Effects of different cold plasma treatments on chemical composition, phenolics bioaccessibility and microbiota of edible red mini-roses.

This study evaluated the effect of dielectric barrier discharge (DBD) and glow discharge (glow) cold plasma treatments in color, sugars, organic acids, phenolics (concentration and bioaccessibility), antioxidant activity, volatiles, and microbiota of edible mini-roses. Plasma treatments did not affect the flowers' color, while they increased organic acids and phenolics. Flowers treated with DBD had a higher concentration of most phenolics, including hesperidin (84.04 µg/g) related to antioxidant activity, and a higher mass fraction of most volatiles, including octanal (16.46% after 5 days of storage). Flowers treated with glow had a higher concentration of pelargonidin 3,5-diglucoside (392.73 µg/g), greater bioaccessibility of some phenolics and higher antioxidant activity. Plasma treatments reduced the microbiota diversity in mini-roses. Regardless of the plasma treatment, phylum Proteobacteria, family Erwiniaceae, and genus Rosenbergiella were the dominant groups. Results indicate plasma treatments as promising technologies to improve the quality and increase phenolic and specific volatile compounds in mini-roses.

Enhancing Titanium Disk Performance through In-Pack Cold Atmospheric Plasma Treatment.

While titanium dental implants have already been clinically established, ongoing research is continuously being conducted to advance the fields of osseointegration and bacterial resistance, seeking further improvements in these areas. In this study, we introduce an innovative method for treating titanium surfaces within tightly sealed packaging. Specifically, titanium discs, enclosed in surgical-grade packaging, underwent treatment using cold atmospheric plasma (CAP). The surfaces were thoroughly characterized in terms of wettability, crystalline structure, and chemical composition. Hemocompatibility analyses were conducted using blood diluted in sodium citrate (1:9) exposed to titanium discs for 30 min inside a CO2 incubator at 37 °C. Subsequently, various blood parameters were evaluated, including prothrombin time (PT), activated partial thromboplastin time (APTT), and platelet adhesion. Microbiological analyses were also performed using Pseudomonas aeruginosa (ATCC 27853) for 4 h at 37 °C. The treatment with CAP Jet resulted in a reduction in contact angle without causing any changes in the crystalline structure. No statistically significant differences were observed in the blood parameters. The plasma-treated samples exhibited lower PT and APTT values compared to those of the control group. The surfaces treated with CAP Jet showed increased platelet activation, platelet density, and thrombus formation when compared with the untreated samples. Moreover, the treated surfaces demonstrated lower bacterial colony formation compared with other surfaces.

Comparative analysis of the biocompatibility of endothelial cells on surfaces treated by thermal plasma and cold atmospheric plasma.

In recent years, cold atmospheric plasma (CAP) is used for surface disinfection. However, little is known about its ability to improve biocompatibility of metallic surfaces when compared to thermal plasma methods. In this context, the study aimed to evaluate the response of human endothelial cells (Ea.hy926) on titanium surfaces treated by non-thermal plasma method and thermal plasma method under nitriding atmosphere. The wettability was characterized by the sessile drop method, the topography and roughness were evaluated by atomic force microscopy (AFM), and the microstructure by grazing angle X-ray diffraction (GIXRD). Endothelial cells were cultured and evaluated for morphology by scanning electron microscopy and viability by an MTT (3-[4,5-dimethylthiazol-2-yl]-2,5 diphenyl tetrazolium bromide) assay. CAP treatment reduced the contact angle of the Ti surface (13.43° ± 1.48; p<0.05), increasing hydrophilicity. Rz roughness was higher on the nitrided surface (220.44±20.30; p< 0.001) compared to the CAP treated surfaces (83.29 ± 11.61; p< 0.001) and polished (75.98 ±34.21a); p<0.001). The different applied plasma treatments created different titanium surfaces improving the biocompatibility of endothelial cells, however CAP results demonstrate its potential for biomedical applications, considering the low cost and ease of use of the technique, allowing surface treatments before clinical procedures.

Effect of the pH on the Antibacterial Potential and Cytotoxicity of Different Plasma-Activated Liquids.

