Determination of ceftriaxone in cerebrospinal fluid by ion-pair liquid chromatography

An ion-pair liquid chromatographic assay was developed and validated for the determination of ceftriaxone in cerebrospinal fluid. Chromatographic separation was achieved on a C18 column (125 x 4 mm, 5 microm) with detection at 270 nm, a 1 mL/min flow rate and a 50 microL loop. The mobile phase consisted of 300 mL acetonitrile, 50 mL 0.1M phosphate buffer (pH 7.4), 3.2 g tetrabutylammonium bromide as the ion-pairing agent, and dilution with distilled deionized water to 1 L. Cephradine was used as the internal standard. The assay was linear for ceftriaxone concentrations of 0.5-50 microg/mL. The coefficients of variation for precision were <4.61%. The accuracy ranged from 96.07 to 102.42%. The detection and quantitation limits were 0.019 and 0.065 microg/mL, respectively. This method was used to quantify ceftriaxone in the cerebrospinal fluid of children with meningitis. The results showed that the method described here is useful for the determination of ceftriaxone in cerebrospinal fluid.     

Spectrophotometric determination of gallium in alloys and fly-ash with pyridoxal derivatives of thiocarbohydrazide and carbohydrazide

The symmetric derivatives of pyridoxal with thiocarbohydrazide and carbohydrazide, and the asymmetric derivatives of pyridoxal and salicylaldehyde with the same hydrazides have been synthesized and their analytical potential for spectrophotometric and kinetic fluorimetric determination of metal ions was studied. Gallium(III) and PyMAU(1,3-bis{[4-(2-methyl-3-hydroxy-5-hydroxymethyl)pyridyl]methyleneaminourea at pH = 4.2 form a complex with a single absorption maximum at 425 nm, which can be extracted into cyclohexanone in the presence of a controlled amount of sodium perchlorate. The extract has maximum absorbance at 435 nm. Both systems can be used for determining gallium. The optimal range of gallium concentration for measurement in a 1-cm cell is 0.5-1.25 gmg/ml for the procedure in homogeneous medium ((425) = 3.76 x 10(4).mole(-1).cm(-1)) and 0.25-1.25 mug/ml for the extraction procedure ((435) = 5.30 x 10(4) 1.mole(-1).cm(-1). The latter procedure has been applied to the determination of gallium in alloys and fly-ash.     

Correlation of natural and artificial radionuclides in soils with pedological,climatological and geographic parameters

Various types of soil samples were collected in the southern part of Brazil, with depth intervals of 5 cm, down to 50 cm, using a specially designed sampler. Pedological analysis of these soils were performed. Nuclear activities of¹³⁷Cs (expressed in Bq m^–2) and radioactive natural element (²²⁶Ra,²²⁸Ra and⁴⁰K) concentrations were determined by low background gamma-ray spectrometry.¹³⁷Cs concentrations were correlated with radioactive natural element concentrations and pedological, climatological and geographic parameters related to the soil samples collected.     

Crystallographic and spectroscopic studies on palladium(II) complexes containing pyrazole and thiocyanate ligands

Mononuclear palladium(II) complexes containing both pyrazole-type ligands and thiocyanate, of general formula [Pd(SCN)₂(L)₂] {L = pyrazole (HPz) and 1-phenyl-3-methylpyrazole (phmPz)} have been prepared and characterized by elemental analysis, i.r. and n.m.r. spectroscopy and by single crystal X-ray diffraction methods. The Pd atom in these structures lies on the crystallographic inversion center; in a square-planar coordination geometry made by two sulfur and two nitrogen atoms of the ligands, both in trans positions.     

Rolling Against a Sphere: The Non-transitive Case

We study the control system of a Riemannian manifold M of dimension n rolling on the sphere \(S^n\). The controllability of this system is described in terms of the holonomy of a vector bundle connection which, we prove, is isomorphic to the Riemannian holonomy group of the cone C(M) of M. Using Berger’s list, we reduce the possible holonomies to a few families. In particular, we focus on the cases where the holonomy is the unitary and the symplectic group. In the first case, using the rolling formalism, we construct explicitly a Sasakian structure on M; and in the second case, we construct a 3-Sasakian structure on M.     

Fast and Simple Preparation of a Sensor Based on Electrochemically Reduced Graphene Oxide (rGO) for the Determination of Zopiclone in Pharmaceutical Dosage by Square Wave Adsorptive Stripping Voltammetry (SWAdSV)

The interactions of zopiclone with electrochemically reduced graphene oxide (rGO) modified electrode were examined. A comparison of GC/rGO and glassy carbon electrode (GC) by electrochemical impedance spectroscopy and scanning electrochemical microscopy (SECM) shows that the modified surface is much less conductive than GC. The role of rGO is to act as a site of specific adsorption of the analyte. Molecular dynamics showed that the monoanionic form of zopiclone presents more interactions with defects of rGO. The analytical methodology allowed obtaining a linearity of 10–130 μg L⁻¹, with a limit of detection of 2.14 μg L⁻¹ using SWAdSV at pH 10.0.     

Multivariate generalized Bernstein polynomials: identities for orthogonal polynomials of two variables

We introduce polynomials $B^n_{k}(\boldmath{x};\omega|q)$ of total degree n, where $\boldmath{k} = (k_1,\ldots,k_d)\in\mathbb N_0^d, \; 0\le k_1+\ldots+k_d\le n$ , and $\boldmath{x}=(x_1,x_2,\ldots,x_d)\in\mathbb R^d$ , depending on two parameters q and ω, which generalize the multivariate classical and discrete Bernstein polynomials. For ω=0, we obtain an extension of univariate q-Bernstein polynomials, introduced by Phillips (Ann Numer Math 4:511–518, 1997). Basic properties of the new polynomials are given, including recurrence relations, q-differentiation rules and de Casteljau algorithm. For the case d=2, connections between $B^n_{k}(\boldmath{x};\omega|q)$ and bivariate orthogonal big q-Jacobi polynomials—introduced recently by the first two authors—are given, with the connection coefficients being expressed in terms of bivariate q-Hahn polynomials. As limiting forms of these relations, we give connections between bivariate q-Bernstein and Dunkl’s (little) q-Jacobi polynomials (SIAM J Algebr Discrete Methods 1:137–151, 1980), as well as between bivariate discrete Bernstein and Hahn polynomials.