Development and validation of an HPLC method for mefloquine hydrochloride determination in tablet dosage form

A simple HPLC method for determination of mefloquine hydrochloride in tablets was developed and validated. The separation was carried out on an Xterra RP18 (250 x 4.6 mm id, 5 pm particle size) analytical column. The mobile phase was 0.05 M monobasic potassium phosphate buffer (pH 3.5)-methanol (40 + 60, v/v). The flow rate and wavelength were set to 1 mL/min and 283 nm, respectively. The method was specific for mefloquine hydrochloride in the presence of hydrolytic, oxidative, and photolytic degradation products. It was also linear, precise, accurate, and robust, being suitable for routine QC analyses and stability studies. The developed HPLC method was compared to a previously described spectrophotometric method.     

Study of layered and defective amorphous solids by means of thermal wave method

In this work the thermal properties and the thickness calibration in layered thick acrylic films using the thermal wave method are reported. The results from acrylic films on two different substrates showed that thermal diffusivity and conductivity can be measured for both supports, metallic and glassy. The experimental applicability of a 1-D model and accuracy of the thickness measurement are also discussed.     

SERS and Raman imaging as a new tool to monitor dyeing on textile fibres

Textile fibres containing Ag nanoparticles have been widely explored for a number of antimicrobial fabrics. Moreover, it is well‐known that textile dyeing is a critical stage in the manufacture thereof. This research shows that surface enhanced Raman scattering (SERS) and Raman imaging can be used with advantage in the monitoring of this process. Using Ag containing linen fibres stained with methylene blue (MB), it was possible to map the local distribution of the MB dye in the fibres by Raman imaging. MB was selected as the SERS molecular probe and as a model dye. Composites of linen fibres and Ag nanoparticles were prepared by distinct methods and used as SERS substrates in order to evaluate the effect of the preparative method on the Raman images. Our results demonstrate that by using Raman imaging associated to the presence of Ag nanoparticles, it is possible to distinguish the local distribution of the dye on the textile surface. This investigation allows to foreseeing the use of this technique in terms of quality control of Ag containing fabrics, which is a market in great expansion. Copyright © 2016 John Wiley & Sons, Ltd.     

Combining stir bar sorptive extraction and MEKC for the determination of polynuclear aromatic hydrocarbons in environmental and biological matrices

In this work, stir bar sorptive extraction and liquid desorption was combined with MEKC and diode-array detection (SBSE-LD-MEKC-DAD) for the determination of polynuclear aromatic hydrocarbons (PAHs) in aqueous medium, using biphenyl, fluorene, anthracene, phenanthrene, fluoranthene and pyrene as model compounds. MEKC-DAD conditions and parameters affecting SBSE-LD efficiency are fully discussed. Assays performed on aqueous samples spiked at trace levels, yielded recoveries ranging from 55.5 +/- 6.1% (pyrene) to 70.7 +/- 7.1% (anthracene), under optimized experimental conditions. The methodology proved to be nearly described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)). The analytical performance showed good precision (<12.0%), suitable detection limits (2-11 microg/L) and convenient linear dynamic ranges (r(2)>0.99) from 5 to 25 microg/L for anthracene and 25 to 125 microg/L for the remaining compounds. The application of the proposed methodology to environmental water, sediments and fish bile matrices demonstrated good selectivity and accuracy. SBSE-LD combined with MEKC-DAD was shown to be an easy, reliable and robustness methodology, as well as a good analytical alternative to monitor environmental priority pollutants.     

