ABSTRACT
OBJECTIVES: This in vitro study evaluated the effect of different colouring solutions and primer systems used in the bonding of brackets on enamel colour change and bond strength. MATERIALS AND METHODS: 120 premolar teeth were divided into four main groups; brackets were bonded with 37% orthophosphoric acid + Transbond XT Primer in Group 1, 3 M Single Bond Universal in Group 2, Transbond Plus SEP in Group 3, and G-Premio Bond in Group 4. Each group was divided into three subgroups, and the teeth were placed in a cup containing coffee and tea mixture, in a cup containing cola and in distilled water. A bond strength test was applied to all teeth. Colour measurements of all teeth were performed at 2 different times: before bonding and after the bond strength test. RESULTS: The average bond strength of the 37% orthophosphoric acid group was higher than that of the other groups. The effect of primer and solution groups on colour change was statistically significant (p = 0.001 and p = 0.023, respectively). CONCLUSIONS: In this study, the bond strength was clinically sufficient in all primer groups. The highest colour change was observed when the tea-coffee solution and Transbond Plus SEP primer were used. CLINICAL RELEVANCE: This study has identified enamel discoloration and bond strength from different colouring solutions and primer systems used for bonding braces, which can be used to inform clinicians and patients to achieve better treatment results.
Subject(s)
Bicuspid , Bisphenol A-Glycidyl Methacrylate , Dental Bonding , Orthodontic Brackets , Resin Cements , Shear Strength , Humans , Dental Bonding/methods , In Vitro Techniques , Resin Cements/chemistry , Color , Coloring Agents , Materials Testing , Dental Enamel/chemistry , Dental Stress Analysis , Phosphoric Acids/chemistry , Surface Properties , Tea/chemistry , Acid Etching, DentalABSTRACT
Iron is routinely supplemented in broiler feeds aiming to prevent dietary deficiencies. Limestone and phosphates are very rich in Fe; however, its contribution from these sources have not been thoroughly investigated with chickens. The present research was conducted to evaluate live performance and blood parameters of broilers when using limestone and dicalcium phosphate as sources of Fe. A total of 576 one-day-old male Cobb x Cobb 500 were allocated into a total of 72 battery cages, 6 treatments with 12 replication cages of 8 chicks at placement. Chicks were fed diets formulated with corn, soybean meal (SBM) with laboratory grade calcium carbonate and phosphoric acid (having traces of Fe). All chicks were fed a common prestarter without Fe supplementation (analyzed total 58.2 ± 2.4 mg/kg Fe) from placement to 7 d. Allocation of birds to dietary treatments was completely randomized on day 8. Treatments had increasing Fe derived from commercial limestone and dicalcium phosphate (analyzed Fe 7,218 and 4,783 mg/kg, respectively) progressively replacing calcium carbonate and phosphoric acid to provide graded increases in total Fe (analyzed Fe in the feeds were 57.6 ± 2.1, 92.0 ± 2.3, 124.1 ± 2.7, 159.3 ± 3.1, 187.2 ± 3.2, 223.7 ± 3.6 mg/kg, respectively). There were no effects of dietary Fe on live performance, hematocrit, and hemoglobin the end of the study on day 28 (P > 0.05). Increasing dietary Fe from commercial limestone and dicalcium phosphate led to a linear reduction in the percent ileal digestible Fe. However, linear increments in Fe retention, serum ferritin and liver Fe occurred when compared to feeds without Fe derived from limestone and phosphate dicalcium. It is concluded that Fe from limestone and dicalcium phosphate can be partially utilized by broiler chickens. It was estimated that the Fe retained from limestone and dicalcium phosphate is of 1.9%. Broilers fed corn-soy feeds (58.2 mg/kg Fe) do not require supplemental Fe.
