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Molecules (Basel, Switzerland) Mar 2020The recent introduction of compact or low-field (LF) NMR spectrometers that use permanent magnets, giving rise to proton (H) NMR frequencies between 40 and 80 MHz, have...
The recent introduction of compact or low-field (LF) NMR spectrometers that use permanent magnets, giving rise to proton (H) NMR frequencies between 40 and 80 MHz, have opened up new areas of application. The two main limitations of the technique are its insensitivity and poor spectral resolution. However, this study demonstrates that the chemometric treatment of LF H NMR spectral data is suitable for unveiling medicines as adulterants of slimming dietary supplements (DS). To this aim, 66 DS were analyzed with LF H NMR after quick and easy sample preparation. A first PLS-DA model built with the LF H NMR spectra from forty DS belonging to two classes of weight-loss DS (non-adulterated, and sibutramine or phenolphthalein-adulterated) led to the classification of 13 newly purchased test samples as natural, adulterated or borderline. This classification was further refined when the model was made from the same 40 DS now considered as representing three classes of DS (non-adulterated, sibutramine-adulterated, and phenolphthalein-adulterated). The adulterant (sibutramine or phenolphthalein) was correctly predicted as confirmed by the examination of the H NMR spectra. A limitation of the chemometric approach is discussed with the example of two atypical weight-loss DS containing fluoxetine or raspberry ketone.
Topics: Dietary Supplements; Drug Contamination; Proton Magnetic Resonance Spectroscopy
PubMed: 32155779
DOI: 10.3390/molecules25051193 -
Polymers Feb 2020Nowadays, concrete degradation is a major problem in the civil engineering field. Concrete carbonation, one of the main sources of structures' degradation, causes...
Nowadays, concrete degradation is a major problem in the civil engineering field. Concrete carbonation, one of the main sources of structures' degradation, causes concrete's pH to decrease; hence, enabling the necessary conditions for corrosion reinforcement. An accurate, non-destructive sensor able to monitor the pH decrease resistant to concrete conditions is envisaged by many researchers. Optical fibre sensors (OFS) are generally used for concrete applications due to their high sensitivity and resistance to external interferences. Organic-inorganic hybrid (OIH) films, for potential functionalization of OFS to be applied in concrete structures, were developed. Polydimethylsiloxane (PDMS) based sol-gel materials were synthesized by the formation of an amino alcohol precursor followed by hydrolysis and condensation. Different ratios between PDMS and (3-aminopropyl)triethoxysilane (3-APTES) were studied. The synthesized OIH films were characterized by Fourier-transformed infrared spectroscopy (FTIR), UV-Vis spectroscopy, electrochemical impedance spectroscopy (EIS) and thermogravimetric analysis (TGA). The OIH films were doped with phenolphthalein (Phph), a pH indicator, and were characterized by UV-Vis and EIS. FTIR characterization showed that the reaction between both precursors, the hydrolysis and the condensation reactions occurred successfully. UV-Vis characterization confirmed the presence of Phph embedded in the OIH matrices. Dielectric and thermal properties of the materials showed promising properties for application in contact with a high alkaline environment.
PubMed: 32046023
DOI: 10.3390/polym12020371 -
Arquivos Brasileiros de Cirurgia... 2019Renal insufficiency is a disease that affects several organs by provoking hypervolemia and uremia. The disease reaches more than 500 million people worldwide and few...
BACKGROUND
Renal insufficiency is a disease that affects several organs by provoking hypervolemia and uremia. The disease reaches more than 500 million people worldwide and few studies bring their influence on the gastrointestinal tract.
AIM
To evaluate the influence of 5/6 nephrectomy-induced hypervolemia on colonic permeability to water and electrolytes.
METHOD
Sixty male Wistar rats weighing between 280-300 g were divided into three groups: 3, 7 and 14 days after nephrectomy, each one having a false-operated/control and partially nephrectomized. For colonic permeability they were submitted to colonic perfusion with a solution of Tyroad containing phenolphthalein. Differences among the concentrations of Na+, K+ and Cl- were used to calculate the rate of colonic permeability for the electrolytes. Phenolphthalein concentrations were used to evaluate the rate of secretion and water absorption.
RESULTS
The colonic secretion of water and electrolytes occurred expressively in the group seven days after nephrectomy. Hemodynamic and biochemical assessments determined the progression of renal failure in all three groups and polyethylene glycol was shown to be effective in reversing the secretory capacity of the colon.
CONCLUSION
Hypervolemia established after 7 days post-nephrectomy 5/6 caused marked colonic secretion for water and electrolytes. The organism presents progressive colonic secretion as the blood volume increases; on the other hand, polyethylene glycol was able to revert this secretory framework of the colon to water and electrolytes by reversing the hypervolemia.
