Manual and automated enrichment procedures for biological samples using lipophilic gels

Aspects of the use of lipophilic gels in manual sample preparation procedures are reviewed. Neutral gels with a controlled hydrophobicity are used for sorbent extraction of non-polar and medium polarity compounds from biological fluids. Acidic amphiphilic compounds can be extracted as ion-pairs with decyltrimethylammonium ions. Solvent or detergent extracts of tissues or faeces can be mixed with hydrophobic gels for transfer of analytes from a solvent to a gel phase, permitting subsequent sample preparation in gel bed systems. Hydrophobic gels, alkyl-bonded silica and polystyrene matrices can be used in series for extraction of compounds with a wide range of polarities. Group fractionations are performed on neutral and ion-exchanging lipophilic gels to yield fractions of neutral, basic and acidic metabolites within selected polarity ranges. Selective isolation of phenolic acids on a strong anion exchanger, of ethynylic steroids on a strong cation exchanger in silver form and of oximes of ketonic steroids on a strong cation exchanger in hydrogen form is possible. A computerized system for automatic sample preparation is also described. It consists of an extraction bed, a cation-exchange column and an anion-exchange column. The pumps and switching valves are arranged so that the columns can operate in series or parallel for isolation of neutral, basic and acidic metabolites of amphiphilic compounds and for regeneration of the column beds. Fractions can be collected, or the effluent from the column beds can be diluted with water to permit sorption on a solid phase. The applicability of the automated method to the analysis of bile acids and metabolites of mono(2-ethylhexyl) phthalate is demonstrated.     

Vibrational and high pressure conformational studies of 1,1,2-trichloroethane

The infrared spectra of 1,1,2-trichloroethane were recorded from 4000 to 50 cm^?1 in the vapour and liquid states. Additional spectra above 200 cm^?1 of the low temperature crystal and of two crystalline solids, prepared by compressing the sample in a diamond anvil cell, were obtained. Also, infrared spectra of the liquid and of the compound dissolved in CS₂ were recorded at increased pressures. Raman spectral data of the liquid (including polarization measurements) and of the low temperature crystal were obtained.The fundamental frequencies for each of the two conformers, C₁ and C_s, were assigned and the results checked by normal coordinate analysis. The same diagonal and off-diagonal force constants were employed for the two conformers and the force fields were derived by means of a least squares refinement, including data for chloroethane, 1,1-dichloroethane and various deuterated species. A standard deviation of 3 % was obtained in the final fit.From the changes in relative intensities for infrared bands belonging to the C₁ and C_s conformers with increasing pressure, the volume differences (ΔV¯between the conformers were determined in CS₂ solution and in the pure liquid.     

Application of high-performance liquid chromatography of some antibiotics in clinical microbiology

During recent years high-performance liquid chromatography has become an excellent tool for the determination of antibiotics in biological fluids. Compared with biological assays, the major benefits of this method are specificity and rapidity. In particular, the determination of biologically inactive metabolites emphasizes that this technique plays an outstanding role for the analysis of antibiotics. This paper describes how the method can be used in the analysis of several antibiotics and demonstrates the efficacy of this method for clinical microbiology. Methods for the determination in biological fluids of acylaminopenicillins (azlocillin, mezlocillin, piperacillin and aspoxicillin), quinolones (ciprofloxacine, norfloxacine and ofloxacine), a penem (imipenem) and a cephalosporin (cefixime) are summarized. Furthermore, their application to in vitro studies and their trial in clinical studies are described.     

Rare Events in Random Geometric Graphs

This work introduces and compares approaches for estimating rare-event probabilities related to the number of edges in the random geometric graph on a Poisson point process. In the one-dimensional setting, we derive closed-form expressions for a variety of conditional probabilities related to the number of edges in the random geometric graph and develop conditional Monte Carlo algorithms for estimating rare-event probabilities on this basis. We prove rigorously a reduction in variance when compared to the crude Monte Carlo estimators and illustrate the magnitude of the improvements in a simulation study. In higher dimensions, we use conditional Monte Carlo to remove the fluctuations in the estimator coming from the randomness in the Poisson number of nodes. Finally, building on conceptual insights from large-deviations theory, we illustrate that importance sampling using a Gibbsian point process can further substantially reduce the estimation variance.

     

90–120 GHz millimeter wave power head

Power-voltage and frequency characteristics of power heads for 90–120 GHz TE₁₀-mode millimeter waves are presented. Operation of the power heads is based on thermo-e.m.f. of hot charge carriers in silicon. The head has been tested both in the pulsed and continuous generation regime. The experiments were carried out in the power range of 2·10^–3–4 W. In the pulse regime, the shortest pulse duration was 1s.     

Ergodicity of a Class of Cocycles Over Irrational Rotations

It is proved that if is irrational and L²(S¹) with o(l/n)then for each mZ\{0} the corresponding skew product is ergodic. The rigidity of specialflows over irrational rotations with roof functions whose Fouriercoefficients are in o(l/n) is also shown.     

Sur le comportement asymptotique des potentiels d'une chaîne de Markov sur ℝ d

Résumé Dans cet article j'étudie le comportement à l'infini des potentiels des chaînes de Markov sur ^d (d3) proches du mouvement brownien, tout spécialement le cas des marches aléatoires, ainsi que des critères de transience et de récurrence inspirés de la méthode utilisée.

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We study the asymptotic behaviour of potentials of Markov chains on ^d (d3), closed to Brownian motion, and particularly the case of random walks. Following a similar approach, we give transience and recurrence criteria.

     

An investigation of intermittency in proton-gold, oxygen-gold, sulphur-gold and sulphur-sulphur interactions at 200 GeV per nucleon

The intermittency phenomenon is investigated in proton-gold, oxygen-gold, sulphur-gold and sulphur-sulphur collisions at 200 GeV per nucleon. The data were taken with the NA 35 streamer chamber detector at the CERN SPS. The data samples are carefully corrected for double counting of tracks and for contamination from photon conversions, particle decays and secondary interactions. The analysis is carried out in terms of factorial moments, using a new definition, and of correlation integrals. Both methods show the presence of nonstatistical fluctuations (intermittency). The main conclusions are: The observation of the effect for pairs of hadrons with negative charges and its near absence for pairs of opposite charges is consistent with the assumption that Bose-Einstein correlations yield the dominant contribution. The intermittency effect is not proportional to (dn/dy)^–1 which would be expected in superposition models. The measured relation between the second and third factorial moment for negative hadrons indicates that genuine 3-particle correlations are small. The predictions of a Monte Carlo simulation which is based on the Lund Fritiof model with the inclusion of Bose-Einstein correlations agree with the experimental results.Deceased     

Essential spectrum and -solutions of one-dimensional Schrödinger operators

In 1949, Hartman and Wintner showed that if the eigenvalue equations of a one-dimensional Schrödinger operator possess square integrable solutions, then the essential spectrum is nowhere dense. Furthermore, they conjectured that this statement could be improved and that under this condition the essential spectrum might always be void. This is shown to be false. It is proved that, on the contrary, every closed, nowhere dense set does occur as the essential spectrum of Schrödinger operators which satisfy the condition of existence of -solutions. The proof of this theorem is based on inverse spectral theory.