In this study, different plasma-activated liquids were evaluated for their antimicrobial effects against Escherichia coli, as well as for their cytotoxicity on mammalian cells. The PALs were prepared from distilled (DIS), deionized (DI), filtered (FIL), and tap (TAP) water. Additionally, 0.9% NaCl saline solution (SAL) was plasma-activated. These PALs were prepared using 5 L/min air gliding arc plasma jet for up to 60.0 min of exposure. Subsequently, the physicochemical properties, such as, the oxidation-reduction potential (ORP), the pH, the conductivity, and the total dissolved solids (TDS) were characterized by a water multiparameter. The PALs obtained showed a drastic decrease in the pH with increasing plasma exposure time, in contrast, the conductivity and TDS increased. In a general trend, the UV-vis analyses identified a higher production of the following reactive species of nitrogen and oxygen (RONS), HNO2, H2O2, NO3-, and NO2-. Except for the plasma-activated filtered water (PAW-FIL), where there was a change in the position of NO2- and NO3- at some pHs, The higher production of HNO2 and H2O2-reactive species was observed at a low pH. Finally, the standardized suspensions of Escherichia coli were exposed to PAL for up to 60.0 min. The plasma-activated deionized water (PAW-DI pH 2.5), plasma-activated distilled water (PAW-DIS pH 2.5 and 3), and plasma-activated tap water (PAW-TAP 3.5) showed the best antimicrobial effects at exposure times of 3.0, 10.0, and 30.0 min, respectively. The MTT analysis demonstrated low toxicity of all of the PAL samples. Our results indicate that the plasma activation of different liquids using the gliding arc system can generate specific physicochemical conditions that produce excellent antibacterial effects for E. coli with a safe application, thus bringing future contributions to creating new antimicrobial protocols.

Corn starch based films treated by dielectric barrier discharge plasma.

Cold plasma is an innovative strategy to strengthen the polysaccharide-based films characteristics. This study evaluated the effects of dielectric barrier discharge (DBD) plasma on the hydrophilic character, water vapor permeability (WVP), and tensile properties of corn starch-based films. Starch films were exposed to plasma processing operating at an excitation frequency of 200 Hz for 10, 15, and 20 min. DBD plasma resulted in further enhanced tensile strength and stiffness, and lower hydrophilicity and water solubility; however, it did not present significant effects on the WVP of the resulting films within the ranges studied. Higher hydrophobicity, strength, and stiffness were verified after 20 min. The results presented in this work suggest that the DBD plasma has the potential to make starch-based films a more suitable packaging material.

Dielectric barrier atmospheric cold plasma applied to the modification of Ariá (Goeppertia allouia) starch: Effect of plasma generation voltage.

The goal of this paper was to evaluate the influence of a range of plasma generation voltages on the physicochemical, structural, and technological properties of Aria (Goeppertia allouia) starch. Untreated (0 kV) and high voltages of cold plasma generation (7, 10, 14, and 20 kV) treated samples were evaluated according to their amylose content, pH, groups carbonyl/carboxyl, molecular size distribution, structure and technological properties (empirical viscosity, hydration properties, thermal analysis and gel strength). The applied voltage of 14 kV resulted in the greatest depolymerization of the starch chains, while 20 kV allowed the formation of oxidized complexes, promoting crosslinking of the starches chain. The cold plasma technique did not affect the levels of resistant starches, but increased the starch digestibility. The increased carbonyl and carboxyl groups also influenced the paste viscosity, improved hydration properties. This study suggests that the cold plasma technique can be useful in the controlled modification of starches, producing starches with different technological properties.

Effect of a plasma synthesized polypyrrole coverage on polylactic acid/hydroxyapatite scaffolds for bone tissue engineering.

Composite biomaterials are solids that contain two or more different materials, combining the properties of their components to restore or improve the function of tissues. In this study, we report the generation of electrospun matrices with osteoconductive properties and porosity using the combination of a biodegradable polyester, polylactic acid (PLA), and hydroxyapatite (HA). Additionally, we report the effects of modifying these matrices through plasma polymerization of pyrrole on the growth and osteogenic differentiation of rabbit bone marrow stem cells. Cells were isolated, seeded and cultured on biomaterials for periods between 7 and 28 days. The matrices we obtained were formed by nano and microfibers containing up to 35.7 wt% HA, presenting a variety of apparent pore sizes to allow for the passage of nutrients to bone cells. Scanning electron microscopy showed that the fibers were coated with polypyrrole doped with iodine, and MTT assay demonstrated this increased cell proliferation and significantly improved cell viability due to the adhesive properties of the polymer. Our results show that PLA/HA/Pyrrole/Iodine matrices are favorable for bone tissue engineering.

Multi-element determination in chocolate bars by microwave-induced plasma optical emission spectrometry.

