Exploring the physicochemical traits, antifungal capabilities, and 3D spatial complexity of hydroxyapatite with Ag+Mg2+ substitution in the biocomposite thin films.

The silver/magnesium doped hydroxyapatite (AgMgHAp, Ca10-x-yAgxMgy(PO4)6(OH)2, xAg=0.05 and yMg=0.02) nanocomposites coatings were deposited on Si substrate using the dip coating technique. The resulting coatings were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared (FTIR-ATR) spectroscopy, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The EDS analysis highlighted the presence of the constitutive elements of the silver/magnesium doped hydroxyapatite (AgMgHAp) nanocomposites coatings. The surface microtexture of the AgMgHAp was assessed by atomic force microscopy (AFM) technique. The AFM data suggested the obtaining of a uniform deposited layer comprised of equally distributed nanoconglomerates. FT-IR studies highlighted the presence of vibrational modes associated with the phosphate and hydroxyl groups. No bands associated with silver or magnesium were observed. The XPS analysis highlighted the presence of the constituent elements of hydroxyapatite (Ca 2p, P 2 s, O 1 s), as well as dopants (Ag 3d, Mg 1 s and Mg 2p). The antifungal evaluation of AgMgHAp coatings was carried out using the Candida albicans ATCC 10231 fungal strain. The results of the antifungal assay revealed that the AgMgHAp coatings exhibited a strong inhibitory antifungal activity. Furthermore, the data highlighted that the AgMgHAp inhibited the development of biofilm on their surface. The results revealed that the antifungal activity of the coating varied based on the duration of incubation. On the other hand, the data also showed that AgMgHAp nanocomposites coatings inhibited the fungal cell adhesion and development from the early stages of the incubation. In addition to morphological analysis, we additionally take advantage of AFM images to investigate and explore the domain of fractal and multifractal analysis applied to the films under evaluation. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. Our studies indicates that nanocomposite coatings made from AgMgHAp demonstrate strong antifungal properties. These results suggest the potential of AgMgHAp nanocomposite coatings as a promising solution for developing innovative antifungal devices in biomedical applications.

Investigation of microstructural, micromorphology, and surface plasmon resonance characteristics in Ni/Al, Ni/Cu, and Ni/SS thin films.

As the first boundary between the environment and the material, the surface plays an important role in their interaction with each other, therefore, the use of appropriate tools and analysis to examine the mechanical properties and morphology of surfaces has particular importance in industry and research. In this research, a thin film of nickel was deposited on metal substrates made of aluminum, copper, and steel by using the RF magnetic cathode. Then, using a non-contact atomic force microscope, the morphological properties of the nickel film with static parameters, Minkowski functionals (MF's), fractal, and multifractal were extracted to be analyzed and studied. After that, using parameters such as root mean square (RMS) roughness, skewness, and kurtosis, it was determined how the surface roughness, distribution, and probability density of particles on the film surface alters with the change of the substrate. Next, by examining and analyzing the Δα and Δf parameters obtained from the multifractal section, the morphology of the produced film on the metal substrates was investigated. Then, the change in the surface plasmon resonance (SPR) peak position is changed for the prepared film in the range of the absorption spectrum due to the substrate effect and the microstructural properties of the formed film. HIGHLIGHTS: Ni film has been deposited by Rf magnetron sputtering. The effect of metal substrates on the topography, fractality, and optical properties was studied. Minkowski functionals were used to investigate the surface morphology of the samples. Substrate's material and the topography of the formed film can changed the surface plasmon resonance position.

Influence of film thickness on structural, optical, and electrical properties of sputtered nickel oxide thin films.

