Complexing properties of methyl and phenyl glycine derivatives in their compounds with H+, Ni(II), Cu(II), and Zn(II)

The influence of the solvent and the substituents on the complexing properties of methyl and phenyl glycine derivatives is discussed. On the basis of a computer analysis of potentiometric titration results, the composition and the stability constants of the complexes ofN-methylglycine,N,N-dimethylglycine,N-phenylglycine and phenylglycine with H⁺ and with Ni(II), Cu(II), Zn(II) were determined. The ligand-metal coordination mode as well as the zwitterion level in percent in ligand/proton systems were determined by spectral analyses and equilibria studies.

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Komplexbildung der Methyl- und Phenylglycin-Derivate in ihren Verbindungen mit dem Proton und Ni(II), Cu(II) und Zn(II)

Zusammenfassung Der Einfluß des Lösungsmittels und der Substituenten auf die komplexbildenden Eigenschaften der Methyl- und Phenylglycin-Derivate wird diskutiert. Anhand einer Computer-Analyse von potentiometrischen Daten wurden die Zusammensetzung und die Beständigkeitskonstanten der Komplexe vonN-Methylglycin,N,N-Dimethylglycin,N-Phenylglycin und Phenylglycin mit H⁺, Ni(II), Cu(II) und Zn(II) festgestellt. Mittels spektroskopischer Methoden und Gleichgewichtstudien wurde der Koordinationstyp des Liganden mit dem Metall festgestellt sowie der Prozentanteil des Zwitterions im Ligand/Proton-System.

     

HPLC–MS Analysis of Isoniazid in Dog Plasma

A simple, rapid, and sensitive liquid chromatography–mass spectrometric (LC–MS) method was developed and validated for the determination of isoniazid in dog plasma. Plasma samples were deproteined with methanol and separated on a C₁₈ column interfaced with a single quadrupole mass spectrometer, using 0.1% formic acid–acetonitrile (91:9 v/v) as mobile phase. Detection was performed by positive electrospray ionization with selected ion monitoring at m/z 138 for isoniazid and 152 for entecavir maleate internal standard. Linearity was obtained over the range of 25–5,000 ng mL^?1, with a lower limit of quantification of 25 ng mL^?1. The intra- and inter-day precision was less than 2.7% in terms of relative standard deviation. Accuracy, expressed as relative error, ranged from ?2.0 to 8.0%. Plasma samples were analysed within 5 min. The method was successfully applied to the evaluation of the pharmacokinetics of isoniazid in dog plasma.     

Inductively coupled plasma mass spectrometric determination of molybdenum in urine

A method was developed for the determination of molybdenum (Mo) in human urine by direct dilution of the sample in doubly distilled water with 1% HNO3 (v/v) and inductively coupled mass spectrometry (ICP-MS). In and Y were used as internal standards. Since (98)Mo provides a higher sensitivity, it was chosen as the reference isotope. The influence of different factors, such as sample dilution, HNO3 concentration and the stability of the analyte were evaluated. The detection limit (LOD) was assessed at 0.2 microg/L Mo, while the lower limit of quantification (LOQ) was 0.6 microg/L. Recoveries ranged between 97.2 and 100.7% from solutions containing from 10 to 50 microg/L Mo. Linear calibration curves were generated from 2.1 and 52.1 microg/L with coefficients of variation (CV ) ranging from 1.62 to 3.56%. In order to establish reference values (RV) for molybdenum, the procedure presented here was used to determine Mo in the urine of a population group living in Tuscany, Italy.     

227-01227-01227-01-property and normal subgroups

Summary D-property (=set of primes) in finite groups is not in general inherited by subgroups. In this paper, as evidence in favor of the following conjecture (F. Gross): (o) If a finite group G satisfies D then its normal subgroups satisfy D-property as well. the Author shows that if the D and the D-properties (=set of the primes not in ) hold together in a finite group G, then both are inherited by the normal subgroups of G. As a corollary, the characterization of the groups satisfying both the properties D and D is given in terms of the composition factors.     

Comparative DSC study of human and bovine serum albumin

The thermal denaturation process of bovine and human both fatty acid containing and fatty acid free albumins in aqueous solution was studied by use of differential scanning calorimetry. Human serum albumins were found to be more stable than their bovine counterparts. Fatty acid free albumins were characterized as generally less stable, more susceptible to aggregation, their unfolding endothermic transition was less cooperative and with the smaller degree of reversibility. Deconvolution analysis with using a non-two-state model with two component transitions showed essential differences in the thermodynamic parameters between all studied albumins, particularly regarding the high-temperature component transition.     

A new convenient synthesis of N-acyl-2-(dimethoxyphosphoryl)glycinates

Easily accessible N-acyl-2-triphenylphosphonioglycinate tetrafluoroborates react smoothly with trimethylphosphite in the presence of methyltriphenylphosphonium iodide to give N-acyl-2-(dimethoxyphosphoryl)glycinates in good or very good yields. The dimethoxyphosphorylglycinates may be isolated by column chromatography, or used directly for the Wadsworth-Emmons synthesis of α,β-dehydro-α-amino acids in a one-pot procedure without purification.     

Mixed Azines of Naloxone with Dihydromorphinone Derivatives

The mixed azines 4 and 5 were prepared by reaction of naloxazone ( 2 ) with either oxymorphone ( 6 ) or 14-O-methyloxymorphone ( 7 ) and tested in vitro using opioid receptor binding assays and in vivo using the AcOH-writhing test in mice. Compound 4 was found to be a partial agonist, while compound 5 was a potent opioid agonist with higher potency than morphine.     

High-performance liquid chromatography with post-column derivatisation and fluorescence detection for sensitive determination of aflatoxin M1 in milk and cheese

A new HPLC method with fluorescence detection using pyridinium hydrobromide perbromide as a post-column derivatising agent has been developed to determine aflatoxin M1 in milk and cheese. The detection limits were 1 ng/kg for milk and 5 ng/kg for cheese. The calibration curve was linear from 0.001 to 0.1 ng injected. The method includes a preliminary C18-SPE clean-up and the average recoveries of Aflatoxin M1 from milk and cheese, spiked at levels of 25-75 ng/kg and 100-300 ng/kg, respectively, were 90 and 76%; the precision (RSDr) ranged from 1.7 to 2.6% for milk and from 3.5 to 6.5% for cheese. The method is rapid, easily automatable and therefore useful for accurate and precise screening of aflatoxin M1 in milk and cheese.     

High-performance liquid chromatographic determination of Levetiracetam in human plasma: comparison of different sample clean-up procedures

An accurate and precise high-performance liquid chromatographic method using diode array detection for the determination of the novel antiepileptic, Levetiracetam, has been developed. Three clean-up procedures for the analysis of Levetiracetam in human plasma were implemented and evaluated, namely solid-phase extraction, deproteinization by addition of organic solvents and formation of insoluble salts. Adenosine was used as the internal standard for all three sample pretreatment procedures. Among the several cartridges used for solid-phase extraction, the hydrophilic-lypophilic balance (Oasis) HLB) phase provides the best extraction yield of Levetiracetam, together with high precision. With the two other clean-up procedures involving plasma deproteinization by addition of methanol or zinc sulphate, lower sensitivity and precision of the assays were obtained. However, they are cheaper and faster when compared with the solid-phase extraction procedure.