Topics: Animals; Colon; Kidney Failure, Chronic; Male; Nephrectomy; Permeability; Rats; Rats, Wistar; Water-Electrolyte Imbalance
PubMed: 31859925
DOI: 10.1590/0102-672020190001e1472 -
ACS Omega Dec 2019Polyphosphazene microspheres were fabricated by ultrasonic-assisted precipitation polymerization using 4,4'-(hexafluoroisopropylidene)diphenol, 4,4'-sulfonyldiphenol,...
Polyphosphazene microspheres were fabricated by ultrasonic-assisted precipitation polymerization using 4,4'-(hexafluoroisopropylidene)diphenol, 4,4'-sulfonyldiphenol, 4,4-(9-fluorenylidene)diphenol, and phenolphthalein to obtain poly[4,4'-(hexafluoroisopropylidene)diphenol]phosphazene (PZAF), poly(4,4'- sulfonyldiphenol)phosphazene (PZS), poly[4,4'-(9-fluorenylidene)diphenol]phosphazene, and poly(phenolphthalein)phosphazene (PZPT) and were incorporated into polybenzoxazines (PBa) to obtain corresponding PZAF/PBa, PZS/PBa, fluorenyl polyphosphazene (PZFP)/PBa, and PZPT/PBa composites. Addition of 5 wt % of PZAF, PZS, PZFP, and PZPT microspheres improved the thermal stability and fire retardancy of PBa resin significantly. Notably, addition of PBa with 5% PZAF led to a 62.5% decrease in the peak heat release rate and 49.3% reduction in total heat release. The role of microspheres in the gas-phase flame-retardancy mechanism in the PBa matrix was studied. Dynamic mechanical analysis results demonstrated that the of PBa flame-retardant composites was still around 210 °C compared to 221 °C of pure PBa. Hence, the synthesized PBa composites had potential applications as high flame-retardancy materials.
PubMed: 31815230
DOI: 10.1021/acsomega.9b02752 -
Polymers Oct 2019In order to obtain membranes with both organic separation and adsorption functions, knitted tube composite β-cyclodextrin/chitosan (β-CD/CS) porous membranes were...
In order to obtain membranes with both organic separation and adsorption functions, knitted tube composite β-cyclodextrin/chitosan (β-CD/CS) porous membranes were prepared by the non-solvent induced phase separation (NIPS) method using CS and β-CD as a membrane-forming matrix, glutaraldehyde as crosslinking agent to improve water stability, and knitted tube as reinforcement to enhance the mechanical properties. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), contact angle, water flux, bovine serum albumin (BSA) rejection and tensile test were carried out. The FTIR demonstrated that the β-CD and CS had been successfully crosslinked. With the crosslinking time increased, the membrane structure became denser, the contact angle and the rejection rate increased, while the water flux decreased. The strength and elongation at a break were 236 and 1.7 times higher than these of bare β-CD/CS porous membranes, respectively. The strength of crosslinking membranes increased further. The adsorption performance of composite membranes was investigated for the removal of phenolphthalein (PP) from aqueous solution. The adsorption process followed the Langmuir isotherm model, and the kinetic behavior was accorded with the Double constant equation and the Elovich equation. The adsorption mechanism could be explained by the synergistic effect of host-guest interaction from β-cyclodextrin, non-uniform diffusion and porous network capture.
PubMed: 31652903
DOI: 10.3390/polym11111737 -
Anais Da Academia Brasileira de Ciencias 2019Seed companies are looking for promising, quick and effective alternatives to determine the physiological quality of seeds. The objective of the current work was to...
Seed companies are looking for promising, quick and effective alternatives to determine the physiological quality of seeds. The objective of the current work was to study the efficiency of the exudate - phenolphthalein pH test to evaluate the seeds of two lots of Libidibia ferrea (Mart. ex Tul.) L. P. Queiroz var. ferrea. The statistical design for the the exudate - phenolphthalein pH test was completely randomized with four replicates of 50 seeds in a factorial design (2 x 5), two seed lots and five soaking periods (30, 60, 90, 120, and 150 minutes), respectively, using two constant temperatures (25 and 30°C). The percentage of viability and germination of the seeds did not differ in the temperatures of 25 and 30°C and in the soaking periods by the exudate - phenolphthalein pH test. Thus, it is recommended that the test be conducted for at least 30 minutes in distilled and deionized water at the constant temperature of 25 or 30°C to evaluate the vigor of the Libidibia ferrea.
Topics: Caesalpinia; Germination; Hydrogen-Ion Concentration; Phenolphthalein; Quality Control; Seeds; Temperature
PubMed: 31644643
DOI: 10.1590/0001-3765201920180734 -
RSC Advances Oct 2019Phenolphthalein type polyphosphazene (PZPT) microspheres were synthesized by an ultrasound assisted precipitation polymerization method, and their structures were...