Utilizing radio frequency magnetron sputtering, we successfully fabricated nickel oxide thin films with different thickness (from 80 to 270 nm), and conducted an in-depth examination of their structural, morphological, optical, and electrical properties. The crystal structure and surface roughness were determined using x-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. The XRD analyses showed that the films were composed of cubic nickel oxide, exhibiting a notable orientation along the (200) direction. This crystal texture partially increased when the film thickness reached 270 nm. In addition, a direct correlation between film thickness and crystallite size was observed, with the latter increasing as the former did. AFM analysis provided insights into the surface morphology, revealing metrics like the bearing area, 3D surfaces intersections, and statistical properties of surface height. These insights underscore the relationship between film thickness and surface properties, which in turn influence the overall electrical, and prominently, optical properties of the films. Employing transmittance UV-visible spectroscopy, we characterized the optical behavior of these films, noting a proportional increase in refractive index with film thickness. Additionally, resistivity was observed to increase concomitantly with film thickness. In conclusion, the deposition process's film thickness acts as a pivotal parameter for fine-tuning the structural, morphological, and optical properties of nickel oxide thin films. This knowledge paves the way for optimizing nickel oxide-based devices across various applications. RESEARCH HIGHLIGHTS: We synthesized and characterized of p-type semiconducting NiO thin films sputtered on substrates by using RF magnetron sputtering with different thickness. Advanced crystalline structures and fractal features extracted from XRD and AFM analysis.  The 2D and 3D surface analysis of the samples indicates a complex structure with an imperfect self-similarity that suggests a multifractal structure. We represented graphically the relative representation of higher geometric objects in the AFM image. We attributed the optical and electrical properties of the samples to the crystallite size, and the concurrent reduction in oxygen vacancies and crystalline defects within the films.

Evaluating the roughness dynamics of kefir biofilms grown on Amazon cupuaçu juice: a monofractal and multifractal approach.

We conducted a comprehensive analysis of the surface microtexture of kefir biofilms grown on Theobroma grandiflorum Shum (cupuaçu) juice using atomic force microscopy. Our goal was to investigate the unique monofractal and multifractal spatial patterns of these biofilms to complement the existing limited literature. The biofilms were prepared dispersing four different concentrations of kefir grains in cupuaçu juice. Our morphological analysis showed that the surface of the obtained biofilms is essentially formed by the presence of cupuaçu fibers and microorganisms like lactobacilli and yeast. The topographic height-based parameter analysis reveals that there is a dependence between surface roughness and the concentration of kefir grains used. The strongly anisotropic well-centralized topographical height distribution of the biofilms also exhibited a quasi-symmetrical and platykurtic pattern. The biofilms exhibit comparable levels of spatial complexity, surface percolation and surface homogeneity, which can be attributed to their similar topographic uniformity. This aspect was further supported by the presence of similar multifractality in the biofilms, suggesting that despite their varying topographic roughness, their vertical growth dynamics follow a similar pattern. Our findings demonstrate that the surface roughness of kefir biofilms cultivated on cupuaçu juice is influenced by the concentration of kefir grains in the precursor solution. However, this dependence follows a consistent pattern across different concentrations. Graphical Abstract.

Dual effect to improve the electrical properties of SZO films grown by nitrogen pneumatic spray pyrolysis.

The principal aim of this study is to reduce considerably, via Sn doping, the resistivity of ZnO thin films prepared by simple, flexible, and cost-effective nitrogen pneumatic spray pyrolysis (NPSP) method on glass substrates at a temperature of 400°C. Different Sn content was tested (Sn/Zn = 0, 1, 3, 5 wt%) in an attempt to reduce the concentration of excessive oxygen atoms and create more free electrons. The microstructural, optical, morphological, and electrical properties of the films have been studied. The x-ray diffraction analysis demonstrated that tin-doped SZO films exhibited polycrystalline nature with a preferential orientation along (002) plane with the appearance of a new orientation (101) with the increase of Sn concentration leading then to bidirectional growth. The deposited SZO films showed an average optical transmittance of about 80% in the UV-visible region (200-800 nm) with optical band gap values at around 3.27 eV. Photoluminescence emissions of SZO samples presented three main peaks: near band edge emission, violet emission, and the blue-green emission. The surface morphology of the films obtained by scanning electron microscope (SEM) exhibited the change in morphology with increasing the Sn content. A minimum electrical resistivity value of about 17·10-3 Ω·cm was obtained for 3% SZO films. SZO films prepared by the NPSP method can be used as transparent window layer and electrodes in solar cells. RESEARCH HIGHLIGHTS: Highly oriented, conducting, and transparent Sn-doped ZnO films are successfully synthesized. The film growth orientation changed from mono-directional (002) axis to bi-directional (002) and (101) axis according to Sn doping. Ultraviolet and green emissions are noted by photoluminescence investigation. A minimum resistivity is observed for 3 wt% SZO film. The dual positive effect of the carrier gas used (N2) and Sn doping is confirmed.