Subject(s)
Calcium Carbonate , Calcium Phosphates , Chickens , Phosphoric Acids , Animals , Male , Iron , Diet/veterinary , Dietary Supplements , Phosphates , Animal Feed/analysis , Animal Nutritional Physiological Phenomena , DigestionABSTRACT
Nucleoside monophosphates (NMPs) are the subunits of RNA. They are incorporated into growing complementary strands when sequences are copied in enzyme-free reactions using organic leaving groups at the phosphates. Amino acids are rarely considered as leaving groups, but proline can act as a leaving group when N-linked to NMPs, so that prolinyl NMPs hydrolyze in aqueous buffer at 37 °C, with half-life times as short as 2.4â h, and they act as monomers in enzyme-free primer extension. Still, their level of reactivity is insufficient for practical purposes, requiring months for some extensions. Herein we report the synthesis of eight substituted prolinyl AMPs together with seven related compounds and the results of a study of their reactivity. A δ-carboxy prolinyl NMP was found to be converted with a half-life time of just 11â min in magnesium-free buffer, and a δ-isopropyl prolinyl NMP was shown to react sevenfold faster than its prolinyl counterpart in enzyme-free genetic copying of RNA. Our results indicate that both anchimeric and steric effects can be employed to increase the reactivity of aminoacidyl nucleotides, i.e. compounds that combine two fundamental classes of biomolecules in one functional entity.
Subject(s)
Amides , Nucleotides , Amides/chemistry , Phosphoric Acids/chemistry , RNA/chemistryABSTRACT
Vegetable oils-based pressure sensitive adhesives (PSAs) are green and sustainable but face unsatisfactory adhesion strengths and are prone to aging during storage and application due to the existence of residual double bonds and massive ester bonds. Nine common antioxidants (tea polyphenol palmitate (TPP), caffeic acid, ferulic acid, gallic acid, butylated hydroxytoluene, tertiary butylhydroquinone, butylated hydroxyanisole, propyl gallate, and tea polyphenols) were grafted into epoxidized soybean oils-PSA (ESO-PSA) system to enhance antiaging properties and adhesion strengths. Results showed ESO-PSAs grafted with caffeic acid, tertiary butylhydroquinone, butylated hydroxyanisole, propyl gallate, tea polyphenols, or TPP didn't occur failure with TPP having best performance. The optimal conditions were ESO reacted with 0.9 % TPP, 70 % rosin ester, and 7.0 % phosphoric acid at 50 °C for 5 min, under which peel strength and loop tack increased to 2.460 N/cm and 1.66 N, respectively, but peel strength residue reduced to 138.09 %, compared with control (0.407 N/cm, 0.43 N, and 1669.99 %). Differential scanning calorimetry and thermogravimetric results showed TPP grafting increased the glass transition temperature of ESO-PSA slightly but improved its thermal stability significantly. Fourier transform infrared spectroscopy and 1H nuclear magnetic resonance results showed TPP, phosphoric acid, and rosin ester all partially participated in the covalently crosslinking polymerization of ESO-PSAs and the rest existed in the network structures in the free form.
Subject(s)
Butylated Hydroxyanisole , Caffeic Acids , Phosphoric Acids , Soybean Oil , Humans , Male , Soybean Oil/chemistry , Butylated Hydroxyanisole/analysis , Propyl Gallate , Polyphenols , Adhesives/chemistry , Prostate-Specific Antigen , Esters , TeaABSTRACT
A flame retardant (FR) hexachlorocyclotriphosphazene diethylenetriamine ammonium phosphoric acid (HDAPA) was synthesized. Vertical flammability test and limiting oxygen index (LOI) results showed that cotton samples finished with HDAPA solutions (15 % and 20 %) could pass vertical flame retardancy test, and LOIs reached 30.1 % and 35.4 % even after 50 laundering cycles according to AATCC 61-2013 3A washing standard (3A), performing flame retardancy and washing durability. Meanwhile, Fourier transform infrared and X-ray photoelectron spectroscopy analyses suggested that HDAPA was grafted on cotton fibers through -P(=O)-O-C covalent bond. Total heat release (1.98 MJ/m2) and char residue (16.2 %) of HDAPA treated cotton were much lower than those (4.26 MJ/m2, 3.2 %) of untreated cotton. Thermogravimetry results showed HDAPA changed thermal decomposition pathway of cotton fabric, which was further supported by thermogravimetric-Fourier infrared spectrometer results, revealing HDAPA performed a condensed phase flame retardancy mechanism. Scanning electron microscopy implied HDAPA entered amorphous region of cotton fibers to react with cellulose. Mechanical properties of HDAPA treated cotton decreased a little. Although the synthesis process used formaldehyde but no free formaldehyde released. In consequence, the aforementioned results indicated that the introduction of -N=P-(N)3- and -P(=O)(O-NH4+)2 groups to FR was an viable method to improve flame retardancy and durability.