Stability of triglyceride liquid films on hydrophilic and hydrophobic glasses

Wetting and dewetting of solid surfaces by oily fluids were investigated in terms of the stability of the liquid film formed between an air bubble and the solid surface. With the objective of understanding how molecules with low polarity but relatively complex molecular structure behave at the solid/liquid interface, three liquid triglycerides with different chain length and saturation were chosen, namely, tributyrin, tricaprylin, and triolein. Tributyrin and tricaprylin exist in milkfat while triolein is present in vegetable oils. The stability of the liquid films may be inferred from the shape of the disjoining pressure isotherms, which represent the dependence of the disjoining pressure on the film thickness. Disjoining pressure isotherms for films of the three triglycerides on hydrophilic and hydrophobic glasses were obtained using a recently developed apparatus, based on the interferometric technique. The experimental curves are compared with the theoretical predictions of London-Hamaker. The deviations between theory and experiment are interpreted in terms of a structural component of the disjoining pressure. All triglycerides form metastable films on both hydrophilic and hydrophobic glasses which means that for disjoining pressures higher than a critical value, pi(c), a wetting transition occurs and the film ruptures. The mechanisms for film rupture are discussed and a correlation between film stability and the apolar (Lifshitz-van der Waals) and the polar components of the spreading coefficient is proposed.     

Copper-promoted carbon-nitrogen bond formation with 2-iodo-selenophene and amides

We present here carbon-nitrogen bond formation via a coupling reaction of 2-iodo-selenophene catalyzed by Cu(I) in the presence of a base and an inexpensive ligand, and establish the first route to obtaining 2-nitrogen-selenophene derivatives in good yields. We can anticipate that this reaction works well with oxazolidinones, lactams, and aliphatic and aromatic amides, as nitrogen sources, in the absence of any supplementary additives. In addition, the reaction proceeded cleanly under mild reaction conditions and was sensitive to the ratio of amide/2-iodo-selenophene, as well as the nature of the ligand, base, and solvent.     

Adsorptive micro-extraction techniques--novel analytical tools for trace levels of polar solutes in aqueous media

A novel enrichment technique, adsorptive μ-extraction (AμE), is proposed for trace analysis of polar solutes in aqueous media. The preparation, stability tests and development of the analytical devices using two geometrical configurations, i.e. bar adsorptive μ-extraction (BAμE) and multi-spheres adsorptive μ-extraction (MSAμE) is fully discussed. From the several sorbent materials tested, activated carbons and polystyrene divinylbenzene phases demonstrated the best stability, robustness and to be the most suitable for analytical purposes. The application of both BAμE and MSAμE devices proved remarkable performance for the determination of trace levels of polar solutes and metabolites (e.g. pesticides, disinfection by-products, drugs of abuse and pharmaceuticals) in water matrices and biological fluids. By comparing AμE techniques with stir bar sorptive extraction based on polydimethylsiloxane phase, great effectiveness is attained overcoming the limitations of the latter enrichment approach regarding the more polar solutes. Furthermore, convenient sensitivity and selectivity is reached through AμE techniques, since the great advantage of this new analytical technology is the possibility to choose the most suitable sorbent to each particular type of application. The enrichment techniques proposed are cost-effective, easy to prepare and work-up, demonstrating robustness and to be a remarkable analytical tool for trace analysis of priority solutes in areas of recognized importance such as environment, forensic and other related life sciences.     

Strong-coupling topological Josephson effect in quantum wires

We investigate the Josephson effect for a setup with two lattice quantum wires featuring Majorana zero energy boundary modes at the tunnel junction. In the weak-coupling regime, the exact solution reproduces the perturbative result for the energy containing a contribution ～ ± cos(?/2) relative to the tunneling of paired Majorana fermions. As the tunnel amplitude g grows relative to the hopping amplitude w, the gap between the energy levels gradually diminishes until it closes completely at the critical value gc [Formula: see text]. At this point the Josephson energies have the principal values [Formula: see text], where m =- 1,0,1 and σ =± 1, a result not following from perturbation theory. It represents a transparent regime where three Bogoliubov states merge, leading to additional degeneracies of the topologically nontrivial ground state with an odd number of Majorana fermions at the end of each wire. We also obtain the exact tunnel currents for a fixed parity of the eigenstates. The Josephson current shows the characteristic 4π periodicity expected for a topological Josephson effect. We discuss the additional features of the current associated with a closure of the energy gap between the energy levels.