Effects of Substitution and Substrate Strain on the Structure and Properties of Orthorhombic Eu1-xYxMnO3 (0 ≤ x ≤ 0.5) Thin Films.

The effects on the structure and magnetic properties of Eu1-xYxMnO3 (0.0 ≤ x ≤ 0.5) thin films due to lattice strain were investigated and compared with those obtained in equivalent composition ceramics. The films were deposited by spin-coating chemical solution onto Pt\TiO2\SiO2\Si (100) standard substrates. X-ray diffraction and Raman spectroscopy measurements revealed that all films crystallize in orthorhombic structure with space group Pnma, observing an added contraction of the unit cell with increasing Y-substitution ou Eu, corresponding to a broadening of the Mn-O1-Mn angle and a gradual decrease in magnetic order response.

Electrolyte pH dependence of composition, roughness parameters, particle diameter and magnetic features of nanostructured Fe-Co-Ni/ITO deposits prepared by electrochemical deposition method.

The composition, structural features, surface morphology, roughness parameters, particle size, and magnetic features of nanostructured Fe-Co-Ni deposits manufactured on conducting indium tin oxide-coated glasses at various electrolyte pH values are studied. The deposit produced at low electrolyte pH contains slightly higher Fe and Co contents but lower Ni content compared to deposits fabricated at high pH values. Further composition analysis confirms that the reduction rates of Fe2+ and Co2+ are higher than the Ni2+ reduction rate. The films consist of nano-sized crystallites with a strong [111] preferred orientation. The results also reveal that the crystallization of the thin films is affected by the electrolyte pH. Surface analysis shows that the deposit surfaces are composed of nano-sized particles with different diameters. The mean particle diameter and surface roughness decrease as the pH of the electrolyte decreases. The effect of the electrolyte pH on the morphology is also discussed in terms of surface skewness and kurtosis parameters. Magnetic analysis shows that the resultant deposits have in-plane hysteresis loops with low and close SQR parameters ranging from 0.079 to 0.108. The results also reveal that the coercive field of the deposits increases from 29.4 Oe to 41.3 Oe as the electrolyte pH decreases from 4.7 to 3.2.

Insights into the Fe3+ Doping Effects on the Structure and Electron Distribution of Cr2O3 Nanoparticles.

Herein, we carefully investigated the Fe3+ doping effects on the structure and electron distribution of Cr2O3 nanoparticles using X-ray diffraction analysis (XRD), maximum entropy method (MEM), and density functional theory (DFT) calculations. We showed that increasing the Fe doping induces an enlargement in the axial ratio of c/a, which is associated with an anisotropic expansion of the unit cell. We found that as Fe3+ replaces Cr in the Cr2O3 lattice, it caused a higher interaction between the metal 3d states and the oxygen 2p states, which led to a slight increase in the Cr/Fe-O1 bond length followed by an opposite effect for the Cr/Fe-O2 bonds. Our results also suggest that the excitations characterize a well-localized bandgap region from occupied Cr d to unoccupied Fe d states. The Cr2O3 and Fe-doped Cr2O3 nanoparticles behave as Mott-Hubbard insulators due to their band gap being in the d-d gap, and Cr 3d orbitals dominate the conduction band. These findings suggest that the magnitude and the character of the electronic density near the O atom bonds in Cr2O3 nanoparticles are modulated by the Cr-Cr distances until its stabilization at the induced quasi-equilibrium of the Cr2O3 lattice when the Fe3+ doping values reaches the saturation level range.

Evaluating structural, morphological, and multifractal aspects of n-ZnO/p-ZnO homojunctions and n-ZnO/p-NiO heterojunctions.

