by Keyword: Characterization
Lozano, H., Millán-Solsona, R., Fabregas, R., Gomila, G., (2019). Sizing single nanoscale objects from polarization forces Scientific Reports 9, (1), 14142
Sizing natural or engineered single nanoscale objects is fundamental in many areas of science and technology. To achieve it several advanced microscopic techniques have been developed, mostly based on electron and scanning probe microscopies. Still for soft and poorly adhered samples the existing techniques face important challenges. Here, we propose an alternative method to size single nanoscale objects based on the measurement of its electric polarization. The method is based on Electrostatic Force Microscopy measurements combined with a specifically designed multiparameter quantification algorithm, which gives the physical dimensions (height and width) of the nanoscale object. The proposed method is validated with ~50 nm diameter silver nanowires, and successfully applied to ~10 nm diameter bacterial polar flagella, an example of soft and poorly adhered nanoscale object. We show that an accuracy comparable to AFM topographic imaging can be achieved. The main advantage of the proposed method is that, being based on the measurement of long-range polarization forces, it can be applied without contacting the sample, what is key when considering poorly adhered and soft nanoscale objects. Potential applications of the proposed method to a wide range of nanoscale objects relevant in Material, Life Sciences and Nanomedicine is envisaged.
Keywords: Characterization and analytical techniques, Imaging techniques
Vidal, E., Buxadera-Palomero, J., Pierre, C., Manero, J. M., Ginebra, M. P., Cazalbou, S., Combes, C., Rupérez, E., Rodríguez, D., (2019). Single-step pulsed electrodeposition of calcium phosphate coatings on titanium for drug delivery Surface and Coatings Technology 358, 266-275
Metallic implants have some limitations related to bioactivity and bacteria colonization leading to infections. In this regard, calcium phosphate coatings can be used as carrier for drug delivery in order to improve the mentioned drawbacks. The present work proposes the introduction of an antibacterial agent in the course of a pulsed and reverse pulsed electrodeposition. Calcium phosphate coatings were prepared in 30 min using different pulse waveforms (unipolar-bipolar), current densities (2–5 mA/cm2) and temperatures (40–60 °C). Mechanical stability of the as-coated surfaces was studied in order to select the optimal electrodeposition conditions. Subsequently, selected coatings were loaded with an antiseptic agent, chlorhexidine digluconate (CHX), via a single-step co-deposition procedure. CHX concentration added to the electrolyte was adjusted to 3 mM based on the antibacterial efficacy of the loaded coatings evaluated in vitro with Staphylococcus aureus and Escherichia coli bacteria strains. Whereas the same chlorhexidine concentration was added to the electrolyte, results showed that the amount of CHX loaded was different for each condition while release kinetics was maintained. The results of this work demonstrate that a pulsed co-deposition strategy has great potential to modulate local delivery of antibacterial agents such as chlorhexidine digluconate, which may prevent early phase infections of metallic implants after insertion.
Keywords: Antibacterial agent, Calcium phosphate, Characterization, Coating, Pulse electrodeposition, Titanium
Garde, A., Giraldo, B. F., Jané, R., Latshang, T. D., Turk, A. J., Hess, T., Bosch, M-.M., Barthelmes, D., Merz, T. M., Hefti, J. Pichler, Schoch, O. D., Bloch, K. E., (2015). Time-varying signal analysis to detect high-altitude periodic breathing in climbers ascending to extreme altitude Medical & Biological Engineering & Computing , 53, (8), 699-712
This work investigates the performance of cardiorespiratory analysis detecting periodic breathing (PB) in chest wall recordings in mountaineers climbing to extreme altitude. The breathing patterns of 34 mountaineers were monitored unobtrusively by inductance plethysmography, ECG and pulse oximetry using a portable recorder during climbs at altitudes between 4497 and 7546 m on Mt. Muztagh Ata. The minute ventilation (VE) and heart rate (HR) signals were studied, to identify visually scored PB, applying time-varying spectral, coherence and entropy analysis. In 411 climbing periods, 30–120 min in duration, high values of mean power (MPVE) and slope (MSlopeVE) of the modulation frequency band of VE, accurately identified PB, with an area under the ROC curve of 88 and 89 %, respectively. Prolonged stay at altitude was associated with an increase in PB. During PB episodes, higher peak power of ventilatory (MPVE) and cardiac (MP LF HR ) oscillations and cardiorespiratory coherence (MP LF Coher ), but reduced ventilation entropy (SampEnVE), was observed. Therefore, the characterization of cardiorespiratory dynamics by the analysis of VE and HR signals accurately identifies PB and effects of altitude acclimatization, providing promising tools for investigating physiologic effects of environmental exposures and diseases.