Subject(s)
Ammonium Compounds , Flame Retardants , Phosphoric Acids , Phosphorus , Flame Retardants/analysis , FormaldehydeABSTRACT
Phosphorus fluoride exchange (PFEx) is a catalytic click reaction that involves exchanging high oxidation state P-F bonds with alcohol and amine nucleophiles, reliably yielding P-O- and P-N-linked compounds. Here, we describe steps for preparing a phosphoramidic difluoride and performing two sequential PFEx reactions to yield a phosphoramidate through careful catalyst selection. We then detail procedures for handling and quenching potentially toxic P-F-containing compounds to ensure user safety when conducting PFEx reactions. For complete details on the use and execution of this protocol, please refer to Sun et al.1.
Subject(s)
Amides , Click Chemistry , Fluorides , Phosphoric Acids , PhosphorusABSTRACT
Two kinds of polyaniline coupled graphitized carbon nitride nanosheets doped with different organic phosphoric acids (CP@PA, with phytic acid; CP@NP, with amino trimethyl phosphonic acid) are developed by in-situ polymerization. According to the analysis of the section morphology and element distribution of epoxy resin (EP) composites, although CP@PA and CP@NP show completely different morphology, they can significantly enhance the dispersion of graphitized carbon nitride nanosheets in EP. Moreover, the different oxidation states of phosphorus contained in the CP@PA and CP@NP lead to varying effects on the fire safety of EP. The flame retardancy Index (FRI) is a dimensionless index to evaluate the performance of flame retardants. When used as a flame retardant, CP@NP (FRI = 3.22) is better than CP@PA (FRI = 1.29) in flame retardant, especially in suppressing thermal hazards. As a synergist of intumescent flame retardants (IFR), CP@PA (FRI = 26.12) is most effective in improving the comprehensive fire safety property of EP and achieves an "Excellent" rating. Therefore, two different flame-retardant mechanisms of CP@PA and CP@NP are summarized by analyzing the combustion behavior and changes of condensed phase. In summary, this research may be helpful to the design of nano synergies for IFR systems.
Subject(s)
Flame Retardants , Epoxy Resins , Amino Acids , Aniline Compounds , Phosphoric Acids , PhosphorusABSTRACT
Soil amendment products, such as biochar, with both sustained nutrient release and heavy metal retention properties are of great need in agricultural and environmental industries. Herein, we successfully prepared a new biochar material with multinutrient sustained-release characteristics and chromium removal potential derived from distiller grain by wet-process phosphoric acid (WPPA) modification without washing. SEM, TEM TG-IR, in situ DRIFTS and XRD characterization indicated that biochar and polyphosphate formed simultaneously and were tightly intertwined by one-step pyrolysis. The optimal product (PKBC-400) had the most stable carbon structure and an adequate P-O-P structure with less P loss. Batch experiments illustrated that 92.83% P (ortho-P), 85.94% K, 41.49% Fe, 78.42% Al and 65.60% Mg were continuously released in water from PKBC-400 within 63 days, and the maximum Cr removal rate reached 83.57% (50 mg/L K2Cr2O7, pH=3.0) with an increased BET surface area (304.0557 m2/g) after nutrient release. SEM, IC and 31P NMR analyses revealed that the dissolution and hydrolysis of polyphosphates not only realized the sustained release of multiple nutrients but also significantly improved the sustained release performance. The proposed resource utilization strategy provided new ideas for Cr hazard control, biomass waste utilization and fertilizer development.
