Determination of three antidepressants in urine using simultaneous derivatization and temperature‐assisted dispersive liquid–liquid microextraction followed by gas chromatography–flame ionization detection

This paper presents a fast and simple method for the extraction, preconcentration and determination of fluvoxamine, nortriptyline and maprotiline in urine using simultaneous derivatization and temperature‐assisted dispersive liquid–liquid microextraction (TA‐DLLME) followed by gas chromatography–flame ionization detection (GC‐FID). An appropriate mixture of dimethylformamide (disperser solvent), 1,1,2,2‐tetrachloroethane (extraction solvent) and acetic anhydride (derivatization agent) was rapidly injected into the heated sample. Then the solution was cooled to room temperature and cloudy solution formed was centrifuged. Finally a portion of the sedimented phase was injected into the GC‐FID. The effect of several factors affecting the performance of the method, including the selection of suitable extraction and disperser solvents and their volumes, volume of derivatization agent, temperature, salt addition, pH and centrifugation time and speed were investigated and optimized. Figures of merit of the proposed method, such as linearity (r² > 0.993), enrichment factors (820–1070), limits of detection (2–4 ng mL^?1) and quantification (8–12 ng mL^?1), and relative standard deviations (3–6%) for both intraday and interday precisions (concentration = 50 ng mL^?1) were satisfactory for determination of the selected antidepressants. Finally the method was successfully applied to determine the target pharmaceuticals in urine. Copyright © 2014 John Wiley & Sons, Ltd.     

Molecular dynamics and alignment studies of silica-filled 4-pentyl-4′-cyanobiphenyl (5CB) liquid crystal

A comprehensive study of the dielectric properties of 4-pentyl-4′-cyanobiphenyl (5CB) liquid crystal filled with silica particles (particle size 30–80 nm, concentration 2, 3, 5, 10 and 15 wt%). Dielectric spectroscopy in the frequency range 100 to 10 7 Hz was applied to investigate the influence of the filler on the dynamic behaviour of the liquid crystal molecules in both the nematic and isotropic phases. In this frequency range one relaxation process is observed (at f>10⁶ Hz). The dynamical behaviour of the 5CB liquid crystal is described by the Cole-Cole relaxation function. The temperature dependence of the relaxation time obeys the empirical Arrhenius equation. The activation energies are approximately 75 kJ mol¹ for the pure 5CB sample in the nematic phase and 50 kJ mol¹ for the 5 wt% silica-filled 5CB sample. These values are compared with the corresponding literature values. The reversible electro-mechanical response of these samples under the influence of an applied a.c. electric field is investigated.     

Flexural strength of silica fume,fly ash,and metakaolin of hardened cement paste after exposure to elevated temperatures

Journal of Thermal Analysis and Calorimetry - The mechanical properties of concrete based mainly on flexural and compressive bearing capacity. Generally, researchers have an interest in the...     

Evaluation of antibacterial and antioxidant activities of Artemisia campestris (Astraceae) and Ziziphus lotus (Rhamnacea)

The present work quantitatively evaluates the antimicrobial and antioxidant potentials of two Libyan folk medicinal plants [Artemisia campestris (Astraceae) and Ziziphus lotus (Rhamnacea)] that commonly grow in the south of Libya. The crude methanolic leaves extracts of both plants are appreciably active against Gram-positive species, associated with week anti-Gram-negative activity. These two plant extracts also showed reasonably high contents of polyphenolics and alkaloids, with minimal inhibitory concentrations between 12.5–25 and 250–1000 μg/ml for Gram-positive and Gram-negative species, respectively. Results collectively suggest that A. campestris and Z. lotus are not only reliable natural sources of antimicrobials but also potential sources of phenolic antioxidants and hence could be nominated for future intensive studies.     

Discontinuous Galerkin method coupled with an integral representation for solving the three-dimensional time-harmonic Maxwell equations

In this paper, we present a mathematical and numerical studies of the three-dimensional time-harmonic Maxwell equations. The problem is solved by a discontinuous Galerkin DG method coupled with an integral representation. This study was completed by some numerical tests to justify the effectiveness of the proposed approach. The numerical simulation was done by an iterative solver implemented in FORTRAN.     

Lot sizing with carbon emission constraints

This paper introduces new environmental constraints, namely carbon emission constraints, in multi-sourcing lot-sizing problems. These constraints aim at limiting the carbon emission per unit of product supplied with different modes. A mode corresponds to the combination of a production facility and a transportation mode and is characterized by its economical costs and its unitary carbon emission. Four types of constraints are proposed and analyzed in the single-item uncapacitated lot-sizing problem. The periodic case is shown to be polynomially solvable, while the cumulative, global and rolling cases are NP-hard. Perspectives to extend this work are discussed.     

Lipase-mediated enantioselective kinetic resolution of racemic acidic drugs in non-standard organic solvents: Direct chiral liquid chromatography monitoring and accurate determination of the enantiomeric excesses

The enantioselective resolution of a set of racemic acidic compounds such as non-steroidal anti-inflammatory drugs (NSAIDs) of the group arylpropionic acid derivatives is demonstrated. Thus, a set of lipases were screened and manipulated in either the esterification or hydrolysis mode for the enantioselective kinetic resolution of these racemates in non-standard organic solvents. The accurate determination of the enantiomeric excesses of both substrate and product during such reaction is demonstrated. This was based on the development of a direct and reliable enantioselective high performance liquid chromatography (HPLC) procedure for the simultaneous baseline separation of both substrate and product in one run without derivatization. This was achieved using the immobilized chiral stationary phase namely Chiralpak IB, a 3,5-dimethylphenylcarbamate derivative of cellulose (the immobilized version of Chiralcel OD) which proved to be versatile for the monitoring of the lipase-catalyzed kinetic resolution of racemates in non-standard organic solvents.