Macro- and microelement determination in chocolate bars by microwave-induced plasma optical emission spectrometry (MIP OES) was evaluated after microwave-assisted sample digestion. Optimization of the sample digestion was carried out, and the recommended conditions were obtained at a temperature of 190 °C, with a digestion time of 40 min and in a mixture constituted by 2.3 mL of nitric acid, 1.0 mL of hydrogen peroxide and 4.7 mL of water. The method was applied in the analysis of chocolate bars, and the concentration ranges of the elements determined were (in mg kg-1): Ca (653-3096); Cr (<0.6-2.8); Cu (<0.16-19.5); Fe (<1.6-227); Mg (147-2775); K (3554-8573); Mn (<0.03-25.2); Na (45.6-1095); Ni (3.2-10.2); P (1111-22594) and Zn (4.8-33.3). The association of the proposed microwave-assisted acid digestion with the MIP OES technique was adequate for multi-element determination in chocolate bars for routine analysis.

Argon Atmospheric Plasma Treatment Promotes Burn Healing by Stimulating Inflammation and Controlling the Redox State.

Burns are a public health problem, with second-degree burns as one of the most common types. Although intense inflammation worsens burn healing, effective therapies are scarce. Thus, infections and hypertrophic scars may occur, which compromise patient quality of life and may delay healing. Argon atmospheric plasma (AP) has been shown to positively influence wound healing. In the context of identifying effective and alternative therapies for the treatment of second-degree burns, the present study evaluated AP in the treatment of second-degree burns in rats compared to that for sham treatment on the 2nd, 7th, 14th, and 21st days post-injury. Our results revealed proinflammatory effect for AP by recruiting predominantly neutrophils on the 7th day and macrophages on the 21st day compared to sham treatment, allowing a greater production of interleukin (IL)-1ß, tumor necrosis factor (TNF)-α, and IL-17, and also controlled the inflammation by IL-10 and transforming growth factor (TGF)-ß1. AP also showed antioxidant activity important for controlling oxidative damage on the 2nd day. This favored the induction of angiogenesis from the 2nd day and induction fibroplasia and fibrillogenesis after the 14th day, which enhanced burn healing with the formation of a thinner burn eschar before the 21st day post-burn. Thus, AP effectively modulated the inflammatory phase of second-degree burn healing through the control of oxidative damage that favored the following phases. Therefore, AP is a relevant alternative in the treatment of second-degree burns.

Effect of different exposure times on physicochemical, mechanical and biological properties of PGS scaffolds treated with plasma of iodine-doped polypyrrole.

Polyglycerol sebacate (PGS) scaffolds obtained using a leaching technique were modified with iodine-doped polypyrrole (PPy-I) in a plasma reactor in order to study the effect of exposure time on the cell viability of hDPSCs. SEM analysis showed the formation and growth of PPy-I particles as the exposure time was increased, while FTIR and XPS analysis revealed the presence of -NH- and N+ groups in the chemical composition of the surfaces, relating to the increase in the amount of PPY-I particles. The water contact angle measurements showed an increase in the scaffold's hydrophilicity with greater exposure times which was also attributed to the rising of PPy-I particles. It was also observed that PPy-I promotes the rigidity of the treated PGS scaffolds. when in direct contact with treated PGS scaffolds, cell viability improved with respect to non-treated scaffolds, however only at shorter time exposures. Extracts of plasma-treated PGS scaffolds showed high cytotoxicity as the time exposure to plasma treatment was increased.

Study of nitrogen implantation in Ti surface using plasma immersion ion implantation & deposition technique as biocompatible substrate for artificial membranes.

The present investigation reports the modification of Ti substrates by a plasma technique to enhance their physio-chemical properties as biocompatible substrates for the deposition of artificial membranes. For that purpose, nitrogen ions are implanted into Ti substrate using the plasma immersion ion implantation & deposition (PIII&D) technique in a capacitively coupled radio frequency plasma. The plasma was characterized using optical emission spectroscopy, together with radio frequency compensated Langmuir probe, while the ion current towards the substrate was measured during the implantation process using an opto-electronic device. X-ray photoelectron spectroscopy (XPS) was used for chemical analysis of the surface, confirming the presence of δ-TiN. The penetration depth of the nitrogen ions into the Ti substrate was measured using secondary ions mass spectroscopy (SIMS) while the morphological changes were observed using atomic force microscopy (AFM). A calorimetric assay was used to prove that the TiN samples maintain the biocompatibility of the untreated Ti surface with its native oxide layer. The ion implantation increases the load bearing ability of Ti surface by the formation of α-Ti(N) and δ-TiN phases on the sub-surface of Ti, and maintains the bio compatibility of Ti surface. After the plasma treatment a thin layer of chitosan (CH) was deposited in order to provide a moisturizing matrix for the artificial membrane of 1,2-dipalmitoyl-sn-3- phosphor glycerocholine (DPPC). The CH and subsequently the DPPC were deposited on the plasma deposited TiN substrate by using physical vapor deposition. The formation of artificial membranes was confirmed by AFM, measuring the topography at different temperatures and performing force curves.