Subject(s)
Metals, Heavy , Water Pollutants, Chemical , Adsorption , Carbon , Charcoal/chemistry , Chromium/chemistry , Delayed-Action Preparations , Fertilizers , Nutrients , Phosphoric Acids , Polyphosphates , Soil , Water , Water Pollutants, Chemical/chemistryABSTRACT
In the phosphorous-sulphur two-step process for the clean production of phosphoric acid, a phosphate-rock acid-insoluble residue (PAIR) is a solid filter residue obtained via the phosphoric acid acidolysis of phosphate rock (PR). PAIR combined with other raw materials can be used to prepare cement, ceramics and glasses, opening a potential avenue for large-scale PAIR utilisation. However, the preparation of such materials requires high-temperatures calcination. Understanding the high-temperature thermal properties of PAIR can enable its more targeted comprehensive utilisation or disposal. In this study, the thermal properties and pyrolysis kinetics of PAIR were systematically studied using a multiple heating rate method based on thermogravimetric analysis and a kinetic model. Results showed that from room temperature to 1200 °C, the main changes in the PAIR were the complete removal of fluorine and sulphur, partial removal of phosphorus and conversion of quartz to cristobalite. Moreover, during these processes, H2O(g), NH3, N2, CO2, SO2, P2O5(g), CO, CF3+ and organic gases were volatilised. Herein, the pyrolysis kinetics of PAIR is divided into five stages. Stage 1 (conversion rate É: 0.05-0.2) conforms to the random nucleation and growth as well as the Avrami-Erofeev (n = 2/3) mechanism; the corresponding mechanism function is F(É) = [-Ln(1 - É)]2/3. Stage 2 (É: 0.2-0.4) conforms to the first-order chemical reaction mechanism; the corresponding mechanism function is F(É) = -Ln(1 - É). Stage 3 (É: 0.4-0.6) conforms to the phase boundary-controlled reaction and one-dimensional movement mechanism; the corresponding mechanism function is F(É) = É. Stage 4 (É: 0.6-0.8) conforms to the three-dimensional diffusion process (Jander model); the corresponding mechanism function is F(É) = [1 - (1 - É)1/3]2. Stage 5 (É: 0.6-0.95) conforms to the one-dimensional diffusion process; the corresponding mechanism function is F(É) = É2.
Subject(s)
Phosphates , Pyrolysis , Kinetics , Phosphates/chemistry , Phosphoric Acids , Phosphorus , Solubility , Sulfur , ThermogravimetryABSTRACT
2'-O-Methyl (2'-OMe) antisense oligonucleotides (AOs) possessing a various number of 4-(trimethylammonio)butylsulfonyl or tosyl phosphoramidates (N+ and Ts-modifications, respectively) instead of a native phosphodiester linkage were designed to skip exon-23 in dystrophin pre-mRNA transcript in mdx mice myotubes. AOs bearing several zwitterionic N+ modifications in the sequence had remarkably increased thermal stability towards complementary mRNA in comparison with 2'-OMe-RNAs having negatively charged Ts and phosphorothioate (PS) linkages. However, only Ts-modified AOs exhibited a similar level of exon skipping in comparison with fully modified PS-containing 2'-OMe-RNA, whereas the exon skipping induced by N+ modified AOs was much lower with no exon-skipping detected for AOs having seven N+ modifications. The level of exon-skipping was improved once Ts and especially N+ moieties were used in combination with PS-modification, most likely through improved cellular and nuclear uptake of AOs. These results provide new insights on expanding the design of novel chemically modified AOs based on phosphate modifications.
Subject(s)
Muscle Fibers, Skeletal , Oligonucleotides, Antisense , Amides , Animals , Exons/genetics , Mice , Mice, Inbred mdx , Oligonucleotides, Antisense/genetics , Phosphates , Phosphoric Acids , Phosphorothioate Oligonucleotides , RNAABSTRACT
In this study, the surface of the spent coffee grounds (SCG) was activated using phosphoric acid to increase the removal efficiency of methylene blue (MB) in aqueous solution, which is one of the harmful substances emitted in industrial processes. According to Fourier transform infra-red analysis, after phosphorylation of the SCG (PSCG), P = O group, P-O-C (aromatic) bond, P = OOH and P-O-P were newly introduced on the surface of the adsorbent, and the peaks of carboxyl groups and OH-group were large and broad. In addition, the surface area and mesopore range of the PSCG adsorbent were increased, and the structure changed, which enabled easy adsorption of MB. The process of adsorbing MB from aqueous solution using PSCG was more suitable for the pseudo-second order and Langmuir models, and the adsorption process was closer to chemisorption than physical adsorption. The maximum adsorption capacity of PSCG was 188.68 mg/g. As a result of the reuse test, PSCG showed excellent performance with a high removal efficiency of 90% up to four consecutive uses. PSCG modified with phosphoric acid, an abundant lignocellulose-based biosorbent that is readily available everywhere, is a promising adsorbent capable of adsorbing MB in aqueous solution.