We have investigated the evolution of the structure and surface morphology of n-ZnO/p-ZnO homojunctions and n-ZnO/p-NiO heterojunctions transparent structures deposited by radio frequency-sputtering on quartz (Q)/ITO substrates. X-ray diffraction (XRD) analysis of the as-deposited and annealed ZnO, n-ZnO/p-NiO/Q/ITO, and n-ZnO/p-ZnO/Q/ITO thin films showed that ZnO had a wurtzite hexagonal structure and (002) preferred growth direction. The annealing temperature played a key role in improving the crystalline structure of the films, as evidenced by the changes in the intensity and position of the XRD (002) peak. Morphological analysis revealed that the roughness of the film varies with increasing annealing temperature. Particle size dictates the vertical growth of p-ZnO homojunctions, while particle shape dictated the p-NiO heterojunctions growth. Fractal analysis showed that p-ZnO homojunctions have similar spatial complexity, surface percolation, and topographical uniformity and are dominated by low dominant frequencies. Moreover, a robust multifractal character was observed, where n-ZnO/p-ZnO homojunctions follow similar vertical growth dynamics, which differed from the n-ZnO/p-NiO heterojunctions growth dynamics. These results prove that annealing temperature plays a key role in the n-ZnO/p-ZnO homojunctions and n-ZnO/p-NiO heterojunctions structure, surface morphology, and vertical growth dynamics.

Investigation of deposition temperature effect on spatial patterns of MgF2 thin films.

In this work, the atomic force microscopy (AFM) technique was used to characterize 3D MgF2 thin film surfaces through advanced analysis involving morphological, fractal, multifractal, succolarity, lacunarity and surface entropy (SE) parameters, consistent with ISO 25178-2: 2012. Samples were synthesized by electron beam deposition, grown in three different temperatures. Three different temperatures of 25°C (laboratory temperature), 150 and 300°C were chosen. The temperature of 300°C is usually the highest temperature that can be deposited with the electron beam evaporation coating system. The substrates were made of glass (diameter 16 mm, thickness 3 mm), and the samples were prepared at a pressure of 5 × 10-5  Torr. The statistical results from the AFM images indicate that topographic asperities decrease with increasing deposition temperature, showing a decrease in roughness values. Regardless of the deposition temperature, all surfaces have a self-similar behavior, presenting a very linear PSD distribution, and, according to our results, the sample deposited at 300° had the highest spatial complexity. On the other hand, surface percolation is increasing when temperature increases, indicating that its low roughness and high spatial complexity play an important role on the formation of their most percolating surface microtexture. Our results demonstrate that the lower deposition temperature promoted the formation of less discontinuous height distributions in the MgF2 films.

Morphological and multifractal properties of Cr thin films deposited onto different substrates.

In this study, the morphological properties and micro-roughness of chromium thin film prepared by thermal evaporation technique and confirmed via EDS analysis are examined on different substrates of BK7, Silicon (Si), and glass using atomic force microscope analysis (AFM). Analysis of amplitude parameters, Minkowski functionals, and films' spatial microtexture extracted from AFM analysis showed the difference between glass substrate and the other two (BK7 and Si) substrates for the growth of chromium thin films. In addition, we observed robust signatures of multifractality of the Cr thin films deposited on all substrates we studied. Moreover, we highlight that the Glass substrates displayed the strongest multifractality indicating that such samples present space filling properties distributed over more spatial scales than the samples of BK7 and Si.

New Physico-Chemical Analysis of Magnesium-Doped Hydroxyapatite in Dextran Matrix Nanocomposites.

The new magnesium-doped hydroxyapatite in dextran matrix (10MgHApD) nanocomposites were synthesized using coprecipitation technique. A spherical morphology was observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) characterization results show hydroxyapatite hexagonal phase formation. The element map scanning during the EDS analysis revealed homogenous distribution of constituent elements of calcium, phosphor, oxygen and magnesium. The presence of dextran in the sample was revealed by Fourier transform infrared (FTIR) spectroscopy. The antimicrobial activity of the 10MgHAPD nanocomposites was assessed by in vitro assays using Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, Streptococcus mutans ATCC 25175, Porphyromonas gingivalis ATCC 33277 and Candida albicans ATCC 10231 microbial strains. The results of the antimicrobial assays highlighted that the 10MgHApD nanocomposites presented excellent antimicrobial activity against all the tested microorganisms and for all the tested time intervals. Furthermore, the biocompatibility assays determined that the 10MgHApD nanocomposites did not exhibit any toxicity towards Human gingival fibroblast (HGF-1) cells.

