles fully covered the surface of the hybrids by a layer composed of spherulites. At higher magnification, very small elongated crystallites could be observed. [...]
2
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Organic/Inorganic bioactive materials Part III: in vitro bioactivity of gelatin/silicocarnotite hybrids

100%
Radev L., Fernandes M., Salvado I., Kovacheva D.
Open Chemistry
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2009
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vol. 7
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issue 4
721-730
EN
In this work we present our experimental results on synthesis, structure evolution and in vitro bioactivity assessment of new gelatin/silicocarnotite hybrid materials. The hybrids were obtained by diluting gelatin (G) and silicocarnotite (S) ceramic powder with G:S ratios of 75:25 and 25:75 wt.% in hot (40°C) water. The hybrids were characterized using XRD, FTIR, SEM/EDS and XPS. FTIR depicts that the “red shift” of amide I and COO− could be attributed to the fact that the gelatin prefers to chelate Ca2+ from S. The growth of calcium phosphates on the surface of the hybrids synthesized and then immersed in 1.5 SBF for 3 days was studied by using of FTIR, XRD and SEM/EDS. According to FTIR results, after an immersion of 3 days, A and B-type CO3HA can be observed on the surface. XRD results indicate the presence of hydroxyapatite with well defined crystallinity. SEM/EDS of the precipitated layers show the presence of CO3HA and amorphous calcium phosphate on the surface of samples with different G/S content when immersed in 1.5 SBF. XPS of the G/S hybrid with 25:75 wt.% proved the presence of Ca-deficient hydroxyapatite after an in vitro test for 3 days.
3
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Silica-carrageenan hybrids used for cell immobilization realizing high-temperature degradation of nitrile substrates

100%
Kabaivanova L., Chernev G., Miranda Salvado I., Fernandes M.
Open Chemistry
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2011
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vol. 9
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issue 2
232-239
EN
In this work the application of hybrid materials, containing TEOS as source of SiO2 and k-carrageenan in different percentage, synthesized by the sol-gel method at room temperature was studied. They were used as matrices for entrapment of whole Bacillus sp. UG-5B cells, producers of thermostable nitrilase. The effect of the surface area and size and quantity of pores in the synthesized materials on the enzyme activity was evaluated. The process of biodegradation of different concentrations of toxic, potentially carcinogenic and mutagenic substrates by the obtained biocatalysts was investigated. The enzyme reaction takes place by the nitrilase pathway, catalysing nitrile hydrolysis directly to the corresponding carboxylic acid, forming ammonia. At batch experiments the influence of the substrate concentration of different nitriles was tested and 20 mM concentration was found most suitable. A two-step biodegradation process in a laboratory-scale column bioreactor of o-, m- and p-tolunitrile as a mixture was followed. After operation of the system for nine hours for the mixture of substrates at a flow rate of 45 mL h−1 and at 60°C, the overall conversion realized was above 90%, showing a good efficiency of the investigated process.
4
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In vitro bioactivity of 70 wt.% SiO2 - 30 wt.% CaO sol-gel glass, doped with 1, 3 and 5 wt.% NbF5

88%
Radev L., Hristova K., Jordanov V., Fernandes M., Salvado I.
Open Chemistry
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2012
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vol. 10
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issue 1
137-145
EN
The 70SiO2-30CaO (wt.%) sol-gel glasses doped with 1, 3 and 5 NbF5 (wt.%) were prepared via polystep sol-gel route. The synthesized glasses were characterized by XRD, FTIR and SEM. Changes in 1.5 SBF solutions were measured by ICP-AES. XRD of the glasses stabilized at 700°C for 6 hours proved the presence of niocalite. FTIR was consistent with XRD data. The in vitro bioactivity study of all glasses prepared were carried out by soaking in 1.5 simulated body fluid (1.5 SBF) at 37°C for 6 and 12 days in static conditions. The FTIR reveals the formation of A-type and B-type carbonate containing hydroxyapatite (CO3HA) layer. Changes in 1.5 SBF solutions, after 6 days of soaking, show that the Ca concentration increased significantly, compared to the initial Ca content in the 1.5 SBF solution before in vitro test. After 12 days of immersion, the Ca concentration decreased, i.e., the formation of HA phase consumed Ca from 1.5 SBF solution. For all soaking times, the concentration of P is much lower than that the used 1.5 SBF. Based on these results we suggest that Ca and P play an active role in the future of the glasses. SEM depicts that the different morphology of hydroxyapatite can be formed as a function of soaking time.
5
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Organic-inorganic hybrid materials based on N=C=O functionalised silan modified with titanium and zirconium

76%
Ivanova Y., Dimitriev Y., Gerganova T., Bryaskova R., Fernandes M., Miranda Salvado I.
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EN
This work investigates the influence of the precursor trimethylsilil isocyanate on the sol-gel synthesis of hybrid materials. The obtained Si−O−C−N network is additionally modified by titanium and zirconium alcoxypropoxides in the range of 10 to 30 wt. %. The structure of the obtained hybrid materials before and after pyrolysis up to 1100°C was investigated by methods of XRD, FTIR and 29Si MAS NMR. We established that the hybrid structure was stable up to 600°C based on IR study. The structural transformation of the hybrid materials into oxycarbonitrogen system started at 800°C. The network of the hybrids modified by titanium remained stable and amorphous up to the final temperature of the pyrolysis (1100°C) compared to the gels modified by more than 10 wt.% Zr. It was confirmed by XRD analysis that the last mentioned are nanocomposite materials, built from carbooxynitrogen vitreous matrix and ZrO2-nanocrystals (tetragonal). The NMR method verified the presence of heterometallic bonds (Si−O−Ti and Si−O−Zr) and Q4, ZrQ3 or TiQ3, NSiO3 and D structural units in the gels.
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