Subject(s)
Methylene Blue , Water Pollutants, Chemical , Adsorption , Coffee/chemistry , Hydrogen-Ion Concentration , Kinetics , Methylene Blue/chemistry , Phosphoric Acids , Water Pollutants, Chemical/chemistryABSTRACT
Phosphoric acid is used in the refining of palm oil for the removal of phosphatides. The high concentration of phosphorus in solvent extracted palm-pressed mesocarp fiber oil hinders palm oil mills to recover this phytonutrients-rich residual oil in pressed fiber which typically contains 0.1 to 0.2% of total oil yield. This study aimed to refine the palm-pressed mesocarp fiber oil and determine the optimum dosage of phosphoric acid for acid-degumming of palm-pressed mesocarp fiber oil while retaining its phytonutrients. The refining process was carried out with combination of wet degumming, acid degumming, neutralisation, bleaching and deodorization. The optimum dose of phosphoric acid was identified as 0.05 wt.% by incorporating the wet degumming process. The refined palm-pressed mesocarp fiber oil showed a reduction in phosphorus content by 97% (from 901 ppm to 20 ppm) and 97% free fatty acid content removal (from 6.36% to 0.17%), while the Deterioration of Bleachability Index increased from 1.76 to 2.48, which showed an increment of 41%. The refined oil retained the key phytonutrients such as carotenoids (1,150 ppm) and vitamin E (1,540 ppm) that can be further developed into high-value products. The oil meets the quality specification of refined, bleached, and deodorized palm oil while preserving the heat-sensitive phytonutrients, which in turn provides a new resource of nutritious oil.
Subject(s)
Food Handling/methods , Liquid-Liquid Extraction/methods , Palm Oil/chemistry , Phospholipids/isolation & purification , Phosphorus/isolation & purification , Phytochemicals/analysis , Carotenoids/analysis , Food Quality , Palm Oil/analysis , Phospholipids/analysis , Phosphoric Acids/chemistry , Phosphorus/analysis , Solvents , Vitamin E/analysisABSTRACT
La adhesión a dentina con sistemas adhesivos polimé-ricos representa un desafío que surge de la necesi-dad de vincular un sustrato dentario heterogéneo y variable con materiales que presentan todavía cier-tos aspectos a atender para poder conseguir el máxi-mo desempeño. El propósito del presente artículo es evaluar algunas de las estrategias propuestas para mejorar la adhesión a dentina, y sugerir un protocolo de trabajo con los diferentes tipos de sistemas adhesivos (AU)
Dentin bonding with polymeric adhesive systems represents a challenge that arises from the need to link a heterogeneous and variable dental substrate with materials that still have certain aspects to be addressed in order to achieve maximum performance. The aim of this article is to evaluate some of the proposed strategies to improve dentin bonding and to suggest a protocol for each different type of bonding systems (AU)
Subject(s)
Clinical Protocols , Dentin-Bonding Agents/therapeutic use , Dentin/drug effects , Phosphoric Acids/chemistry , Acid Etching, Dental/methods , Smear Layer , Composite Resins/chemistry , Dental Enamel/drug effects , PolymerizationABSTRACT
The excellent adhesion of mussels under wet conditions has inspired the development of numerous catechol-based wet adhesives. Nevertheless, the performance of catechol-based wet adhesive suffers from the sensitivity toward temperature, pH, or oxidation stimuli. Therefore, it is of great significance to develop non-catechol-based wet adhesives to fully recapitulate nature's dynamic function. Herein, a novel type of non-catechol-based wet adhesive is reported, which is readily formed by self-assembly of commercially available branched polyethylenimine and phosphotungstic acid in aqueous solution through the combination of electrostatic interaction and hydrogen bonding. This wet adhesive shows reversible, tunable, and strong adhesion on diverse substrates and further exhibits high efficacy in promoting biological wound healing. During the healing of the wound, the as-prepared wet adhesive also possesses inherent antimicrobial properties, thus avoiding inflammations and infections due to microorganism accumulation.
