scholarly journals Synthesis, Structural, Morphological and Thermal Characterization of Five Different Silica-Polyethylene Glycol-Chlorogenic Acid Hybrid Materials

Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1586
Author(s):  
Michelina Catauro ◽  
Pavel Šiler ◽  
Jiří Másilko ◽  
Roberta Risoluti ◽  
Stefano Vecchio Ciprioti

The present study investigated the structure, morphology, thermal behavior, and bacterial growth analysis of novel three-component hybrid materials synthesized by the sol-gel method. The inorganic silica matrix was weakly bonded to the network of two organic components: a well-known polymer such as polyethylene glycol (PEG, average molar mass of about 4000 g/mol), and an antioxidant constituted by chlorogenic acid (CGA). In particular, a first series was made by a 50 wt% PEG-based (CGA-free) silica hybrid along with two 50 wt% PEG-based hybrids containing 10 and 20 wt% of CGA (denoted as SP50, SP50C10 and SP50C20, respectively). A second series contained a fixed amount of CGA (20 wt%) in silica-based hybrids: one was the PEG-free material (SC20) and the other two contained 12 and 50 wt% of PEG, respectively (SP12C20 and SP50C20, respectively), being the latter already included in the first series. The X-ray diffraction (XRD) patterns and scanning electron microscope (SEM) images of freshly prepared materials confirmed that all the materials were amorphous and homogeneous regardless of the content of PEG or CGA. The thermogravimetric (TG) analysis revealed a higher water content was adsorbed into the two component hybrids (SP50 and SC20) because of the availability of a larger number of H-bonds to be formed with water with respect to those of silica/PEG/CGA (SPC), where silica matrix was involved in these bonds with both organic components. Conversely, the PEG-rich materials (SP50C10 and SP50C20, both with 50 wt% of the polymer) retained a lower content of water. Decomposition of PEG and CGA occurred in almost the same temperature interval regardless of the content of each organic component. The antibacterial properties of the SiO2/PEG/CGA hybrid materials were studied in pellets using either Escherichia coli and Enterococcus faecalis, respectively. Excellent antibacterial activity was found against both bacteria regardless of the amount of polymer in the hybrids.

Materials ◽  
2019 ◽  
Vol 12 (1) ◽  
pp. 155 ◽  
Author(s):  
Elisabetta Tranquillo ◽  
Federico Barrino ◽  
Giovanni Dal Poggetto ◽  
Ignazio Blanco

Implanted biomedical devices can induce adverse responses in the human body, which can cause failure of the implant—referred to as implant failure. Early implant failure is induced numerous factors, most importantly, infection and inflammation. Natural products are, today, one of the main sources of new drug molecules due to the development of pathogenic bacterial strains that possess resistance to more antibiotics used currently in various diseases. The aim of this work is the sol–gel synthesis of antibacterial biomedical implants. In the silica matrix, different percentages (6, 12, 24, 50 wt %) of polyethylene glycol (PEG) or poly(ε-caprolactone) (PCL) were embedded. Subsequently, the ethanol solutions with high amounts of chlorogenic acid (CGA 20 wt %) were slowly added to SiO2/PEG and SiO2/PCL sol. The interactions among different organic and inorganic phases in the hybrid materials was studied by Fourier transform infrared (FTIR) spectroscopy. Furthermore, the materials were soaked in simulated body fluid (SBF) for 21 days and the formation of a hydroxyapatite layer on their surface was evaluated by FTIR and XRD analysis. Finally, Escherichia coli and Pseudomonas aeruginosa were incubated with several hybrids, and the diameter of zone of inhibition was observed to assessment the potential antibacterial properties of the hybrids.


Molecules ◽  
2018 ◽  
Vol 23 (10) ◽  
pp. 2447 ◽  
Author(s):  
Michelina Catauro ◽  
Elisabetta Tranquillo ◽  
Alessia Salzillo ◽  
Lucia Capasso ◽  
Michela Illiano ◽  
...  