Keywords: High-altitude periodic breathing, Cardiorespiratory characterization, Time-varying spectral analysis, Acclimatization, Hypoxia
Castaño, O., Sachot, N., Xuriguera, E., Engel, E., Planell, J. A., Park, J. H., Jin, G. Z., Kim, T. H., Kim, J. H., Kim, H. W., (2014). Angiogenesis in bone regeneration: Tailored calcium release in hybrid fibrous scaffolds ACS Applied Materials & Interfaces 6, (10), 7512-7522
In bone regeneration, silicon-based calcium phosphate glasses (Bioglasses) have been widely used since the 1970s. However, they dissolve very slowly because of their high amount of Si (SiO2 > 45%). Recently, our group has found that calcium ions released by the degradation of glasses in which the job of silicon is done by just 5% of TiO2 are effective angiogenic promoters, because of their stimulation of a cell-membrane calcium sensing receptor (CaSR). Based on this, other focused tests on angiogenesis have found that Bioglasses also have the potential to be angiogenic promoters even with high contents of silicon (80%); however, their slow degradation is still a problem, as the levels of silicon cannot be decreased any lower than 45%. In this work, we propose a new generation of hybrid organically modified glasses, ormoglasses, that enable the levels of silicon to be reduced, therefore speeding up the degradation process. Using electrospinning as a faithful way to mimic the extracellular matrix (ECM), we successfully produced hybrid fibrous mats with three different contents of Si (40, 52, and 70%), and thus three different calcium ion release rates, using an ormoglass–polycaprolactone blend approach. These mats offered a good platform to evaluate different calcium release rates as osteogenic promoters in an in vivo subcutaneous environment. Complementary data were collected to complement Ca2+ release analysis, such as stiffness evaluation by AFM, ζ-potential, morphology evaluation by FESEM, proliferation and differentiation analysis, as well as in vivo subcutaneous implantations. Material and biological characterization suggested that compositions of organic/inorganic hybrid materials with a Si content equivalent to 40%, which were also those that released more calcium, were osteogenic. They also showed a greater ability to form blood vessels. These results suggest that Si-based ormoglasses can be considered an efficient tool for calcium release modulation, which could play a key role in the angiogenic promoting process.
Keywords: Biological materials, Blood vessels, Calcium, Electrospinning, Glass, Hybrid materials, Silicon oxides, Sol-gel process, Sol-gels, Angiogenesis, Biological characterization, Calcium phosphate glass, Calcium-sensing receptors, Degradation process, Extracellular matrices, Organic/inorganic hybrid materials, ormoglasses, Silicon
Serra, T., Ortiz-Hernandez, M., Engel, E., Planell, J. A., Navarro, M., (2014). Relevance of PEG in PLA-based blends for tissue engineering 3D-printed scaffolds Materials Science and Engineering: C 38, (1), 55-62
Achieving high quality 3D-printed structures requires establishing the right printing conditions. Finding processing conditions that satisfy both the fabrication process and the final required scaffold properties is crucial. This work stresses the importance of studying the outcome of the plasticizing effect of PEG on PLA-based blends used for the fabrication of 3D-direct-printed scaffolds for tissue engineering applications. For this, PLA/PEG blends with 5, 10 and 20% (w/w) of PEG and PLA/PEG/bioactive CaP glass composites were processed in the form of 3D rapid prototyping scaffolds. Surface analysis and differential scanning calorimetry revealed a rearrangement of polymer chains and a topography, wettability and elastic modulus increase of the studied surfaces as PEG was incorporated. Moreover, addition of 10 and 20% PEG led to non-uniform 3D structures with lower mechanical properties. In vitro degradation studies showed that the inclusion of PEG significantly accelerated the degradation rate of the material. Results indicated that the presence of PEG not only improves PLA processing but also leads to relevant surface, geometrical and structural changes including modulation of the degradation rate of PLA-based 3D printed scaffolds.