Subject(s)
Adhesives/therapeutic use , Anti-Bacterial Agents/therapeutic use , Hemostatics/therapeutic use , Phosphoric Acids/therapeutic use , Polyethyleneimine/therapeutic use , Staphylococcal Skin Infections/drug therapy , Tungsten Compounds/therapeutic use , Adhesiveness , Adhesives/chemistry , Animals , Anti-Bacterial Agents/chemistry , Escherichia coli/drug effects , Hemostatics/chemistry , Hydrogen Bonding , Mice , Phosphoric Acids/chemistry , Polyethyleneimine/chemistry , Staphylococcus aureus/drug effects , Static Electricity , Tungsten Compounds/chemistry , Water/chemistry , Wound Healing/drug effectsABSTRACT
This work reports the synthesis and characterization by Fourier transform infrared spectroscopy (FTIR), 1H, 13C, and 79Se nuclear magnetic resonance (NMR), mass spectrometry, and elemental analysis techniques as well as the in vitro evaluation of the leishmanicidal activity of 13 new selenophosphoramidate derivatives. Among the new compounds, four of them (compounds 1f, 1g, 2f, and 2g), which exhibited the best profiles, were tested against infected macrophages and were selected for further studies related to their leishmanicidal mechanism. In this regard, trypanothione redox system alteration was determined. Compound 1g, under similar conditions, was more effective than the corresponding references. In addition, theoretical calculations showed that this compound also presents most physicochemical and pharmacokinetic properties within the ranges expected for orally available drugs. It is believed that selenophosphoramidate functionalities may represent a scaffold to be explored toward the development of new agents for leishmania treatment.
Subject(s)
Antiprotozoal Agents , Leishmania , Pharmaceutical Preparations , Selenium , Amides , Antiprotozoal Agents/pharmacology , Antiprotozoal Agents/therapeutic use , Phosphoric Acids , Selenium/pharmacologyABSTRACT
The tea shrub is grown in long-standing orchards, an environment that is suitable for persistent weed growth, which is increasingly controlled by herbicides. Therefore, there is increasing concern that tea consumers may be exposed to herbicide residues. In this study, the levels of glufosinate-ammonium (GLU), glyphosate [N-(phosphonomethyl) glycine; PMG], and its metabolite aminomethyl phosphoric acid (AMPA) were determined in tea samples by HPLC-MS/MS using several current purification methods and a new method that we developed herein. The matrix effect of our proposed method was between -27.3 and 27.7%, which was lower than that in other methods, indicating that this method effectively reduced the interference of tea matrix in the mass spectrometry process. This method was used to determine the levels of PMG, GLU, and AMPA in 780 samples, including six traditional Chinese teas (green tea, black tea, oolong tea, dark tea, white tea, and yellow tea) and a floral tea, from 14 provinces of China. Probability estimates showed that the 95th percentile risk entropy values of the three pesticide residues were far below the acceptable risk level. The risk assessment results showed that exposure to PMG, GLU, and AMPA caused by drinking tea beverages poses no significant risk to human health.
Subject(s)
Herbicides , Tandem Mass Spectrometry , Aminobutyrates , China , Chromatography, High Pressure Liquid , Glycine/analogs & derivatives , Herbicides/analysis , Humans , Phosphoric Acids , Risk Assessment , Tea , GlyphosateABSTRACT
Natural anthocyanin dyes are safe for human and the environment due to their biocompatibility and rapid biodegradability. In this paper, an aqueous anthocyanin extract from grapes was used as a colouring reagent for the determination of humic acid (a cancer-promoting agent) in water and caffeine/phosphoric acid-containing caramelized soft drink. Three techniques, viz: chromametry, ultraviolet-visible spectrophotometry (UV-Vis) and Fourier transform infrared spectroscopy (FTIR) were employed for comparative quantifications. The results showed that the chromametry technique exhibited better sensing performance than the spectroscopic techniques in terms of the limit of detection (LOD) and % recovery. However, both chromametry and UV-Vis techniques agreed that the presence of HA could easily be detected in the soft drink at a spiked concentration of 6.4 ppm where less interference occurred.