An Electrochemical Immunosensor Based on Carboxylated Graphene/SPCE for IgG-SARS-CoV-2 Nucleocapsid Determination.

The COVID-19 pandemic has emphasized the importance and urgent need for rapid and accurate diagnostic tests for detecting and screening this infection. Our proposal was to develop a biosensor based on an ELISA immunoassay for monitoring antibodies against SARS-CoV-2 in human serum samples. The nucleocapsid protein (N protein) from SARS-CoV-2 was employed as a specific receptor for the detection of SARS-CoV-2 nucleocapsid immunoglobulin G. N protein was immobilized on the surface of a screen-printed carbon electrode (SPCE) modified with carboxylated graphene (CG). The percentage of IgG-SARS-CoV-2 nucleocapsid present was quantified using a secondary antibody labeled with horseradish peroxidase (HRP) (anti-IgG-HRP) catalyzed using 3,3',5,5'-tetramethylbenzidine (TMB) mediator by chronoamperometry. A linear response was obtained in the range of 1:1000-1:200 v/v in phosphate buffer solution (PBS), and the detection limit calculated was 1:4947 v/v. The chronoamperometric method showed electrical signals directly proportional to antibody concentrations due to antigen-antibody (Ag-Ab) specific and stable binding reaction.

Biodefensive Based on Piper nigrum Essential Oil for Controlling of Anopheles aquasalis Larvae: Influence of Temperature (35 °C) and Preservatives.

Considerable efforts have been spent on the development of biodefensives based on the encapsulation of essential oils for controlling of urban pests from their larval stage, especially as anopheline controlling agents. The larval source management of Anopheles aquasalis is important for malaria prevention. For this reason, this research proposes larvicidal biodefensives based on polymeric particles loaded with Piper nigrum essential oil, considering the influence of temperature (35 °C) and preservatives on the formulation stability. The biodefensive containing the preservative phenoxyethanol/methylisothiazolinone (PNE) resulted in 5 months of shelf-life storage with an Encapsulation Efficiency (EE%) of essential oil of 70%. The biodefensive PNE (containing 500 µg.mL-1 of encapsulated essential oil) presented a polydisperse particle size distribution, ranging from D10 = (127 ± 10) nm to D90 = (472 ± 78) nm and a particle mean size of (236 ± 34) nm. The AFM images revealed a spherical morphology with an external surface almost regular and smooth. The controlled release of the essential oil was evaluated up to 72 h according to the Korsmeyer-Peppas mathematical model, confirming the anomalous transport (n = 0.64 in pH = 3 and pH = 10, and n = 0.65 in pH = 7). The total larvae mortality on the in loco bioassays was almost reached (92%) after 24 h. However, according to the in vitro bioassays applying the in natura essential oil alone, the concentration of 454 µg.mL-1 resulted on the mortality of 70% of the larvae after 24 h. For this reason, the highest efficiency of the biodefensive PNE may be related to the encapsulation of essential oil, delivering the loaded particles more efficiently inside the larvae. From this perspective, the present study shows that a formulation based on P. nigrum essential oil may be taken into account in the integrated management of disease vector mosquitoes.

ITO:n-ZnO:p-NiO and ITO:n-ZnO:p-NZO thin films: Study of crystalline structures, surface statistical metrics, and optical properties.

The article presents results on fabrication and characterization of transparent, oxide-based junction diodes on quartz substrates. The devices are made by radio frequency magnetron sputtering in the form of sandwich structures: ITO:n-ZnO:p-NiO (homojunction) and ITO:n-ZnO:p-NZO (heterojunction). The microstructure, crystalline structure, and micromorphology features of deposited samples are studied by means of X-ray diffraction, Atomic Force Microscopy, and Scanning Electron Microscopy. Obtained results are used to derive statistical, fractal and functional surface characteristics that exhibited secondary alignment patterns. Apart from that, optical and electrical measurements are carried out as well. Optical transmittance peaked at 80% in visible range, but substantially increased after annealing. Due to structural differences, heterojunction was found to follow linear current-voltage dependence specific of ohmic contacts, whereas homojunction was found to follow non-linear characteristics as in junction diode.