Phenolphthalein type polyphosphazene (PZPT) microspheres were synthesized by an ultrasound assisted precipitation polymerization method, and their structures were confirmed by scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. Benzoxazine/PZPT (Ba/PZPT) hybrid materials were fabricated and cured to prepare polybenzoxazine/PZPT (PBa/PZPT) composites. The effects of PZPT microspheres on the curing kinetics and behaviors of Ba were systematically analyzed and supported by differential scanning calorimetry (DSC) and FTIR. The thermogravimetric (TGA) results demonstrated good thermal stability of the PBa composites incorporating PZPT. The peak of heat release rate and total heat release values of PBa/PZPT-5% composites obviously deceased by 57.8% and 17.3% compared to those of the pristine PBa. Moreover, the smoke released from the PZPT/PBa system significantly reduced with the loading of microspheres. Finally, the dynamical mechanical analysis results demonstrated that the of PBa flame retardant composites was approximately 210 °C, not affecting further applications of PBa composites.
PubMed: 35527950
DOI: 10.1039/c9ra06857k -
International Journal of Analytical... 2019There has been an increasing interest in the search for colour indicators of natural origin for titrimetric analysis. This is due to some challenges associated with the...
There has been an increasing interest in the search for colour indicators of natural origin for titrimetric analysis. This is due to some challenges associated with the currently used synthetic ones. This study evaluates and validates the acid-base indicator property of plumbagin isolated from Linn. Plumbagin (5-hydroxy-2-methyl-1,4-naphthoquinone) was isolated from the roots of Linn using silica gel chromatography and characterized using spectroscopic methods in comparison with those reported in the literature. Its acid-base indicator property was evaluated alongside phenolphthalein and methyl orange, after it was found to exhibit a sharp change in colour at various pH ranges. The plumbagin indicator was successfully used to assay ibuprofen powder and tablets (400 mg) using the British Pharmacopoeia (2013) method. Data obtained were analyzed statistically by Student's -test and one-way ANOVA in GraphPad Prism (version 5.01, 2010). Analysis of the use of the plumbagin indicator in acid-base titrations between strong acids and strong bases and between weak acids and strong bases has been evaluated and validated according to the ICH guidelines. Plumbagin use in ibuprofen powder and tablets has also been verified. Plumbagin has been validated for use as an indicator suitable for different acid-base titrations and the analysis of ibuprofen.
PubMed: 31531024
DOI: 10.1155/2019/4061927 -
ACS Omega Apr 2019Peptides that recognize artificial materials including synthetic polymers and small molecules are drawing attention in the fields of biotechnology and chemical biology....
Peptides that recognize artificial materials including synthetic polymers and small molecules are drawing attention in the fields of biotechnology and chemical biology. In particular, reversible peptide aptamers that associate with the target molecules only under specific conditions are interesting. In this work, peptide aptamers that recognize a phenolphthalein derivative (PhP: a pH-sensitive organic dye) immobilized on a solid surface in a pH-dependent manner were selected using an in vitro display method (cDNA display). Considering the hydrophobic and aromatic nature of PhP, we prepared a biased DNA library (3A library) that encodes more aromatic amino acids than the standard random codon and performed seven rounds of selection from >10 peptide species. The selected peptides including LVFLIWWM (LV59) associated with PhP-modified solid support (sepharose resin and magnetic beads) in neutral buffer but readily dissociated under basic conditions where PhP undergoes large structural change from lactone to quinoid, which is accompanied by increase of hydrophilicity and anionic charge. Control experiments suggested that LV59 recognized both phenol and lactone moieties, and the association under neutral pH is mainly driven by π-stacking and hydrophobic interaction between the peptide and PhP. Notably, however, total hydrophobicity and number of aromatic rings did not completely explain the affinity, and sequence specificity was observed to some extent. After further optimization, this interaction pair would be practically useful for protein purification.
PubMed: 31459836
DOI: 10.1021/acsomega.9b00631 -
ACS Omega Jan 2019β-cyclodextrin (β-CD) forms a host-guest inclusion complex with many organic and amphiphilic compounds found in pharmaceutical, textile, cosmetic, food, and personal...
β-cyclodextrin (β-CD) forms a host-guest inclusion complex with many organic and amphiphilic compounds found in pharmaceutical, textile, cosmetic, food, and personal care systems. Therefore, grafting of β-CD onto a cellulose nanocrystal (CNC) offers a possible strategy to use functionalized CNC to complex with surface-active molecules. We have successfully grafted β-CD onto CNCs in a stepwise manner using cyanuric chloride as the linker. The structure of β-CD-grafted CNC (CNC-CD) was characterized by UV-vis and Fourier-transform infrared spectroscopy, and the grafting ratio of β-CD was determined by the phenolphthalein inclusion protocol. Ionic surfactants induced the aggregation of CNC-CDs by forming inclusion complexes with β-CDs on the surface of CNC. The interactions of amphiphilic compounds with CNC-CD were examined by surface tensiometry, conductometric and potentiometric titration, and isothermal titration calorimetry. Mechanisms describing the complex formation between surfactants and CNC-CD were proposed, where an improved understanding of CD interactions with surfactants and lipids would enable better strategies for drug encapsulation and delivery with CDs.
PubMed: 31459458
DOI: 10.1021/acsomega.8b02534