Determination of melengestrol acetate in bovine tissues by automated coupled-column normal-phase high-performance liquid chromatography

A method has been developed for the determination of melengestrol acetate in bovine tissues at lower levels than previously reported. Liquid-liquid extraction of tissue homogenates provided crude clean-up while final isolation, screening, and quantification was done on-line with an automated, normal-phase, coupled-column high-performance liquid chromatographic system. The chromatographic system included phenyl and silica analytical columns for the purposes of isolation and final separation, respectively. These columns provided a large difference in selectivity when operated under normal-phase conditions which allowed for the efficient isolation of melengestrol acetate from the complex tissue extracts. Mobile phases were composed of hexane and dichloromethane modified with methanol and water. Transfer and enrichment of the analyte from the primary phenyl column to the silica column was via a short (12 mm x 4 mm I.D.) silica column. Regeneration and equilibration of the phenyl column was performed after the injection of each tissue extract and was accomplished simultaneously while analytical separation occurred on the final silica column. Routing of the mobile phases and regeneration solvent was performed with automated switching valves. The total time required for each analysis was 12 min. Quantification is demonstrated using external standards with UV detection at 287 nm. The overall recovery of the method was 86% with a coefficient of variation of 9.84% at the 10 ppb [the American billion (10(9] is used in this article] level in bovine liver extracts.     

Derivation of fluorine-containing pyridine dicarboxylates. II. Elaboration at the 4-position

In response to the bio-activity found in fluorine-containing 4-alkyl-3, 5-pyridinedicarboxylates, a series of novel 4-substituted derivatives, not directly available by Hantzsch sequences, were prepared. Starting 4-alkylpyridines, 1 , were converted via enamine 2 to materials 3–8 . Derivatives 9–16 in turn were derived from aldehyde 3 , while acid derivatives 28–36 were prepared from 14 . Addition of oxygen, sulfur, and carbenoids effected conversion of 4-allylpyridine 16 to epoxy and cyclopropyl derivative 16–22 . A number of neighboring group effects were noted, including those forming the fused-ring systems 23-27 .     

On the heterogeneity of125I-labelled proteins used as tracers in radioimmunoassay

The distribution of mono- poly- and unlabelled protein molecules in the radiolabelling mixture was calculated from probability point of view as a function of the radioiodine/protein ratio.     

Analysis and prediction of primary structures of proteins using a computer

On the basis of a computer analysis of four classes of toxic polypeptides, generalized primary structures of each class have been obtained which can be used for planning the synthesis of biologically active compounds.     

Quantitative Bestimmungen mittels cyclischer Voltammetrie an der Phasengrenze zweier mischbarer Elektrolytl?sungen

Summary This paper presents some applications of cyclic voltammetry at the interface of two immiscible electrolyte solutions by means of an experimental set-up described in a former publication. When using special sample preparation good results are obtained for the determination of iodide and quinine in pharmaceutical products as well as for the determination of quinine in tonic water and dodecylsulfate in a tooth-salt.

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Herrn Prof. Dr. Günther Tölg zum 60. Geburtstag gewidmet     

The auction algorithm for the transportation problem

The auction algorithm is a parallel relaxation method for solving the classical assignment problem. It resembles a competitive bidding process whereby unassigned persons bid simultaneously for objects, thereby raising their prices. Once all bids are in, objects are awarded to the highest bidder. This paper generalizes the auction algorithm to solve linear transportation problems. The idea is to convert the transportation problem into an assignment problem, and then to modify the auction algorithm to exploit the special structure of this problem. Computational results show that this modified version of the auction algorithm is very efficient for certain types of transportation problems.     

Numerical differentiation of photomechanical data using smoothing spline functions with generalized boundary conditions

The smoothing spline function has been used for differentiation of photomechanical data in experimental stress analysis. However, since the available software packages use the algorithm with the so-called natural boundary conditions which are not necessarily suitable in many circumstances, errors tend to occur in both the first and second derivatives. In this paper we have modified the algorithm so that the user can have more freedom in selecting boundary conditions which suit the problem best and therefore, as a result, improve the accuracy of the analysis. Two examples are given to show the improvement achievable using the new scheme.