Keywords: 3D-printing, Polylactic acid, Rapid prototyping, Scaffold, Surface characterization
Torrent-Burgués, J., Cea, P., Giner, I., Guaus, E., (2014). Characterization of Langmuir and Langmuir-Blodgett films of an octasubstituted zinc phthalocyanine Thin Solid Films , 556, 485-494
In this work we report the fabrication of Langmuir and Langmuir-Blodgett (LB) films of a substituted ZnPc (octakis(oxyoctyl)phthalocyanine of zinc), and their characterization by means of several techniques. These characterization techniques include surface pressure (Ï€-A) and surface potential (Î”V-A) isotherms as well as UV-vis Reflection spectroscopy and Brewster Angle Microscopy (BAM) for the films at the air-water interface together with UV-vis absorption and IR spectroscopies and Atomic Force Microscopy (AFM) for the LB films. The Ï€-A and Î”V-A isotherms and BAM images indicate a phase transition at a surface pressure of ca. 9 mN/m and a multilayer formation at surface pressures around 19-20 mN/m; at a surface pressure around 27 mN/m a disordered collapse of the film occurs. In addition, AFM images of LB films at Ï€ = 10 mN/m and Ï€ = 20 mN/m show a monomolecular and a multilayered film, respectively. The comparison of the UV-vis spectrum of ZnPc in solution, the reflection spectra of the Langmuir films and UV-vis spectra of LB films reveals a significant reduction in the Q band intensity for the films, indicative of an organization of ZnPc in the Langmuir and LB films versus the random distribution in solution. The UV-vis Reflection spectra are also consistent with multilayer formation at surface pressures around 19-20 mN/m. The relative intensities of the IR spectrum bands change from the KBr pellet to the LB film which is also attributable to orientation effects in the film. Cyclic voltammetric experiments of LB films incorporating the ZnPc derivative show peaks that can be correlated with redox processes occurring in the phthalocyanine ring. A small but significant influence of the surface pressure and the number of deposited layers in the electrochemical behaviour is observed. The electrochemical response of cast films exhibits some differences with respect to that of LB films which have been attributed to their different molecular organizations.
Keywords: Atomic Force Microscopy, Electrochemistry, Langmuir-Blodgett, Multilayers, Optical spectroscopy techniques, Zinc phthalocyanine, Atomic force microscopy, Electrochemistry, Interfaces (materials), Isotherms, Multilayers, Nitrogen compounds, Optical multilayers, Organic polymers, Zinc compounds, Brewster angle microscopy, Characterization techniques, Electrochemical behaviour, Langmuir and langmuir-blodgett films, Langmuir-blodgett, Optical spectroscopy techniques, UV-Vis Reflection Spectroscopy, Zinc phthalocyanines, Langmuir Blodgett films
Arcentales, A., Voss, A., Caminal, P., Bayes-Genis, A., Domingo, M. T., Giraldo, B. F., (2013). Characterization of patients with different ventricular ejection fractions using blood pressure signal analysis CinC 2013 Computing in Cardiology Conference (CinC) , IEEE (Zaragoza, Spain) , 795-798
Ischemic and dilated cardiomyopathy are associated with disorders of myocardium. Using the blood pressure (BP) signal and the values of the ventricular ejection fraction, we obtained parameters for stratifying cardiomyopathy patients as low- and high-risk. We studied 48 cardiomyopathy patients characterized by NYHA ≥2: 19 patients with dilated cardiomyopathy (DCM) and 29 patients with ischemic cardiomyopathy (ICM). The left ventricular ejection fraction (LVEF) percentage was used to classify patients in low risk (LR: LVEF > 35%, 17 patients) and high risk (HR: LVEF ≤ 35%, 31 patients) groups. From the BP signal, we extracted the upward systolic slope (BPsl), the difference between systolic and diastolic BP (BPA), and systolic time intervals (STI). When we compared the LR and HR groups in the time domain analysis, the best parameters were standard deviation (SD) of 1=STI, kurtosis (K) of BPsl, and K of BPA. In the frequency domain analysis, very low frequency (VLF) and high frequency (HF) bands showed statistically significant differences in comaprisons of LR and HR groups. The area under the curve of power spectral density was the best parameter in all classifications, and particularly in the very-low-and high- frequency bands (p <; 0.001). These parameters could help to improve the risk stratification of cardiomyopathy patients.