Chlorogenic acid (CGA) is a very common dietary polyphenolic compound. CGA is becoming very attractive due to its potential use as preventive and therapeutic agent in many diseases, including cancer. Inorganic/organic hybrid materials are gaining considerable attention in the biomedical field. The sol-gel process provides a useful way to obtain functional organic/inorganic hybrids. The aim of this study was to synthesize silica/polyethylene glycol (PEG) hybrids with different percentages of CGA by sol-gel technique and to investigate their impact on the cancer cell proliferation. Synthesized materials have been chemically characterized through the FTIR spectroscopy and their bioactivity evaluated looking by SEM at their ability to produce a hydroxyapatite layer on their surface upon incubation with simulated body fluid (SBF). Finally, their effects on cell proliferation were studied in cell lines by direct cell number counting, MTT, flow cytometry-based cell-cycle and cell death assays, and immunoblotting experiments. Notably, we found that SiO2/PEG/CGA hybrids exhibit clear antiproliferative effects in different tumor, including breast cancer and osteosarcoma, cell lines in a CGA dependent manner, but not in normal cells. Overall, our results increase the evidence of CGA as a possible anticancer agent and illustrate the potential for clinical applications of sol-gel synthesized SiO2/PEG/CGA materials.


Drug Delivery ◽  
2013 ◽  
Vol 21 (8) ◽  
pp. 595-604 ◽  
Author(s):  
M. Catauro ◽  
F. Bollino ◽  
F. Papale ◽  
S. Pacifico ◽  
S. Galasso ◽  
...  

2021 ◽  
Vol 11 (19) ◽  
pp. 9311
Author(s):  
Michelina Catauro ◽  
Ylenia D’Errico ◽  
Antonio D’Angelo ◽  
Ronald J. Clarke ◽  
Ignazio Blanco

The aim of this work was the synthesis of hybrid materials of iron (II)-based therapeutic systems via the sol-gel method. Increasing amounts of polyethylene glycol (PEG 6, 12, 24, 50 wt%) were added to SiO2/Fe20 wt% to modulate the release kinetics of the drug from the systems. Fourier-transform infrared (FTIR) spectroscopy was used to study the interactions between different components in the hybrid materials. The release kinetics in a simulated body fluid (SBF) were investigated, and the amount of Fe2+ released was detected via ultraviolet-visible spectroscopy (UV-Vis) after reaction with ortho-phenanthroline. Furthermore, biological characterization was carried out. The bioactivity of the synthesized hybrid materials was evaluated via the formation of a layer of hydroxyapatite on the surface of samples soaked in SBF using spectroscopy. Finally, the potential antibacterial properties of seven different materials against two different bacteria—E. coli and S. aureus—were investigated.


Materials ◽  
2020 ◽  
Vol 13 (2) ◽  
pp. 394 ◽  
Author(s):  
Michelina Catauro ◽  
Federico Barrino ◽  
Giovanni Dal Poggetto ◽  
Giuseppina Crescente ◽  
Simona Piccolella ◽  
...  

The sol–gel route represents a valuable technique to obtain functional materials, in which organic and inorganic members are closely connected. Herein, four hybrid materials, containing caffeic acid entrapped in a silica matrix at 5, 10, 15, and 20 wt.%, were synthesized and characterized through Fourier-Transform Infrared (FT-IR) and Ultraviolet-Visible (UV–Vis) spectroscopy. FT-IR analysis was also performed to evaluate the ability to induce the hydroxyapatite nucleation. Despite some structural changes occurring on the phenol molecular skeleton, hybrid materials showed scavenging properties vs. 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical and 2,2′-azinobis-(3-ethylbenzothiazolin-6-sulfonic acid) radical cation (ABTS•+), which was dependent on the tested dose and on the caffeic acid wt.%. The SiO2/caffeic acid materials are proposed as valuable antibacterial agents against Escherichia coli and Enterococcus faecalis.


Materials ◽  
2019 ◽  
Vol 12 (1) ◽  
pp. 148 ◽  
Author(s):  
Michelina Catauro ◽  
Federico Barrino ◽  
Giovanni Dal Poggetto ◽  
Giuseppina Crescente ◽  
Simona Piccolella ◽  
...  

