Enhanced selectivity of the isolation of basic drugs from body fluids by means of extraction minicolumns and sophisticated elution schemes.

The paper presents results and experience obtained in the isolation of a number of basic polar/non-polar solutes (drugs, their metabolites and structural derivatives) from biological samples by using the separation minicolumns Separcol SI and Separcol SI C18 L/T. The aim was to provide insight into some simple procedures yielding optimal selectivity/specificity of the isolation of the studied solutes either by proper selection of the sorbent or by applying sophisticated elution schemes which use to advantage different properties of the eluents/solvents.     

Flame Temperature Effect on the Structure of SiC Nanoparticles Grown by Laser Pyrolysis

Small SiC nanoparticles (10 nm diameter) have been grown in a flow reactor by CO₂ laser pyrolysis from a C₂H₂ and SiH₄ mixture. The laser radiation is strongly absorbed by SiH₄ vibration. The energy is transferred to the reactive medium and leads to the dissociation of molecules and the subsequent growth of the nanoparticles. The reaction happens with a flame. The purpose of the experiments reported in this paper is to limit the size of the growing particles to the nanometric scale for which specific properties are expected to appear. Therefore the effects of experimental parameters on the structure and chemical composition of nanoparticles have been investigated. For a given reactive mixture and gas velocity, the flame temperature is governed by the laser power. In this study, the temperature was varied from 875°C to 1100°C. The chemical analysis of the products indicate that their composition is a function of the temperature. For the same C/Si atomic ratio in the gaseous phase, the C/Si ratio in the powder increases from 0.7 at 875°C up to 1.02 at 1100°C, indicating a growth mechanism limited by C₂H₂ dissociation. As expected, X-ray diffraction has shown an improved crystallisation with increasing temperature. Transmission electron microscopy observations have revealed the formation of 10 nm grains for all values of laser power (or flame temperature). These grains appear amorphous at low temperature, whereas they contain an increasing number of nanocrystals (2 nm diameter) when the temperature increases. These results pave the way to a better control of the structure and chemical composition of laser synthesised SiC nanoparticles in the 10 nm range.     

Thickness dependence of free‐standing thin films

Below a critical thickness, of about 60 nm, the glass transition temperature of polystyrene (PS) films decreases with film thickness, as demonstrated using free‐standing films. A geometrical model is developed here describing this phenomenon in the case of ideal (Gaussian) chains. This model, which can be considered as an application of the free volume model, assumes that the decrease of the glass transition temperature from thick to ultrathin films is due to the modification of the interpenetration between neighboring chains. The theoretical curve deduced from the model is in excellent agreement with the PS experimental results, without using any adjustable parameters. From these results, it can be concluded that new chain motions, usually buried in bulk samples, are expressed by the presence of the surface. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 10–17, 2007     

Producing and transferring low-spatial-frequency grids for measuring displacement fields with moiré and grid methods

Experimental Techniques -     

Rate of Convergence of a Stochastic Particle System for the Smoluchowski Coagulation Equation

By continuing the probabilistic approach of Deaconu et al. (2001), we derive a stochastic particle approximation for the Smoluchowski coagulation equations. A convergence result for this model is obtained. Under quite stringent hypothesis we obtain a central limit theorem associated with our convergence. In spite of these restrictive technical assumptions, the rate of convergence result is interesting because it is the first obtained in this direction and seems to hold numerically under weaker hypothesis. This result answers a question closely connected to the Open Problem 16 formulated by Aldous (1999).     

An iterative procedure for differential analysis of gene expression

Microarrays are a popular technology to study genes that are differentially expressed between two conditions. In this Note, we propose an iterative procedure to determine the biggest subset of non-differentially expressed genes. We prove a pseudo Markov relationship that allows practical computations. We obtain explicit expressions for FDR and the level of the proposed test at each step. To cite this article: A. Bar-Hen, S. Robin, C. R. Acad. Sci. Paris, Ser. I 337 (2003).     

Photonic crystals--a step towards integrated circuits for photonics.

The field of photonic crystals has, over the past few years, received dramatically increased attention. Photonic crystals are artificially engineered structures that exhibit a periodic variation in one, two, or three dimensions of the dielectric constant, with a period of the order of the pertinent light wavelength. Such structures in three dimensions should exhibit properties similar to solid-state electronic crystals, such as bandgaps, in other words wavelength regions where light cannot propagate in any direction. By introducing defects into the periodic arrangement, the photonic crystals exhibit properties analogous to those of solid-state crystals. The basic feature of a photonic bandgap was indeed experimentally demonstrated in the beginning of the 1990s, and sparked a large interest in, and in many ways revitalized, photonics research. There are several reasons for this attention. One is that photonic crystals, in their own right, offer a proliferation of challenging research tasks, involving a multitude of disciplines, such as electromagnetic theory, nanofabrication, semi-conductor technology, materials science, biotechnology, to name a few. Another reason is given by the somewhat more down-to-earth expectations that photonics crystals will create unique opportunities for novel devices and applications, and contribute to solving some of the issues that have plagued photonics such as large physical sizes, comparatively low functionality, and high costs. Herein, we will treat some basics of photonic crystal structures and discuss the state-of-the-art in fabrication as well give some examples of devices with unique properties, due to the use of photonic crystals. We will also point out some of the problems that still remain to be solved, and give a view on where photonic crystals currently stand.     

Two Stage Solid Phase Extraction with Subsequent HPLC Isolation for Structure Elucidation of Major Metabolites of (+)-(R)-2-{3-(benzo[1,4]dioxan-2-yl-methylamino)-1-propyl}-3(2H)-pyridazinone (GYKI-16084)

GYKI-16084 – (+)-(R)-2-{3-(benzo[1,4]dioxan-2-yl-methylamino)-1-propyl}-3(2H)-pyridazinone hydrochloride – is a new drug candidate for the treatment of benign prostatic hyperplasia. In our study the major metabolites formed in the rat and dog were isolated from dog and rat urine, then their structures were elucidated by means of MS and NMR. A two stage solid phase extraction (SPE) procedure and a semi-preparative HPLC method were developed utilizing various mechanisms of separation. The major metabolites proved to be isomeric glucuronides of the benzodioxane moiety hydroxylated at positions 6 or 7 and {2-(2-carboxyethyl)-3(2H)-pyridazinone}.