New extraction method for the analysis of linear alkylbenzene sulfonates in marine organisms. Pressurized liquid extraction versus Soxhlet extraction

A new method has been developed for the determination of linear alkylbenzene sulfonates (LAS) from various marine organisms, and compared with Soxhlet extraction. The technique applied includes the use of pressurized liquid extraction (PLE) for the extraction stage, preconcentration of the samples, purification by solid-phase extraction (SPE) and analysis by liquid chromatography with fluorescence detection. The spiked concentrations were added to the samples (wet mass of the organisms: Solea senegalensis and Ruditapes semidecussatus), which were homogenized and agitated continuously for 25 h. The samples were extracted by pressurized hot solvent extraction using two different extraction temperatures (100 and 150 degrees C) and by traditional Soxhlet extraction. The best recoveries were obtained employing pressurized hot solvent extraction at 100 degrees C and varied in the range from 66.1 to 101.3% with a standard deviation of between 2 and 13. Detection limit was between 5 and 15 microg kg(-1) wet mass using HPLC-fluorescence detection. The analytical method developed in this paper has been applied for LAS determination in samples from a Flow-through exposure system with the objective of measuring the bioconcentration of this surfactant.     

Indirect automatic atomic absorption determination of sulphate based on its precipitation with barium

A continuous precipitation flame atomization atomic absorption spectrometric method for the indirect determination of sulphate is proposed. By using a reversed flow-injection configuration for precipitation as barium sulphate, this anion was determined in the range 10–150 g/ml, with a relative standard deviation of 2.6%. The sensitivity was increased by a factor of seven by using a nitrous oxide-acetylene flame to measure barium.     

Determination of N-nitrosamines by HPTLC with Fluorescence Detection — Use of Non-Ionic Surfactants as Enhancing Agents

JPC – Journal of Planar Chromatography – Modern TLC - The dansyl derivatives of N-nitrosodimethylamine, N-nitrosodi-ethylamine, and N-nitrosodibuthylamine have been separated by HPTLC...     

Development and Validation of a High-Performance Thin-Layer Chromatographic Method,with Densitometry,for Quantitative Analysis of Tizoxanide (a Metabolite of Nitazoxanide) in Human Plasma

JPC – Journal of Planar Chromatography – Modern TLC - A new simple, rapid, and selective high-performance thin-layer chromatographic (HPTLC) method with metronidazole as the internal...     

Defect concentration in Ti-substituted YIG from TG curves

The article discusses theory and experiment about the measurement of defect concentration in Ti-substituted yttrium iron garnet by means of thermogravimetry techniques. The two possible cases arising from oxygen interchange with atmosphere, oxygen vacancies and interstitial cations, may be analyzed quantitatively from the derived expressions. The possibility of another type of defects being present in the samples, not associated to oxygen evolution, is not excluded. Measurements were carried out in air and CO₂ for different Ti contents. The substitution tends to increase slightly the defect parameter θ in YIG, while a CO₂ reducing atmosphere is much more effective than the Ti substitution for increasing θ. Calculations for a given single-phased sample sintered in air show two possibilities: a deficit of one oxygen atom for every 2.5 unit cells of 96 atoms, or one excess cation for every 3.5 cells. Other samples show very similar results. The accuracy involved in the measurements is about 2–3%.     

Dependence of the rate constants on the treatment of internal rotation modes: the reaction OH + CH3SH --> CH3S + H2O as an example

The title reaction has been used as an example to test the importance of using a hindered rotor treatment instead of a harmonic oscillator model for calculating vibrational partition functions corresponding to low-frequency internal rotation modes. First, a normal-mode analysis according to the Ayala and Schlegel's algorithm has been used to identify the internal rotation modes of methanethiol and the transition state structure. Then, after calculation of the energy barrier for each internal rotation, the corresponding hindered rotor partition functions have been calculated following the CW scheme of Chuang and Truhlar. The results show that the anharmonic treatment produces a rather modest improvement of the rate constants at room temperature or below.     

Thermodynamic excess quantities in the adsorption of sodium alkylsulfonates at the air-solution interface

Colloid and Polymer Science - Data on the surface tension of sodium alkylsulfonate solutions at different temperatures and surfactant concentrations are presented. By applying the thermodynamic...     

Neutron activation analysis of final molasses from Cuban sugar industry

Thermal and epithermal non-destructive activation analyses have been performed on samples of final molasses from 14 different sugar factories, covering the most important regions in Cuba. From the first measurement after irradiation at the Triga Mark reactor (VTT), the concentration of more than 15 elements is reported. The almost constant elemental composition shows that they can be used equally for different purposes as animal foodstuff and for the manufacture of biotechnological products. This work is part of a research project developed in order to establish a complete characterization of Cuban sugar molasses.     

Complexation of the Non-steroidal Anti-inflammatory Drug Nabumetone with Modified and Unmodified Cyclodextrins

The inclusion of the anti-inflammatory drug, Nabumetone, in -, - and hydroxypropyl--cyclodextrin (CDs) is studied using UV-VIS absorption and steady-state fluorescence emission. Binding constants and thermodynamic parameters of complex formation are determined by spectrofluorimetry. The inclusion phenomena of Nabumetone with the three cyclodextrins is compared with that of the well known similar anti-inflammatory drug Naproxen. In the case of Nabumetone pronounced differences are observed in the complexation process with each cyclodextrin whereas the respective Naproxen complexes are nearly identical. ¹H-NMR experiments show that the inclusion process in Nabumetone can occur either through the substituents in the -2 (butanone) or -6 (methoxy) positions in the naphthalene ring.     

Single-step preparation and catalytic activity of mesoporous MCM-41 and SBA-15 silicas functionalized with perfluoroalkylsulfonic acid groups analogous to Nafion

Preparation of hybrid organic-inorganic MCM-41 and SBA-15 silicas functionalized with perfluoroalkylsulfonic acid groups has been achieved in a single step by reacting the mesoporous silicas with 1,2,2-trifluoro-2-hydroxy-1-trifluoromethylethane sulfonic acid beta-sultone; the catalysts showed higher activity than commercial Nafion-silica composite for the esterification of long chain fatty acids with ethanol.