Simultaneous determination of cloramphenicol, salicylic acid and resorcinol by capillary zone electrophoresis and its application to pharmaceutical dosage forms

This study demonstrates the separation of active ingredients in acne formulations (salicylic acid, cloramphenicol and resorcinol in presence of azulene) by capillary zone electrophoresis. Factors affecting their separations were the buffer pH and concentration, applied voltage, sample preparation, and presence of additives. Optimun results were obtained with a 50 mM sodium tetraborate-50 mM sodium phosphate, pH 9.0. The carrier electrolyte gave baseline separation with good resolution, short migration times (<6 min), great reproducibility and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, the lower limits of detection being within the range 0.39-1.25 μg ml⁻¹. The procedure was fast and reliable and commercial pharmaceuticals could be analysed without prior sample clean-up procedure.     

Hydroformylation: a versatile tool for the synthesis of new β-formyl-metalloporphyrins

Formyl derivatives of protoporphyrin-IX dimethyl ester metal complexes were obtained via hydroformylation reactions, catalysed by rhodium-triphenylphosphine complexes. The regioselectivity of the reaction is remarkably dependent on the metal centre of the porphyrin, yielding 100% of the branched aldehyde with zinc(II) complexes and 75% with the nickel(II). The NMR characterisation of the new compounds was carried out after their derivatisation into acetals.     

Comparison of Several Calibration Procedures for Glass Electrodes in Proton Concentration

Several reported procedures for calibrating glass electrodes in proton concentration are compared. Some recommendations for non-experts are also given. The examined procedures can be classified into two broad categories, namely: those based on direct potential difference measurements of solutions of known proton concentration and those that use one or several pH standards to calibrate the electrode and subsequently measure the pH of solutions containing known proton concentrations. With a single buffer, the two types of procedures lead to equivalent results. However, if two pH buffers are used, the slope of the calibration graph in proton concentration will differ from the real electrode slope to an extent proportional to the difference between the liquid junction potentials of the two buffers. Therefore, any other method is preferable under these circumstances.     

Gravitational collapse of a charged and radiating fluid ball in the diffusion limit

The collapse of a charged and radiating ball in the diffusion limit is studied using a method reported by Herrera and collaborators. The interior solution is matched with the exterior Reissner-Nordström-Vaidya metric to obtain a system of differential equations at the surface of the distribution, which can be integrated numerically for some set of initial data. For one model, the profiles of the physical variables are obtained at any piece of the material in terms of Schwarzschild-like coordinates.     

Mathematical problem solving: an evolving research and practice domain

Research programs in mathematical problem solving have evolved with the development and availability of computational tools. I review and discuss research programs that have influenced and shaped the development of mathematical education in Mexico and elsewhere. An overarching principle that distinguishes the problem solving approach to develop and learn mathematics is to conceptualize the discipline as a set of dilemmas or problems that need to be explored and solved in terms of mathematical resources and strategies. In this context, relevant questions that help structure and organize this paper include: What does it mean to learn mathematics in terms of problem solving? To what extent do research programs in problem solving orient curricular proposals? What types of instructional scenarios promote the students’ development of mathematical thinking based on problem solving? What type of reasoning do students develop as a result of using distinct computational tools in mathematical problem solving?     

Perfect fluid spacetimes admitting curvature collineations

Some basic concepts about curvature collineations are reviewed and the existing results on this topic are applied to the case of perfect fluids, giving a characterization of those amongst them which admit proper curvature collineations.     

Large-scale production of cellulose-binding domains. Adsorption studies using CBD-FITC conjugates

A method for the gram-scale production of cellulose-binding domains (CBD) through the proteolytic digestion of a commercial enzymatic preparation (Celluclast) was developed. The CBD obtained, isolated from Trichoderma reesei cellobiohydrolase I, is highly pure and heavily glycosylated. The purified peptide has a molecular weight of 8.43 kDa, comprising the binding module, a part of the linker, and about 30% glycosidic moiety. Its properties may thus be different from recombinant ones expressed in bacteria. CBD-fluorescein isothiocyanate conjugates were used to study the CBD-cellulose interaction. The presence of fluorescent peptides adsorbed on crystalline and amorphous cellulose fibers suggests that amorphous regions have a higher concentration of binding sites. The adsorption is reversible, but desorption is a very slow process.     

Synthesis of poly(vinyl chloride)‐b‐poly(n‐butyl acrylate)‐b‐poly(vinyl chloride) by the competitive single‐electron‐transfer/degenerative‐chain‐transfer‐mediated living radical polymerization in water

The synthesis of a block copolymer poly(vinyl chloride)‐b‐poly(n‐butyl acrylate)‐b‐poly(vinyl chloride) is reported. This new material was synthesized by single‐electron‐transfer/degenerative‐chain‐transfer‐mediated living radical polymerization (SET‐DTLRP) in two steps. First, a bifunctional macroinitiator of α,ω‐di(iodo)poly (butyl acrylate) [α,ω‐di(iodo)PBA] was synthesized by SET‐DTLRP in water at 25 °C. The macroinitiator was further reinitiated by SET‐DTLRP, leading to the formation of the desired product. This ABA block copolymer was synthesized with high initiator efficiency. The kinetics of the copolymerization reaction was studied for two PBA macroinitiators with number–average molecular weight of 10 k and 20 k. The relationship between the conversion and the number–average molecular weight was found to be linear. The dynamic mechanical thermal analysis suggests just one phase, indicating that copolymer behaves as a single material with no phase separation. This methodology provides the access to several block copolymers and other complex architectures that result from combinations of thermoplastics (PVC) and elastomers (PBA). From industrial standpoint, this process is attractive, because of easy experimental setup and the environmental friendly reaction medium. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 3001–3008, 2006     

Single electron transfer–degenerative chain transfer living radical polymerization of N‐butyl acrylate catalyzed by Na2S2O4 in water media

Living radical polymerization of n‐butyl acrylate was achieved by single electron transfer/degenerative‐chain transfer mediated living radical polymerization in water catalyzed by sodium dithionate. The plots of number–average molecular weight versus conversion and ln[M]₀/[M] versus time are linear, indicating a controlled polymerization. This methodology leads to the preparation of α,ω‐di(iodo) poly (butyl acrylate) (α,ω‐di(iodo)PBA) macroinitiators. The influence of polymerization degree ([monomer]/[initiator]), amount of catalyst, concentration of suspending agents and temperature were studied. The molecular weight distributions were determined using a combination of three detectors (TriSEC): right‐angle light scattering (RALLS), a differential viscometer (DV), and refractive index (RI). The methodology studied in this work represents a possible route to prepare well‐tailored macromolecules made of butyl acrylate in an environmental friendly reaction medium. Moreover, such materials can be subsequently functionalized leading to the formation of different block copolymers of composition ABA. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2809–2825, 2006     

Efficient Synthesis of Nitroflavones by Cyclodehydrogenation of 2′-Hydroxychalcones and by the Baker-Venkataraman Method

Summary. Several nitroflavone derivatives were synthesized by cyclodehydrogenation of 2′-hydroxychalcones and by the Baker-Venkataraman approach, starting from 2′-hydroxyacetophenones and benzoic acid derivatives. Nitroflavones synthesised by the first synthetic approach were obtained in better global yields than those obtained by the later method. The structures of all new compounds were elucidated by microanalyses, 1D and 2D NMR, IR, and mass spectroscopic measurements.