Generalized GIPSCAL re-revisited: a fast convergent algorithm with acceleration by the minimal polynomial extrapolation

Generalized GIPSCAL, like DEDICOM, is a model for the analysis of square asymmetric tables. It is a special case of DEDICOM, but unlike DEDICOM, it ensures the nonnegative definiteness (nnd) of the model matrix, thereby allowing a spatial representation of the asymmetric relationships among ??objects??. A fast convergent algorithm was developed for GIPSCAL with acceleration by the minimal polynomial extrapolation. The proposed algorithm was compared with Trendafilov??s algorithm in computational speed. The basic algorithm has been adapted to various extensions of GIPSCAL, including off-diagonal DEDICOM/GIPSCAL, and three-way GIPSCAL.     

Axiomatizability of positive algebras of binary relations

We consider all positive fragments of Tarski??s representable relation algebras and determine whether the equational and quasiequational theories of these fragments are finitely axiomatizable in first-order logic. We also look at extending the signature with reflexive, transitive closure and the residuals of composition.     

A Bernstein type inequality and moderate deviations for weakly dependent sequences

In this paper we present a Bernstein-type tail inequality for the maximum of partial sums of a weakly dependent sequence of random variables that is not necessarily bounded. The class considered includes geometrically and subgeometrically strongly mixing sequences. The result is then used to derive asymptotic moderate deviation results. Applications are given for classes of Markov chains, iterated Lipschitz models and functions of linear processes with absolutely regular innovations.     

Extending and relating different approaches for solving fuzzy quadratic problems

Quadratic programming problems are applied in an increasing variety of practical fields. As ambiguity and vagueness are natural and ever-present in real-life situations requiring solutions, it makes perfect sense to attempt to address them using fuzzy quadratic programming problems. This work presents two methods used to solve linear problems with uncertainties in the set of constraints, which are extended in order to solve fuzzy quadratic programming problems. Also, a new quadratic parametric method is proposed and it is shown that this proposal contains all optimal solutions obtained by the extended approaches with their satisfaction levels. A few numerical examples are presented to illustrate the proposed method.     

The blow-up of critical anisotropic equations with critical directions

We investigate blow-up theory for doubly critical anisotropic problems in bounded domains of the Euclidean space.     

Multivariate Optimization and Validation of a CZE Method for the Analysis of Pridinol Mesylate and Meloxicam in Tablets

A capillary zone electrophoresis method for the simultaneous determination of pridinol mesylate (PRI) and meloxicam (MEL) employing epinastine hydrochloride and piroxicam as internal standards, was developed and optimized employing experimental design and response surface methodologies. The separation was optimally achieved in less than 2 min at 30 kV in an uncoated fused-silica capillary (41.4 cm × 75 ??m I.D.), employing an 18 mmol L^?1 sodium phosphate buffer solution (pH 5.90) at 25 °C. Samples were injected in hydrodynamic mode (50 mbar, 5 s) and the analytes were spectrophotometrically detected at 200 nm. Method robustness was demonstrated by ANOVA of determinations performed under conditions slightly different from the optimum. The method was validated regarding separation selectivity (peak purity factors > 0.99), linearity and range (PRI = 17.6?C31.4 mg L^?1; MEL = 66.5?C122.5 mg L^?1), accuracy (PRI = 100.2?C101.9%; MEL = 98.9?C100.7%) and precision. The RSD values obtained were ??1.3% for injection repeatability and ??1.9% for intra-day precision. The limits of detection (1.0 and 0.9 mg L^?1) and quantification (3.3 and 16.5 mg L^?1) of PRI and MEL, respectively, were also determined. The method was successfully applied to the determination of both drugs in three brands of tablet formulations. No statistically significant differences were observed when these results were compared with those of a RP-HPLC method.     

MEKC Determination of Nilutamide in Human Serum Using Sweeping in High Salt Sample Matrix

The determination of the antiandrogen drug nilutamide in human serum by MEKC using flutamide as an internal standard is described. Several parameters influencing the separation, such as the running electrolyte composition concerning the micelle concentration and pH, are discussed. MEKC separation was achieved within 7 min using 50 mM sodium borate pH 9.0 with the addition of 50 mM sodium dodecylsulfate at +20 kV. The proposed method was applied to determination of nilutamide in spiked human serum samples after protein precipitation with acetonitrile. The increasing of sensitivity for determination of nilutamide in serum was done by sweeping in a high salt concentration sample matrix when the injection of a larger volume of sample diluted in 150 mM NaCl was applied. The limit of detection after the preconcentration step for nilutamide was 26 ??g L^?1.     

Comparison of LC Columns Packed with 2.6?��m Core-Shell and Sub-2?��m Porous Particles for Gradient Separation of Antibiotics

The recently introduced Kinetex C18 column packed with core-shell 2.6 ??m particles is declared to provide similar efficiency and short analysis as Acquity BEH C18 column with 1.7 ??m porous particles. Unlike Acquity BEH C18 column, Kinetex C18 column exhibited lower column backpressure making this column compatible to conventional LC systems. The performance of Kinetex C18 column (2.1 × 50 mm) and Acquity BEH C18 column (2.1 × 50 mm) for gradient separation of tetracyclines under acidic conditions (oxytetracycline, tetracycline, chlortetracycline, and doxycycline) and macrolides under alkaline conditions (tylosin, clarithromycin, roxithromycin, and carbomycin) was studied. The columns were compared by evaluation of their experimental peak capacity and its dependence on linear velocity and gradient slope. The maximal experimental peak capacities for analysis of tetracyclines were 51.8 (Acquity BEH C18 column) and 48.4 (Kinetex C18 column). This indicated that Kinetex C18 was a suitable alternative to Acquity BEH C18 column for the analysis of tetracyclines under acidic conditions. On the contrary, the maximal experimental peak capacities for analysis of macrolides on Acquity BEH C18 column was higher (46.7) than that on Kinetex C18 column (36.9). Moreover, application of Kinetex C18 column for the analysis of macrolides under alkaline conditions was limited with respect to its decreasing performance with growing number of injections on the column.     

Mercury characterisation in urban particulate matter

A five-step sequential extraction procedure was proposed in order to assess the distribution of mercury (Hg) forms in urban particulate matter (PM): exchangeable, HCl-soluble, organic-bound, elemental and other slightly soluble Hg species, mercury(II) sulphide (HgS), and residual Hg. This process was applied to the analysis of urban dust samples collected at locations in Prague (Czech Republic) with high traffic density. In addition to sequential extractions, thermal desorption analysis was performed. The differences in Hg concentrations between untreated and thermally treated samples were indicated as the thermally releasable amount of Hg. For the study of PM-adsorbing capacity, Hg vapours were passed through the samples as long as the enrichment of materials was observed. The retained elemental Hg was readily released by thermal desorption. All Hg analyses were based on the highly sensitive pyrolysis technique of atomic absorption spectrometry using the mercury analyser AMA-254.