Keywords: blood pressure measurement, cardiovascular system, diseases, medical disorders, medical signal processing, statistical analysis, time-domain analysis, BP signal, HR groups, LR groups, blood pressure signal analysis, cardiomyopathy patients, diastolic BP, dilated cardiomyopathy, frequency domain analysis, high-frequency bands, ischemic cardiomyopathy, left ventricular ejection fraction, low-frequency bands, myocardium disorders, patient characterization, power spectral density curve, standard deviation, statistical significant differences, systolic BP, systolic slope, systolic time intervals, time domain analysis, ventricular ejection fraction, Abstracts, Databases, Parameter extraction, Telecommunication standards, Time-frequency analysis
Giraldo, B. F., Chaparro, J. A., Caminal, P., Benito, S., (2013). Characterization of the respiratory pattern variability of patients with different pressure support levels Engineering in Medicine and Biology Society (EMBC) 35th Annual International Conference of the IEEE , IEEE (Osaka, Japan) , 3849-3852
One of the most challenging problems in intensive care is still the process of discontinuing mechanical ventilation, called weaning process. Both an unnecessary delay in the discontinuation process and a weaning trial that is undertaken too early are undesirable. In this study, we analyzed respiratory pattern variability using the respiratory volume signal of patients submitted to two different levels of pressure support ventilation (PSV), prior to withdrawal of the mechanical ventilation. In order to characterize the respiratory pattern, we analyzed the following time series: inspiratory time, expiratory time, breath duration, tidal volume, fractional inspiratory time, mean inspiratory flow and rapid shallow breathing. Several autoregressive modeling techniques were considered: autoregressive models (AR), autoregressive moving average models (ARMA), and autoregressive models with exogenous input (ARX). The following classification methods were used: logistic regression (LR), linear discriminant analysis (LDA) and support vector machines (SVM). 20 patients on weaning trials from mechanical ventilation were analyzed. The patients, submitted to two different levels of PSV, were classified as low PSV and high PSV. The variability of the respiratory patterns of these patients were analyzed. The most relevant parameters were extracted using the classifiers methods. The best results were obtained with the interquartile range and the final prediction errors of AR, ARMA and ARX models. An accuracy of 95% (93% sensitivity and 90% specificity) was obtained when the interquartile range of the expiratory time and the breath duration time series were used a LDA model. All classifiers showed a good compromise between sensitivity and specificity.
Keywords: autoregressive moving average processes, feature extraction, medical signal processing, patient care, pneumodynamics, signal classification, support vector machines, time series, ARX, autoregressive modeling techniques, autoregressive models with exogenous input, autoregressive moving average model, breath duration time series, classification method, classifier method, discontinuing mechanical ventilation, expiratory time, feature extraction, final prediction errors, fractional inspiratory time, intensive care, interquartile range, linear discriminant analysis, logistic regression analysis, mean inspiratory flow, patient respiratory volume signal, pressure support level, pressure support ventilation, rapid shallow breathing, respiratory pattern variability characterization, support vector machines, tidal volume, weaning trial, Analytical models, Autoregressive processes, Biological system modeling, Estimation, Support vector machines, Time series analysis, Ventilation
Kuphal, M., Mills, C.A., Korri-Youssoufi, H., Samitier, J., (2012). Polymer-based technology platform for robust electrochemical sensing using gold microelectrodes Sensors and Actuators B: Chemical 161, (1), 279-284
Rapid and inexpensive development of electrochemical sensors with good exploitation potential may be produced using a polymer as a substrate material. However, fabrication of polymer-based sensors is challenging. Using photolithography and etching of gold-coated poly(ethylene-2,6-naphthalate) (PEN), we have succeeded in fabricating disk-shaped and interdigitated microelectrodes (uEs). The electrodes have an excellent adhesion to the polymer and are encapsulated using a novel room-temperature process, applicable for low-cost, high-throughput fabrication. The PEN surface has been characterized in respect of wettability, surface energy and surface roughness. Finally, the electrodes give stable and reproducible electrochemical impedance spectroscopy and cyclic voltammetry responses, using the redox couple ferrocyanide and ruthenium hexamine. The results demonstrate the robustness and functionality of the polymer-based sensor platform with minimum feature sizes of 6 um.
Keywords: Poly(ethylene naphthalate), Photolithography, Microelectrodes, Interdigitated electrodes, Electrochemical characterization, Electrochemical sensor