Thermal analysis characterization of PAAm-<Emphasis Type="Italic">co</Emphasis>-MC hydrogels

This paper reports the thermal characterization of polyacrylamide-co-methylcellulose hydrogels and the constituent monomers (acrylamide and methylcellulose). Polymeric materials can be used to produce hydrogels, which can be natural, synthetic, or a mixture. The hydrogels described here were obtained by free radical polymerization, in the presence of N,N′-methylene-bis-acrylamide as a cross-linker agent. Four acrylamide concentrations were used for the synthesis of hydrogels: 3.6, 7.2, 14.7, and 21.7% (w/v). The materials so obtained were analyzed by TG, DTG, DSC, and FT-IR. The TG curves of acrylamide and methylcellulose showed three mass loss events. In DSC curves, the acrylamide exhibited one melting peak at 84.5 °C, and methylcellulose indicated one exothermic event. Nevertheless, acrylamide was considered more stable than methylcellulose. The TG curves of the hydrogels exhibited three mass loss events, and on the DSC curves, three endothermic events were observed. It was verified that the different acrylamide proportions influenced the thermic behavior of hydrogels, and that the authors considered the 7.2% hydrogel a promising drug carrier system. The absorption bands were well defined, confirming the presence of the functional groups in the samples.     

Synthesis and application of imprinted polyvinylimidazole-silica hybrid copolymer for Pb determination by flow-injection thermospray flame furnace atomic absorption spectrometry

A novel ion imprinted polyvinylimidazole-silica hybrid copolymer (IIHC) was synthesized and used as a selective solid sorbent for Pb²⁺ ions preconcentration using an on-line solid phase extraction (SPE) system coupled to TS-FF-AAS. The ionic hybrid sorbent was prepared using 1-vinylimidazole and 3-(trimethoxysilyl)propylmethacrylate as monomers, Pb²⁺ ions as template, tetraethoxysilane as reticulating agent and 2,2′-azobis-isobutyronitrile as initiator. The best on-line SPE conditions concerning sorption behavior, including sample pH (6.46), buffer concentration (9.0 mmol L⁻¹), eluent (HNO₃) concentration (0.5 mol L⁻¹) and preconcentration flow rate (4.0 mL min⁻¹), were optimized by means of full factorial design and Doehlert matrix. The analytical curve ranged from 2.5 to 65.0 μg L⁻¹ (r = 0.999) with limit of detection of 0.75 μg L⁻¹; the precision (repeatability) calculated as relative standard deviation (n = 10) was 5.0 and 3.6% for Pb²⁺ concentration of 10.0 and 60.0 μg L⁻¹, respectively. From on-line breakthrough curve, column capacity was 3.5 mg g⁻¹. Preconcentration factor (PF), consumptive index (CI) and concentration efficiency (CE) were 128.0, 0.16 mL and 25.6 min⁻¹, respectively. The selective performance of the sorbent, based on relative selectivity coefficient, was compared to NIC (non imprinted copolymer) for the binary mixture Pb²⁺/Cd²⁺, Pb²⁺/Cu²⁺ and Pb²⁺/Zn²⁺. The results showed that ion imprinted polyvinylimidazole-silica hybrid polymer had higher selectivity for Pb²⁺ than NIC at 64.9, 16.0 and 8.8 folds. The developed method was successfully applied for highly sensitive and selective Pb²⁺ determination in different kinds of water samples, parenteral solutions and urine. Accuracy was also assessed by analyzing certified reference fish protein (DORM-3) and marine sediment (MESS-3 and PACS-2) with satisfactory results.     

Biosensor for phenol based on the direct electron transfer blocking of peroxidase immobilising on silica–titanium

Horseradish peroxidase (HRP) was immobilised on silica gel modified with titanium oxide. This material was employed to prepare modified carbon paste electrode. The direct electron transfer of the hydrogen peroxide reduction by HRP was blocked when immobilised on silica–titanium. This biosensor presented a very sensitive response for phenol (1 μmol l⁻¹) at an applied potential of 0 mV vs SCE. The best condition was achieved in phosphate buffer pH 6.8, ratio of hydrogen peroxide/phenol higher than 0.35. The biosensor showed a linear response range between 10 and 50 μmol l⁻¹ of phenol, adjusted by the equation j=−32.8+16.3 [phenol], for n=5 with a correlation coefficient of 0.9995. The response time of the biosensor was about 3 s.     

Radon determination by activated charcoal adsorption and liquid scintillation measurement

A passive diffusion method for the determination of radon concentration has been optimised and calibrated. The device consists of a scintillation vial containing activated charcoal, a diffusion barrier and a desiccant agent. The response to diverse atmospheric humidity and variable exposure intervals was studied. The result is a detector independent of atmospheric humidity till 7 days of exposure. The method was compared with electret detectors (US EPA) with very satisfactory results. The advantages of this method are its simplicity, low cost, low detection limit, the total automatization of the measurement and its total independence of humidity to measure in a wide range of radon concentrations.     

Quercetin-PVP K25 solid dispersions

Quercetin is a flavonoid very well studied and has already entered clinical trials emerging as prospective anticancer drug candidate. In addition, quercetin has being reported to its free-radical scavenging activity and suggests potential uses for the prevention and treatment of pathologies as atherosclerosis, chronic inflammation, and others. However, quercetin is sparingly soluble in water, which may be responsible for its limited absorption upon oral administration. The solid dispersion of quercetin with polyvinylpyrrolidone Kollidon^® 25 (PVP K25) suggests an interesting way to increase quercetin solubility, antioxidant activity, and consequently bioavailability. Then, the purpose of this study was to prepare solid dispersions of quercetin with PVP K25 and evaluate their thermal characterization, antioxidant activity and quercetin improvement solubility. For this purpose, quercetin-PVP K25 solutions were dried and quercetin-PVP K25 solids were obtained. The formation of quercetin-PVP K25 solid dispersion was evaluated by solubility studies, powder X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetry (TG), and antioxidant activity. It was observed that PVP K25 was able to provide quercetin clear aqueous solutions and that quercetin solubility was increased in a PVP K25 concentration dependent manner, improving solubility even 436-fold the pure quercetin. The results obtained with XRD, FT-IR, DSC, and TG demonstrated possible quercetin-PVP K25 solid dispersion formation. Besides, the antioxidant activity of the quercetin-PVP K25 solid dispersions dissolved in aqueous solution and pure quercetin dissolved in methanol showed IC₅₀ value of 0.61 ± 0.03 and 1.00 ± 0.02 μg/mL, respectively, demonstrating that the solid dispersions presented a significant increase in antioxidant activity (P < 0.05). Putting results together, it was possible to conclude there was the formation of quercetin-PVP K25 solid dispersion.