Investigating the Correlation between the Microstructure and Electrical Properties of FeSbO4 Ceramics.

FeSbO4 powder was prepared using the solid-state reaction method in this work. Afterward, the dense and porous ceramics were obtained by sintering the pressed powder calcined at temperatures of 900 and 1000 °C for 4 h. Rietveld profile analysis of the X-ray powder diffraction data showed that FeSbO4 adopts the trirutile-type structure (space group P42/mnm, with a ≅ 4.63 Å and c ≅ 9.23 Å). SEM images showed that the powder calcined at 900 °C after being sintered at 1200 °C resulted in ceramics of higher crystallinity, larger grains, and consequently, low porosity. The dielectric properties were measured in the frequency range of 10−1 Hz−1 MHz as a function of temperature (25−250 °C). The real (σ') and imaginary (σ″) parts of the complex conductivity increase with rising annealing temperature for both samples. The real conductivity in the AC region for 𝑓 = 100 kHz was 1.59×10−6 S·cm−1 and 7.04×10−7 S·cm−1 for the ceramic samples obtained from the powder calcined at 900 (C-900) and 1000 °C (C-1000), respectively. Furthermore, the dielectric constants (k') measured at room temperature and f=100 kHz were 13.77 (C-900) and 6.27 (C-1000), while the activation energies of the grain region were Ea = 0.53 eV and Ea = 0.49 eV, respectively. Similar activation energy (Ea = 0.52 eV and 0.49 eV) was also obtained by the brick-layer model and confirmed by the adjustment of activation energy by DC measurements which indicated an absence of the porosity influence on the parameter. Additionally, loss factor values were obtained to be equal to 3.8 (C-900) and 5.99 (C-1000) for measurements performed at 100 Hz, suggesting a contribution of the conductivity originated from the combination or accommodation of the pores in the grain boundary region. Our results prove that the microstructural factors that play a critical role in the electrical and dielectric properties are the average grain size and the porosity interspersed with the grain boundary region.

Experimental and Theoretical Studies on Optical Properties of Tetra(Imidazole) of Palladium (II) Phthalocyanine.

In this work, the optical properties of tetra(imidazole) of palladium phthalocyanine (PdPc(Im)4) in solution form and thin films on glass and fluorine-doped tin oxide (FTO) substrates were investigated via the thermal evaporation technique. The optical band gap was evaluated by ultraviolet-visible spectroscopy (UV-Vis). The energy band gap values were determined based on the Tauc graph. In addition, time-dependent density functional theory (TD-DFT) was used to simulate the UV-Vis absorption spectrum of the (PdPc(Im)4) molecule in the Dimethyl Sulfoxide (DMSO) solution phase. A good correlation was found between the DFT results and the experimental optical results. The band gap values between the experimental and DFT-simulated values are presented. The energy band gap of (PdPc(Im)4) obtained from the DFT calculations showed that it can be efficiently regulated. Frontier molecular orbitals and molecular electrostatic potentials were also proposed in this work. The surface study of the layers deposited on FTO was considered by atomic force microscopy (AFM) and scanning electron microscopy (SEM), and the results demonstrated good homogeneity covering the entire surface. The SEM image showed a homogeneous distribution of the grains with some spherical or rod-shaped structures and no agglomeration structures. This work rendered a strategy for regulating the energy band gap and compared the experimental observations obtained with theoretical studies, which provides a fundamental insight into the optical band for optoelectronic and thin-film solar cells.

Head-to-Tail and Head-to-Head Molecular Chains of Poly(p-Anisidine): Combined Experimental and Theoretical Evaluation.