Hollow cathode plasma nitriding of medical grade Ti6Al4V: A comprehensive study.

Ti6Al4V used in biomedical applications still has several surface-related problems, such as poor bone compatibility and low wear resistance. In this work, the formation of a protective layer of titanium nitride obtained by plasma treatment in hollow cathode was studied, and the best experimental conditions were verified by a statistical factorial design of experiments. The samples were characterized in terms of their physical and chemical properties, correlating the effects of time (min) and temperature (°C). An achieved ideal condition was further analysed in terms of in vitro cytotoxicity, micro-abrasion, and electrochemical properties. The carried-out assessment has shown that nitrided condition has an improvement in wettability, microhardness, along with TixNy formation and roughness increment, when compared to pristine condition.

Dielectric barrier atmospheric cold plasma applied on camu-camu juice processing: Effect of the excitation frequency.

The aim of this paper was to evaluate the effect of cold plasma excitation frequency on camu-camu juice processing. Different levels of frequency (200, 420, 583, 698 and 960 Hz) were applied on camu-camu juice to measure the contents of ascorbic acid and anthocyanins, as well as to evaluate the antioxidant compounds (DPPH, ABTS, FRAP and phenolic compounds), peroxidase and polyphenol oxidase enzymatic activity and color. Furthermore, the juice bioaccessibility was evaluated after simulated digestion. The ascorbic acid concentration was increased when higher excitation frequencies were employed, increasing their bioavailability. Anthocyanins, peroxidase and polyphenol oxidase presented considerable degradation with increasing the plasma excitation frequency. For this reason, the juice processing proposed herein represents an alternative to enhance its nutritional quality. Moreover, the use of cold plasma reduced the activity concentration of endogenous enzymes, presenting considerable degradation for higher excitation frequency.

Influence of gelatinization process and HMDSO plasma treatment on the chemical changes and water vapor permeability of corn starch films.

In this study, surface, chemical, physicochemical and barrier properties of films treated with hexamethyldisiloxane (HMDSO) cold plasma were investigated. Normal and high amylose starches were gelatinized at different level to obtain films with different amount of free amylopectin. The obtained films were subjected to HMDSO plasma treatment. XPS analysis indicated chemical changes including substitution and crosslinking of the starch molecule, as reflected by the CSi bond increasing and the C-OH bonds reduction on treated films. These changes modified the thermal transitions (Tm and ΔH). The highest amount of CSi bonds was more noticeable in the TF50 film, suggesting a better interaction between active species of plasma and the free amylopectin released into the continuous phase of the film. Moreover, active species of plasma increased the crystallinity in all films. These results suggested that a higher helical packaging, crosslinking and hydrophobic blocking groups (CSi) of starch molecules resulted in films with improved barrier performance against water molecules.

Effects of cold atmospheric plasma on squid proteases and gel properties of protein concentrate from squid (Argentinus ilex) mantle.

The effect of cold atmospheric plasma (CAP) on protein concentrate from squid (Argentinus ilex) mantle has been evaluated in terms of gel properties, protease inhibition, texture profile, color attributes, and water holding capacity. Different exposure time (15, 60, 120, 180, 240 and 300 s) at 60 kV have been employed. Our results indicated that protease activity decreases with increasing treatment time. The highest reduction (p < 0.05) in protease activity (64%) was observed after 240 s of CAP treatment. Texture profile analysis, color properties and water holding capacity of the treated squid gel revealed a significant increase. Protein carbonyl and sulfhydryl group contents findings' showed a significant increase in carbonyl content (about three times of the original content), while the total sulfhydryl group decreased (up to about 40%) in the crude extract. Microstructure and SDS-PAGE analysis revealed a high degree of protein aggregation in the squid gel treated with CAP.

Micrometric Wrinkled Patterns Spontaneously Formed on Hydrogel Thin Films via Argon Plasma Exposure.

