Simultaneous LC-MS-MS Analysis of Capecitabine and its Metabolites (5′-deoxy-5-fluorocytidine, 5′-deoxy-5-fluorouridine, 5-fluorouracil) After Off-Line SPE from Human Plasma

A new single extraction procedure was developed to isolate capecitabine and its major metabolites (5′-deoxy-5-fluorocytidine, 5′-deoxy-5-fluorouridine, and 5-fluorouracil) from human plasma. The simultaneous extraction of the four analytes was performed on an Atoll XWP solid phase support. Separation and detection were by liquid chromatography (5 µm Atlantis C₁₈, 150 × 2.1 mm) and Turbospray Mass spectrometry in negative mode. To our knowledge, this report is the first to use these conditions for the simultaneous analysis of capecitabine and its metabolites.     

Morphology determination of small particles by electron microscopy and electrical conduction measurements

In this paper, we show that it is possible to deduce the actual morphology of small particle condensed onto an insulator by combining the granularity analysis from electron micrographs and the electrical sheet conductance of the deposit on its substrate. Assuming the particles are truncated ellipsoids, we determine the excentricity and the contact angle with the substrate for Au on amorphous carbon and MgO substrates.     

Euclidian distance-weighted smoothing for quantitative MRI: application to intervoxel anisotropy index mapping with DTI

During the computation of intervoxel anisotropy features, the inclusion of both eigenvalues and eigenvectors reduces the effect of noise, but spatial averaging blurs the resulting maps. We propose a new adaptive technique that uses data-dependent weights in the averaging process so that the influence of each neighbor in the local window is proportional to the similarity of characteristics of the neighbor considered to those of the reference central voxel. This likeness criterion is based on the multidimensional Euclidian distance using the entire available multispectral information contained in the diffusion-weighted images. This solution is controlled by a single parameter beta that results from a compromise between edge-preserving and noise-smoothing abilities. This Euclidian distance-weighted technique is a generic solution for filtering noise during parametric reconstruction. It was applied to map anisotropy using an intervoxel lattice index (LI) from experimental images of mouse brain in vivo and achieves noise reduction without distorting small anatomical structures. We also show how to employ in the discrimination scheme the images not used in the estimation of the considered feature.     

Detection of susceptibility effects using simultaneous T(2)* and magnetic field mapping

Tracking susceptibility effects is a convenient way to detect small inclusions in a bulk tissue matrix by MRI. We propose a quantitative assessment of these susceptibility effects by simultaneously mapping T(2)* and magnetic field from the time course of magnitude and phase using a multiple GE sequence at 4.7 T. A high-pass scheme is also introduced to highlight the mesoscopic magnetic field variations due to local susceptibility differences specifically in the magnetic field map. Applying this method to muscle tissue, we demonstrate that connective tissue generates detectable susceptibility effects through concomitant local magnetic field variation and T(2)* shortening.     

Small-scale measurements in a partially stirred reactor

This paper describes an experimental study of a partially stirred reactor (PaSR). The reactor is a cubic box in which air (either pure or mixed with a tracer) is continuously injected through 12 jets situated in two opposite planes and impinging through the center. The flow in the reactor interior is well approximated as stationary, globally homogeneous and isotropic. Global properties of turbulent flow and passive scalar mixing are studied, in terms of length scales, characteristic times, spectra, etc. Particular attention has been paid to a proper determination of the mean value of the passive scalar variance dissipation rate 〈ε _Z 〉, in the central quasi-homogeneous zone of the reactor.     

Failure of the Ingard-Myers boundary condition for a lined duct: an experimental investigation

This paper deals with experimental investigation of the lined wall boundary condition in flow duct applications such as aircraft engine systems or automobile mufflers. A first experiment, based on a microphone array located in the liner test section, is carried out in order to extract the axial wavenumbers with the help of an "high-accurate" singular value decomposition Prony-like algorithm. The experimental axial wavenumbers are then used to provide the lined wall impedance for both downstream and upstream acoustic propagation by means of a straightforward impedance education method involving the classical Ingard-Myers boundary condition. The results show that the Ingard-Myers boundary condition fails to predict with accuracy the acoustic behavior in a lined duct with flow. An effective lined wall impedance, valid whatever the direction of acoustic propagation, can be suitably found from experimental axial wavenumbers and a modified version of the Ingard-Myers condition with the form inspired from a previous theoretical study [Aure?gan et al., J. Acoust. Soc. Am. 109, 59-64 (2001)]. In a second experiment, the scattering matrix of the liner test section is measured and is then compared to the predicted scattering matrix using the multimodal approach and the lined wall impedances previously deduced. A large discrepancy is observed between the measured and the predicted scattering coefficients that confirms the poor accuracy provided from the Ingard-Myers boundary condition widely used in lined duct applications.     

Chiral resolution by crystallization of host-guest supramolecular complexes

The crystallization behaviour and the physical characterization of supramolecular complexes formed between permethylated-α-cyclodextrin (TMα-CD) and the enantiomers of phenylethanol (PE) are investigated. According to crystal structure analyses, complexes containing the pure guest enantiomers are almost isomorphous, indicating that the host presents a poor ability to distinguish PE enantiomers at a molecular level. Nevertheless, crystallizations from racemic PE in water induce an efficient chiral discrimination and allow the enantio-separation of the guests despite the existence of a solid solution revealed by XRPD and coupled TG-DSC analyses. The enantiodifferentiation is explained by solubility differences between the two diastereomeric complexes in the studied temperature range. Moreover, it is shown that the diastereomeric complex TMα-CD/(S)-PE crystallizes in two distinct phases: a monohydrate and an anhydrous form, with a transition temperature close to 37°C. The insertion of a water molecule in the crystals grown below 37°C does not involve any other change of the crystal packing nor of the molecular conformation, but leads to different crystal growth mechanisms inducing different morphologies and distinct thermal behaviours. This revised version was published online in July 2006 with corrections to the Cover Date.     

Structure of an icosahedral palladium particle

Small icosahedral palladium particles have been studied using high resolution electron microscopy. In these small particles (d?15 nm) no dislocations have been found so that internal strains are necessary to maintain their coherency. The structural deformations induced by these strains have been investigated and compared to existing models.     

Conserved scalar mixing in a confined-opposed-jets flow

The focus of this paper is on the mixing of a conserved passive scalar for Sc = 1 (Sc is the Schmidt number) in axisymmetric turbulence for which the initial injections of turbulent kinetic energy and scalar variance are similar. Two confined-opposed-jets (COJ) are experimentally studied through simultaneous PIV (particle image velocimetry) and PLIF (planar laser induced fluorescence) measurements, for different flow regimes. One-point transport equation for the scalar variance is assessed through experimental data, along the common axis of the two opposed jets, and different physical phenomena are revealed (production, diffusion, dissipation). The production of scalar variance is equilibrated by the diffusion term (～75%) and the mean dissipation of the scalar variance (～25%). To further assess the scalar behaviour at each scale in this anisotropic, but axisymmetric, flow, a scale-by-scale scalar variance budget equation is derived for axisymmetric turbulence. This equation reduces to Yaglom's 4/3 law, under additional restrictions. The equation is assessed through experimental data, in the impingement region between the two COJ. In particular, the anisotropic energy transfer along different directions is quantified. It is shown that for scales smaller than the size of the central region, Δ, the cascade of the scalar variance is completely inhibited, independently of the particular direction. For scales larger than Δ, the apparent aspect of the energy transfer is that of an inverse cascade, with positive values of the scalar variance transfer. Nonetheless, inhomogeneity of the flow and mixing at those scales is directly responsible for these positive values.