Poly(p-anisidine) (PPA) is a polyaniline derivative presenting a methoxy (-OCH3) group at the para position of the phenyl ring. Considering the important role of conjugated polymers in novel technological applications, a systematic, combined experimental and theoretical investigation was performed to obtain more insight into the crystallization process of PPA. Conventional oxidative polymerization of p-anisidine monomer was based on a central composite rotational design (CCRD). The effects of the concentration of the monomer, ammonium persulfate (APS), and HCl on the percentage of crystallinity were considered. Several experimental techniques such as X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), multifractal analysis, Nuclear Magnetic Resonance (13C NMR), Fourier-transform Infrared spectroscopy (FTIR), and complex impedance spectroscopy analysis, in addition to Density Functional Theory (DFT), were employed to perform a systematic investigation of PPA. The experimental treatments resulted in different crystal structures with a percentage of crystallinity ranging from (29.2 ± 0.6)% (PPA1HT) to (55.1 ± 0.2)% (PPA16HT-HH). A broad halo in the PPA16HT-HH pattern from 2θ = 10.0-30.0° suggested a reduced crystallinity. Needle and globular-particle morphologies were observed in both samples; the needle morphology might have been related to the crystalline contribution. A multifractal analysis showed that the PPA surface became more complex when the crystallinity was reduced. The proposed molecular structures of PPA were supported by the high-resolution 13C NMR results, allowing us to access the percentage of head-to-tail (HT) and head-to-head (HH) molecular structures. When comparing the calculated and experimental FTIR spectra, the most pronounced changes were observed in ν(C-H), ν(N-H), ν(C-O), and ν(C-N-C) due to the influence of counterions on the polymer backbone as well as the different mechanisms of polymerization. Finally, a significant difference in the electrical conductivity was observed in the range of 1.00 × 10-9 S.cm-1 and 3.90 × 10-14 S.cm-1, respectively, for PPA1HT and PPA16HT-HH.

Encapsulation of Bromelain in Combined Sodium Alginate and Amino Acid Carriers: Experimental Design of Simplex-Centroid Mixtures for Digestibility Evaluation.

Bromelain has potential as an analgesic, an anti-inflammatory, and in cancer treatments. Despite its therapeutic effects, this protein undergoes denaturation when administered orally. Microencapsulation processes have shown potential in protein protection and as controlled release systems. Thus, this paper aimed to develop encapsulating systems using sodium alginate as a carrier material and positively charged amino acids as stabilizing agents for the controlled release of bromelain in in vitro tests. The systems were produced from the experimental design of centroid simplex mixtures. Characterizations were performed by FTIR showing that bromelain was encapsulated in all systems. XRD analyses showed that the systems are semi-crystalline solids and through SEM analysis the morphology of the formed systems followed a pattern of rough microparticles. The application of statistical analysis showed that the systems presented behavior that can be evaluated by quadratic and special cubic models, with a p-value < 0.05. The interaction between amino acids and bromelain/alginate was evaluated, and free bromelain showed a reduction of 74.0% in protein content and 23.6% in enzymatic activity at the end of gastric digestion. Furthermore, a reduction of 91.6% of protein content and 65.9% of enzymatic activity was observed at the end of intestinal digestion. The Lis system showed better interaction due to the increased stability of bromelain in terms of the amount of proteins (above 63% until the end of the intestinal phase) and the enzymatic activity of 89.3%. Thus, this study proposes the development of pH-controlled release systems aiming at increasing the stability and bioavailability of bromelain in intestinal systems.

A review of cardiac troponin I detection by surface enhanced Raman spectroscopy: Under the spotlight of point-of-care testing.

Cardiac troponin I (cTnI) is a biomarker widely related to acute myocardial infarction (AMI), one of the leading causes of death around the world. Point-of-care testing (POCT) of cTnI not only demands a short turnaround time for its detection but the highest accuracy levels to set expeditious and adequate clinical decisions. The analytical technique Surface-enhanced Raman spectroscopy (SERS) possesses several properties that tailor to the POCT format, such as its flexibility to couple with rapid assay platforms like microfluidics and paper-based immunoassays. Here, we analyze the strategies used for the detection of cTnI by SERS considering POCT requirements. From the detection ranges reported in the reviewed literature, we suggest the diseases other than AMI that could be diagnosed with this technique. For this, a section with information about cardiac and non-cardiac diseases with cTnI release, including their release kinetics or cut-off values are presented. Likewise, POCT features, the use of SERS as a POCT technique, and the biochemistry of cTnI are discussed. The information provided in this review allowed the identification of strengths and lacks of the available SERS-based point-of-care tests for cTnI and the disclosing of requirements for future assays design.