The generation of microstructured patterns on the surface of a specific polymeric material could radically improve their performance in a particular application. Most of the interactions with the environment occur at the material interface; therefore, increasing the exposed active surface considerably improves their range of application. In this article, a simple and reliable protocol to form spontaneous wrinkled patterns using a hydrogel layer is reported. For this purpose, we took advantage of the doctor blade technique in order to generate homogenous films over solid substrates with controlled thickness and large coverage. The hydrogel wrinkle formation involves a prepolymerization step which produces oligomers leading to a solution with increased viscosity, enough for doctor blade deposition. Subsequently, the material was exposed to vacuum and plasma to trigger wrinkled pattern formation. Finally, a UV-polymerization treatment was applied to fix the undulations on top. Interestingly, the experimental parameters allowed us to finely tune the wrinkle characteristics (period, amplitude, and orientation). For this study, two main aspects were explored. The first one is related to the role of the substrate functionalization on the wrinkle formation. The second study correlates the deswelling time and its relationship with the dimensions and distribution of the wrinkle pattern. In the first batch, four different 3-(trimethoxysilyl)propyl methacrylate (TSM) concentrations were used to functionalize the substrate in order to enhance the adhesion between hydrogel film and the substrate. The wrinkles formed were characterized in terms of wrinkle amplitude, wavelength, pattern roughness, and surface Young modulus, by using AFM in imaging and force spectroscopy modes. Moreover, the chemical composition of the hydrogel film cross-section and the effect of the plasma treatment were analyzed with confocal Raman spectroscopy. These results demonstrated that an oxidized layer was formed on top of the hydrogel films due to the exposure to an argon plasma.

Effect of plasma-nitrided titanium surfaces on the differentiation of pre-osteoblastic cells.

A titanium surface nitrided by plasma contains nitrogen ions that guarantee resistance to corrosion and biocompatibility. Despite this, no descriptions concerning the influence of the expression of cell adhesion proteins and their influence on osteogenic cell differentiation are available. Thus, the present study aimed to assess the response of murine pre-osteoblastic cells (MC3T3-E1) cultured on nitrided titanium surfaces. Pre-osteoblastic cells were grown on polished titanium discs, used as controls, and on previously characterized plasma-nitrided titanium discs. Cells from both groups were submitted to the MTT cell viability test. The expressions of α5, α2, and ß1 integrin were assessed by flow cytometry and immunofluorescence, while osteocalcin expression was assessed by flow cytometry. The nitrided surface presented higher α2 and ß1 integrin expressions, as well as osteocalcin expression, when compared to the polished surface, with no alterations in cell viability. These findings seem to suggest that the plasma nitriding treatment produces a titanium surface with the potential for effective in vitro osseointegration.

Hexamethyldisiloxane cold plasma treatment and amylose content determine the structural, barrier and mechanical properties of starch-based films.

In this study, the effect of amylose content and cold plasma treatment on starch films properties was investigated. Films from normal (30%) and high amylose (50 and 70%) starches were subjected to hexamethyldisiloxane (HMDSO) cold plasma treatment. Morphological, structural, mechanical and barrier properties of the films were evaluated. The amount of remnant starch granules (RSG) in the films depended on the amylose content and on the gelatinization extent of the starch. This behavior was corroborated on the films from starch with 50% amylose, where the loss of RSG resulted in poor barrier properties and high hydrophilicity. Moreover, HMDSO cold plasma treatment incorporated methyl groups improving the hydrophobic properties and favored the helix ordering of the starch components resulting in a limited water-film interaction. Furthermore, the simultaneous effect of HMDSO coating and the ordering of the structures reinforced the surface of the films, improving the mechanical properties.

S-incorporated TiO2 coatings grown by plasma electrolytic oxidation for reduction of Cr(VI)-EDTA with sunlight.

The plasma electrolytic oxidation (PEO) technique was used to prepare photocatalytic S-TiO2 coatings on Ti sheets; the incorporation of the S ions was possible from the electrolyte for modifying the structural and optics characteristics of the material. In this work, substrates of Ti (ASME SB-265 of 20 × 20 × 1 mm) were used in a PEO process in 10 min, using constant voltage pulses of 340 V with frequency of 1 kHz and duty cycles of 10% and of 30%. Solutions with H2SO4 (0.1 M) and CH4N2S (52 and 79 mM) were used as electrolytes. X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy (EDS) were utilized to analyze the surface morphology, crystalline phase, and chemical composition of the samples. According to the results, the catalyst coatings had microporous structure and contained anatase-rutile TiO2 nanocrystalline mixture, until 73.2% rutile and 26.8% anatase in the samples grown with 30% duty cycle and the lowest concentration of CH4N2S. From the EDS measurements, the incorporation of sulfur ions to the coatings was 0.08 wt%. 99.5% reduction efficiency of Cr(VI)-EDTA with sunlight was observed after 2 h; it was determined by diphenyl carbazide spectrophotometric method. These coatings have potential for effective sunlight heterogeneous photoreduction of this toxic, cumulative, and non-biodegradable heavy metal that contaminates the soil and water and is a serious risk to sustainability, ecosystems, and human health.