The formation of pro-oxidant species after implantation of biomaterials could be responsible for the failure of the implant itself, because of oxidative stress-induced damage. In this work, the SiO2/polyethylene glycol (PEG)/chlorogenic acid (CGA) hybrids synthesized by the sol–gel method with 50 wt% of the polymer and different amounts of CGA (5, 10, 15 and 20 wt%) were studied. The hybrids soaked in simulated body fluid (SBF) showed the formation of hydroxyapatite layers on their surface, suggesting that the hybrids are bioactive. Their radical scavenging capacity towards DPPH· and ABTS·+ (2,2′-Azino-bis(3-ethylbenzthiazoline-6-sulfonic acid), evaluated at three different doses (0.5, 1 and 2 mg), showed probe- and dose-dependent behavior. In addition, the antioxidant properties of CGA were not affected by the presence of high amounts of the polymer. The in vitro biocompatibility in three cell lines (NIH 3T3, HaCaT and SH-SY5Y) was assessed by using the 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay. Apart from SH-SY5Y, the cell viability—expressed as mitochondrial redox activity percentage of cells directly exposed to powders—and morphology was not affected, suggesting that the hybrids have the ability to interfere and act selectively against tumor cells. The antibacterial properties of the different materials against Escherichia coli and Enterococcus faecalis were affected by different amounts of the natural antioxidant component.


2014 ◽  
Vol 898 ◽  
pp. 37-40
Author(s):  
Xiao Tian Ke ◽  
Cao Huang ◽  
Jin Ling Zhang ◽  
Gang Wu

PCEC-CaO-SiO2hybrid material was synthesized by a two steps method. FTIR results proved the structure of the telechelic PCEC with triethoxysilane-propyl end groups synthesized in the first step. Then the PCEC-CaO-SiO2hybrid material was synthesized by Sol-gel method. The chemical link between the functionalized polymer and the organic components prevent the hybrid materials brittle crack. The compressive strength was increased with the inorganic contents increasing in the hybrid materials. The hydrophilic PEG contents of PCEC accelerate the hydroxyapatite deposition on the hybrid materials after it was soaked in the SBF for a period of time.


Materials ◽  
2018 ◽  
Vol 11 (11) ◽  
pp. 2270 ◽  
Author(s):  
Michelina Catauro ◽  
Elisabetta Tranquillo ◽  
Federico Barrino ◽  
Ignazio Blanco ◽  
Francesco Dal Poggetto ◽  
...  

The use of oral iron integration is commonly recommended for the treatment of iron deficiency, nevertheless the diagnosis and treatment of this disease could clearly be improved. The aim of this work was the synthesis of therapeutic systems, iron (II) based, by sol-gel method. In an SiO2 matrix, we embedded different weight percentages of polyethylene glycol (PEG6, 12, 24 wt%) and ferrous citrate (Fe(II)C5, 10, 15 wt%) for drug delivery applications. Fourier Transform Infrared (FTIR) spectroscopy was used to study the interactions among different components in the hybrid materials. Release kinetics in a simulated body fluid (SBF) were investigated and the amount of Fe2+ released was detected by Ultraviolet–Visible spectroscopy (UV-VIS) after reaction with ortho-phenantroline. Furthermore, the biological characterization was carried out. The bioactivity of the synthesized hybrid materials was evaluated by the formation of a layer of hydroxyapatite on the surface of samples soaked in SBF using FTIR spectroscopy. Finally, also, the potential antibacterial properties of the different materials against two different bacteria, E. coli and P. aeruginosa, were investigated.


2016 ◽  
Vol 88 (12) ◽  
pp. 1117-1128 ◽  
Author(s):  
Bruno Sena da Fonseca ◽  
Susana Piçarra ◽  
Ana Paula Ferreira Pinto ◽  
Maria de Fátima Montemor

AbstractThe overall performance of alkoxysilanes as stone consolidants is constrained by stone mineralogy (particularly in the carbonate varieties) and by their tendency to crack during drying. In an attempt to overcome these problems, polyethylene glycol “chains” with two carboxylic acid end-groups (PEG-CA) were introduced in siloxane sols obtained by sol-gel chemistry using tetraethoxysilane (TEOS) as precursor. Different pre-condensation degrees (by varying the stirring times of sol-gel reaction: 10 min, 2, and 24 h) and PEG-CA chains with different molecular weights were studied as variables affecting the initial efficacy of the consolidants when applied into a limestone. The sol containing siloxanes with the lowest pre-condensation degree (10 min stirring) was quite susceptible to the carbonate media and thus a poor consolidation was achieved. The sol with the highest pre-condensation degree (24 h stirring) together with the PEG-CA chains with intermediate molecular weight produced significant and uniform strength gains along the stone depth. The consolidation also showed to be highly dependent on the molecular weight of the PEG-CA chains, the PEG-CA with highest molecular weight produced a non-uniform strength increase with potential harmful side effects. The results confirmed the role of carboxylic acid end-groups as efficient sol-gel catalysts and their ability to be incorporated into the silica matrix in the presence of carbonate stone.


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