Optimization of a liquid chromatography ion mobility-mass spectrometry method for untargeted metabolomics using experimental design and multivariate data analysis

High-resolution mass spectrometry coupled with pattern recognition techniques is an established tool to perform comprehensive metabolite profiling of biological datasets. This paves the way for new, powerful and innovative diagnostic approaches in the post-genomic era and molecular medicine. However, interpreting untargeted metabolomic data requires robust, reproducible and reliable analytical methods to translate results into biologically relevant and actionable knowledge. The analyses of biological samples were developed based on ultra-high performance liquid chromatography (UHPLC) coupled to ion mobility - mass spectrometry (IM-MS). A strategy for optimizing the analytical conditions for untargeted UHPLC-IM-MS methods is proposed using an experimental design approach. Optimization experiments were conducted through a screening process designed to identify the factors that have significant effects on the selected responses (total number of peaks and number of reliable peaks). For this purpose, full and fractional factorial designs were used while partial least squares regression was used for experimental design modeling and optimization of parameter values. The total number of peaks yielded the best predictive model and is used for optimization of parameters setting.     

Electrical Resistivity Index in Multiphase Flow through Porous Media

The simultaneous flow of two phases through a three-dimensional porous medium is calculated by means of a Lattice-Boltzmann algorithm. The time-dependent phase configurations can be derived and also macroscopic quantities such as the relative permeabilities. When one phase only is supposed to be conductive, the Laplace equation which governs electrical conduction can be solved in each phase configuration; an instantaneous value of the macroscopic conductivity is obtained and it is averaged over many configurations. The influence of saturation on the resistivity index is studied for six different samples and two viscosity ratios. The saturation exponent is systematically determined. The numerical results are also compared to other possible models and also to experimental results; finally, they are discussed and criticized.     

Improving the Estimations of Petrophysical Transport Behavior of Carbonate Rocks Using a Dual Pore Network Approach Combined with Computed Microtomography

Due to the intricate structure of carbonate rocks, relationships between porosity or saturation and petrophysical transport properties classically used for reservoir estimation and recovery strategies are either very complex or nonexistent. Thus, further understanding of the influence of the rock structure on the petrophysical transport properties becomes relevant. We therefore present a Dual Pore Network approach (D-PNM) applied to???-CT images of bimodal porous media. The major advantage of this method lies in the fact that it takes into account the real architecture of the connected macropore network as well as the microporosity unresolved by???-CT imaging. Whereas governing equations are solved in each individual macropore, transport behavior of microporosity is simulated by average quantities. Thus, D-PNM is particularly suited for the investigation of carbonate rocks, characterized by broad pore size distributions. We describe the principles of the image acquisition and network extraction procedure and the governing equations of D-PNM. The model is tested on three carbonate samples, two outcrop, and one reservoir carbonate. Calculated petrophysical transport properties are compared to experimental data and we show that D-PNM correctly reproduces conventional as well as unconventional electrical transport behavior. A major restriction of D-PNM is the requirement of a connected macropore network, that is, especially in the case of carbonates, not always available. Solutions to that are presented.     

Two New Triterpene Saponins from Cyclamen africanum Boiss. & Reuter

Two new oleanane‐type triterpene saponins, afrocyclamins A and B ( 1 and 2 , resp.), were isolated from a MeOH extract of the roots of Cyclamen africanum Boiss . & Reuter , together with three known triterpenoid saponins, lysikokianoside, deglucocyclamin I, and its dicrotalic acid derivative. The structures were elucidated, on the basis of 1D‐ and 2D‐NMR experiments and mass spectrometry as (3β,20β)‐13,28‐epoxy‐16‐oxo‐3‐{O‐β‐D ‐xylopyranosyl‐(1→2)‐O‐β‐D ‐glucopyranosyl‐(1→4)‐O‐[β‐D ‐glucopyranosyl‐(1→2)]‐α‐L ‐arabinopyranosyl}oxy}oleanan‐29‐al ( 1 ) and (3β,16α,20β)‐16,28,29‐trihydroxy‐olean‐12‐en‐3‐yl O‐4‐O‐(4‐carboxy‐3‐hydroxy‐3‐methyl‐1‐oxobutyl)‐β‐D ‐xylopyranosyl‐(1→2)‐O‐β‐D ‐glucopyranosyl‐(1→4)‐O‐[β‐D ‐glucopyranosyl‐(1→2)]‐α‐L ‐arabinopyranoside ( 2 ).     

Theoretical study of some nitrososulfamide compounds with antitumor activity

The lowest-energy conformations of four 2-chloroethylnitrososulfamides were determined using the MM+ molecular mechanics method as implemented in Hyperchem 6.0. Some of the calculated structural parameters, angles and bonds lengths were compared with the crystal structure data of N-nitroso-N-(2-chloroethyl)-N'-sulfamoyl- proline. Using MM+, AM1 and PM3 the anti conformation was predicted to be more stable than the syn conformation in each of these compounds. With these methods we found that the relative energy of the transition state (TS) was considerably higher, but with the ab initio method using RHF with minimal basic function STO-3G we found that the syn conformation is predicted to be slightly more stable. The determination of some atomic charges of a selection of atoms on the syn, anti and TS structures of the various compounds provided some details about the nature of the transition state.     

Fluidised bed pyrolysis of Moroccan oil shales using the hamburg pyrolysis process

In the present work, the pyrolysis of the Moroccan Timahdit oil shale was studied, using a fluidised bed process. Four experiments were carried out at different temperatures between 520 and 630 °C. By mass balance could be shown that in relation to the kerogen content up to 60 wt.% of oil and 25 wt.% of gas are obtained. These are 40% higher yields compared with the Fischer assay. It was shown that the carbon in the residue, which is much lower (only 12 wt.%) than in the Fischer assay (26 wt.%), explains this difference.