Sorptive thin film microextraction followed by direct solid state spectrofluorimetry: A simple,rapid and sensitive method for determination of carvedilol in human plasma

A poly acrylate-ethylene glycol (PA-EG) thin film is introduced for the first time as a novel polar sorbent for sorptive extraction method coupled directly to solid-state spectrofluorimetry without the necessity of a desorption step. The structure, polarity, fluorescence property and extraction performance of the developed thin film were investigated systematically. Carvedilol was used as the model analyte to evaluate the proposed method. The entire procedure involved one-step extraction of carvedilol from plasma using PA-EG thin film sorptive phase without protein precipitation. Extraction variables were studied in order to establish the best experimental conditions. Optimum extraction conditions were the followings: stirring speed of 1000 rpm, pH of 6.8, extraction temperature of 60 °C, and extraction time of 60 min. Under optimal conditions, extraction of carvedilol was carried out in spiked human plasma; and the linear range of calibration curve was 15–300 ng mL⁻¹ with regression coefficient of 0.998. Limit of detection (LOD) for the method was 4.5 ng mL⁻¹. The intra- and inter-day accuracy and precision of the proposed method were evaluated in plasma sample spiked with three concentration levels of carvedilol; yielding a recovery of 91–112% and relative standard deviation of less than 8%, respectively. The established procedure was successfully applied for quantification of carvedilol in plasma sample of a volunteer patient. The developed PA-EG thin film sorptive phase followed by solid-state spectrofluorimetric method provides a simple, rapid and sensitive approach for the analysis of carvedilol in human plasma.     

Numerical analysis of the internal flow and the mixing chamber length effects on the liquid film thickness exiting from the effervescent atomizer

Journal of Thermal Analysis and Calorimetry - Two-phase flow was simulated within the effervescent atomizer by the volume of fluid interface tracing model. Different gas-to-liquid mass ratios...     

Effect of the thermal treatment conditions on the formation of zinc ferrite nanocomposite, ZnFe2O4, by sol–gel method

Zinc ferrite nanocomposite was synthesized via thermal decomposition of zinc acetate and iron nitrate at three different temperatures (350, 450, and 550 °C). The influence of the thermal decomposition of precursors on the formation zinc ferrites was studied by differential thermal gravimetry and thermogravimetry (TG). The TG curve shows two steps for the thermal decomposition with mass loss of 17.3 % at 78 °C and 63.3 % at 315 °C. The prepared zinc ferrites nanocomposite was characterized by X-ray diffraction and scanning electron microscopy. The X-ray diffractograms of ZnFe₂O₄ shows that a crystalline phase, spinel system is formed. SEM micrograph of the zinc ferrite nanocomposite indicates the formation of uniformly spherical 48-nm nanograins. The properties of the zinc ferrite phase were strongly dependent on their calcinations temperature and molar ratio of precursors.     

Synthesis and application of a novel solid-phase microextraction adsorbent: Hollow fiber supported carbon nanotube reinforced sol–gel for determination of phenobarbital

A novel solid-phase microextraction technique using a hollow fiber-supported sol–gel combined with multi-walled carbon nanotubes was employed in the determination of phenobarbital in wastewater. In this new technique, a silica-based, organic–inorganic polymer containing functionalized multi-walled carbon nanotubes (MWCNTs) was prepared with sol–gel technology via the reaction of tetraethylorthosilicate (TEOS) with an acidic catalyst (HCl). This sol was injected into a polypropylene hollow fiber segment for in situ gelation. This device operated in direct immersion sampling mode. The experimental setup is simple and affordable, and the device is disposable, so there is no risk of cross-contamination or carry-over. Parameters affecting extraction such as pH of the aqueous solution, ageing and extraction times, aqueous sample volume, agitation speed and carbon nanotube amount were optimized. Linearity was observed over a range of 0.50–5000 ng mL⁻¹, with an estimation coefficient (r²) higher than 0.982. The limit of detection (LOD) was 0.32 ng mL⁻¹ (n = 5), and repeatability (RSD% = 2.9) was from the average of three levels of analyte concentrations (1, 1000 and 4500 ng mL⁻¹) with three replicates for each within a single day. Finally, a pre-concentration factor of 2100 was obtained for phenobarbital.     

Theoretical investigation of the weak interactions of rare gas atoms with silver clusters by resonance Raman spectroscopy modeling

The interactions of rare gas atoms (Rg = Ar, Kr, and Xe) with small neutral and cationic silver clusters have been investigated by density functional methods and the effect of these weak interactions on the resonance Raman spectra of the complexes has been evaluated. The resonance Raman technique that depends on the properties of ground and excited state, seems deeply sensitive to the weak rare gas–metal cluster interactions, and the use of inert gases has been proven to be an excellent approach to recognize the ability of this technique to detect extremely weak interactions. In this work, for , and complexes the IR, normal and resonance Raman spectra have been calculated and the effect of rare gas–cluster stretching vibration ( ) on the pattern and the relative intensities of different spectra have been investigated. The resonance Raman spectra for the weakly interacted complexes (with the interaction energies less than ?2.0 kcal/mol) exhibit the vibration with the detectable intensity that its intensity increases by going from Ag₆–Ar to Ag₆–Xe complex. Moreover, the resonance Raman spectra (based on the excited state gradient approximation) for high intensity nearly degenerate excited states, proved the effect of accumulation of the excited state charge density on the relative intensity of vibration.     

Acid-induced gelation behavior of sonicated casein solutions

Casein gels were made from solutions sonicated by 24 and 130 kHz ultrasounds for 0, 60 and 120 min, followed by acidification with glucono-δ-lactone at 30 °C. The dynamics of gel formation were studied using rheological methods and microstructure of gels was monitored using scanning electron microscopy. Sonication postponed the gelation point to a lower pH value and increased the elasticity of freshly formed gels. It also resulted in gels with a more interconnected structure and smaller non-distinguishable particulates. This structure was especially dominant for the gel made from the solution already sonicated for 120 min.