Subject(s)
Carbonated Beverages/analysis , Humic Substances/analysis , Plant Extracts/chemistry , Spectrophotometry, Ultraviolet , Spectroscopy, Fourier Transform Infrared , Vitis/chemistry , Caffeine/analysis , Humans , Limit of Detection , Phosphoric Acids/analysis , Vitis/metabolism , Water/chemistryABSTRACT
Research advances in electropolishing, with respect to the field of metalworking, have afforded significant improvements in the surface roughness and conductivity properties of aluminum polished surfaces in ways that machine polishing and simple chemical polishing cannot. The effects of a deep eutectic medium as an acid-free electrolyte were tested to determine the potential energy thresholds during electropolishing treatments based upon temperature, experiment duration, current, and voltage. Using voltammetry and chronoamperometry tests during electropolishing to supplement representative recordings via atomic force microscopy (AFM), surface morphology comparisons were performed regarding the electropolishing efficiency of phosphoric acid and acid-free ionic liquid treatments for aluminum. This eco-friendly solution produced polished surfaces superior to those surfaces treated with industry standard acid electrochemistry treatments of 1 M phosphoric acid. The roughness average of the as-received sample became 6.11 times smoother, improving from 159 nm to 26 nm when electropolished with the deep eutectic solvent. This result was accompanied by a mass loss of 0.039 g and a 7.2 µm change in step height along the edge of the electropolishing interface, whereas the acid treatment resulted in a slight improvement in surface roughness, becoming 1.63 times smoother with an average post-electropolishing roughness of 97.7 nm, yielding a mass loss of 0.0458 g and a step height of 8.1 µm.
Subject(s)
Aluminum/chemistry , Electrochemistry/methods , Electrolytes/chemistry , Electric Conductivity , Ionic Liquids/chemistry , Materials Testing/methods , Microscopy, Atomic Force/methods , Phosphoric Acids/chemistry , Solvents/chemistry , Surface Properties , TemperatureABSTRACT
The NS5B RNA-dependent RNA polymerase of the hepatitis C virus (HCV) is a validated target for nucleoside antiviral drug therapy. We endeavored to synthesize and test a series of 4'-thionucleosides with a monophosphate prodrug moiety for their antiviral activity against HCV and other related viruses in the Flaviviridae family. Nucleoside analogs were prepared via the stereoselective Vorbrüggen glycosylation of various nucleobases with per-acetylated 2-C-methyl-4-thio-d-ribose built in a 10-step synthetic sequence from the corresponding ribonolactone. Conjugation of the thionucleoside to a ProTide phosphoramidate allowed for evaluation of the prodrugs in the cellular HCV replicon assay with anti-HCV activities ranging from single-digit micromolar (µM) to >200 µM. The diminished anti-HCV potency of our best compound compared to its 4'-oxo congener is the subject of ongoing research in our lab and is proposed to stem from changes in sugar geometry imparted by the larger sulfur atom.
Subject(s)
Antiviral Agents/chemical synthesis , Antiviral Agents/pharmacology , Prodrugs/chemical synthesis , Thionucleosides/chemistry , Amides/chemistry , Cell Line , Drug Evaluation, Preclinical , Hepacivirus/drug effects , Hepatitis C/drug therapy , Humans , Nucleosides/chemical synthesis , Phosphates/chemistry , Phosphoric Acids/chemistry , Prodrugs/pharmacology , Viral Nonstructural Proteins/antagonists & inhibitorsABSTRACT
With the growing environmental concerns and an emergent demand, a growing attention is turned to eco-friendly superabsorbent hydrogels instead of synthetic counterparts. Hydrogels based on cellulose derivatives can absorb and retain a huge amount of water in the interstitial sites of their structures, stimulating their uses in various useful industrial purposes. In this work, cross-linked superabsorbent composite hydrogel films (CHF) were designed, manufactured and characterized, by taking advantage of the combination of carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC) and newly developed regenerated cellulose (RC) spheres. RC with sphere-like shape was successfully prepared using a green method based on cold phosphoric acid-mediated dissolution of microcrystalline cellulose (MCC) followed by regeneration process using water as anti-solvent. Prior to be used, the morphological and structural properties of RC spheres, with an average diameter of 477 ± 270 nm, were examined by SEM, AFM, XRD, FTIR and TGA techniques. CHF crosslinked with citric acid were, in fact, prepared by solvent casting method with different RC weight fractions (i.e. 0, 2.5, 5, 10 and 15 wt%), then the crosslinking reaction was triggered by thermal treatment at 80 °C during 8 h. Prepared CHF were then characterized in terms of their structural, thermal, tensile and transparency properties. Swelling tests were carried at three different aqueous media (i.e. with a pH = 3, 6.4 or 11) to evaluate the water retention capacity of hydrogel films, as well as, the pH effect on their swelling and hydrolytic degradation properties. Collected results reveal that CHF with low RC content (i.e. RC weight fraction of 2.5 or 5 wt%) have the best tensile and swelling properties, with a tensile strength and a swelling capacity (at pH = 6.4) up to 95 MPa and 4000%, respectively.