Optimization and validation of a nonaqueous micellar electrokinetic chromatography method for determination of polycyclic musks in perfumes

A nonaqueous micellar electrokinetic chromatography method was developed for determination of Tonalide®, Galaxolide®, and Traseolide® polycyclic musks (PCMs). These compounds are widely used as fragrance ingredients in cosmetics. The method was optimized by using a three variable Box‐Behnken experimental design and response surface methodology. A modified chromatographic response function was defined in order to adequately weigh the terms in the response function. After optimization of experimental conditions, an electrolyte solution of 195 mM SDS and 40 mM NaH₂PO₄ in formamide was selected for the separation of the three PCMs, and the applied voltage was fixed at 30 kV. The nonaqueous MEKC method was then checked in terms of linearity, limits of detection and quantification, repeatability, intermediate precision and accuracy, providing appropriate values (i.e. RSD values for precision never exceeding 7%, and accuracy 96–107%). Nonaqueous MEKC for determination of the selected compounds was successfully applied to the analysis of commercial perfume samples.     

Synthesis of core-shell composites using an inverse surfmer

Anilinium dodecylsulfate was prepared from aniline and sodium dodecylsulfate. The critical micellar concentration of the salt was determined using electrical conductimetry, which revealed that the change of countercation, sodium by anilinium, reduced the critical micellar concentration with respect to the conventional counterpart, sodium dodecylsulfate. The anilinium dodecylsulfate was used as the surfmer in the synthesis of polystyrene/polyaniline core-shell composites, first performing as the surfactant to stabilize the emulsion polymerization of styrene, and later as the monomer to synthesize polyaniline via oxidative polymerization. Here, the surfmer function was directed toward the external phase instead of to the internal phase, as with conventional surfmers with carbon-carbon double bonds. Consequently, the term inverse surfmer is proposed. Analyses of its composite microstructure using electron microscopy and thermogravimetric analysis confirmed the core-shell arrangement.     

A flow-injection biamperometric method for determination of pantoprazole in pharmaceutical tablets

A flow-injection biamperometric method for determination of pantoprazole (PTZ) in pharmaceutical tablets is reported for the first time. The reversible redox couples Fe3+/Fe2+, Fe(CN)6(3-)/Fe(CN)6(4-), Ce4+/Ce3+, VO3(-)NO2+, and I2/I- were tested as indicating redox systems for biamperometric determination of PTZ in a flow-injection assembly with optimized flow parameters. The best results were obtained using V03(-)NO2+, which showed to be a selective and sensitive biamperometric indicating system for PTZ even in the presence of excipients and antioxidants that typically are found in drugs. The analytical graph was linear (r = 0.99945) in the range from 10 to 100 mg/L using 25 mmol/L VO3(-) as the reagent and water as the carrier stream and applying 100 mV between the 2 platinum wire electrodes. The limits of detection and quantitation were 200 and 667 microg/L, respectively, with a sensibility of calibration of 22.6 mV/mg/L. The proposed method was successfully applied to determine PTZ in commercial pharmaceutical tablets with a mean relative error of 1.60% (n = 5) and mean relative standard deviation of 3.10%. Recoveries close to 100% showed good agreement between the expected amount of PTZ in tablets (40 mg) and the results found by the application of the proposed method and demonstrated that the formulations used in the tablet compositions do not interfere in the PTZ analysis. The system had good stability, with a relative standard deviation of 3.80% for 9 sequential injections of a 60 mg/L PTZ solution. A sampling rate of about 100 samples/h was obtained.     

Frontal polymerizations carried out in Deep-Eutectic mixtures providing both the monomers and the polymerization medium

Deep Eutectic Solvents (DESs) based upon mixtures of Acrylic Acid (AA) or Methacrylic Acid (MAA) and Choline Chloride (CCl) demonstrated superior performance than regular organic solvents and even ionic liquids for frontal polymerizations (FPs). Full recovering of CCl after FP provided an interesting green character to the process.     

The SmA phase of a bent-core V-shaped compound: structure and electric-field response

The smectic A (SmA) phase of a V-shaped mesogen with a molecular bending angle of 60° was studied. According to X-ray measurements, the molecules are arranged with the ‘bow-string’ direction parallel to the smectic layer. This point was confirmed by birefringence analysis and the result is compatible with a non-polar structure. A detailed study of the (001) smectic layer reflection versus temperature was also carried out to determine the smectic translational order parameter. The results indicate that the material presents a high degree of translational order. In addition, the electric field response of the material was studied by means of second harmonic generation. This technique turned out to be highly sensitive to small structural distortions due to the V-shape of the constituent molecules.