Analytical strategies for sensitive quantitation of drugs and biomarkers from low blood sample volumesUniversity of LiegeBelgium
Marianne Fillet completed Master’s degree in Pharmaceutical Sciences at the University of Liège in 1993 and PhD in 1998 from the same university. She was a Postdoctoral Researcher at FRS-FNRS (National Funds for Scientific Research). She worked as the Professor at the University of Liège and the Head of the Laboratory for the Analysis of Medicines during the year 2010. She is now the Director of the CIRM (Centre for Interdisciplinary Research on Medicines). Her research activity includes: development of analytical methods for drug assays (synthetic drugs and drugs coming from the biotechnology) by HPLC, CE coupled with UV, LIF or MS; discovery and quantification of new disease biomarkers in biological fluids by proteomic and metabolomic approaches and enantiomeric separation of chiral compounds: fundamentals and applications. He has H index of 35 with citations 3302 and 134 publications in peer reviewed journals with cumulative impact factor of 465.8.
In bioanalysis, samples are often available in limited volumes. For example, pharmacokinetic studies on rodents only provide a few dozen microliters of material at a time. In this context, analytical techniques requesting the smallest sample volume possible while keeping a high sensitivity are therefore preferred. To meet these requirements, LC miniaturization (micro- and nano-LC) presents undeniable advantages such as a small injection volume (down to 0.1 ?L), low peak dispersion and reduced flow rates, both favorable to MS sensitivity. The concept of the 3Rs (refine, reduce, replace) is widely followed for in vivo testing, with the aim of reducing the use of animals. In the context of pharmacokinetic or toxicokinetic studies, 3Rs principle is mainly carried out by reducing the sampling volume to perform serial collection on the same animal over the whole study, while preserving animal health and welfare. This evolution requires the development of robust sampling and analytical approaches that handle very small sample volumes. In this presentation, we will discuss on one hand the potential of Dried Blood Spot (DBS) and Volumetric Absorptive MicroSampling (VAMS) compared to classical micro-Solid Phase Extraction (SPE) for the quantitation of hepcidin, chosen as model peptide, in blood samples. This low-concentration peptide was analysed by miniaturised liquid chromatography coupled to tandem MS (LC-Chip-MS/MS) to reach the appropriate sensitivity. On the other hand, a quantitative method was also developed and subsequently validated for the poorly soluble drug itraconazole (ITZ) using VAMS and ultra-high performance liquid chromatography (UHPLC) coupled to tandem mass spectrometry (MS). A proof of concept study showed that the optimized method is applicable to test the bioavailability of drug formulations containing ITZ. To compare the performance of the sample preparation methods, protocols were carefully optimized using the Design of Experiment (DoE) methodology. A special attention was also paid to phospholipid removal (PR) using 96 wellplates. Since whole blood is probably one of the most complex biological matrices than can be analyzed, matrix effect was expected to occur during blood analysis, especially when using a specific sample preparation technique. Matrix effects were thus carefully investigated and quantified.
Thermogravimetric study on preparation of NiTiO3 in different reactions timesSão Paulo UniversityBrazil
Rodrigo V Rodrigues develops materials using the TG/DTG/DSC Thermal Analysis Techniques and TG/MS in the part of obtaining and characterizing the application of thermogravimetry to obtain nanomaterials and luminescent materials, studying kinetic methods (Ozawa) in determining the time of life of compounds. And in the study of photoluminescence applications of the excitation and emission spectra of the luminescence of rare earth elements RE. Has work with collaborations of São Paulo University USP – Brazil, Turku University – Finland and Institute of Low Temperature of Wroclaw – INTIBS – Poland
The thermodynamic properties of the fabrication of NiTiO3 material in different reaction times are reported. The design of this material is accessible through a new efficient sol–gel method, utilizing Ni(Ac)2•4H2O and Ti(OiPr)4 as starting materials for the formation of NiTiO3 final product through thermal decomposition. The Thermogravimetric (TG) and differential scanning calorimetric (DSC) techniques were used to analyze the reaction of Ni(Ac)2•4H2O and Ti(OiPr)4, which produce precursor materials at 0.5, 1, 2, 24, 48 and 72 h of reaction times, as well as the thermal stability of these precursors and the final product. The DSC data show an exothermic phenomenon of releasing large amount of energy: -1393 J/g at TPeak: 655 K as the first event of decomposition started at TOnset: 607 K and finished at TEndset: 663 K for the precursor materials obtained at 0.5 h of reaction, showing the presence of starting materials in this precursor. A similar exothermic behavior was observed in the sample of 1 h of reaction time, and was vanished in the materials obtained at 2 to 72 h of reaction, indicating the influence of the time on the completion of reaction and formation of NiTiO3 crystalline phase as final product of thermal decomposition. In addition, using the information obtained from the TG/DSC, XRD and FTIR analyses, the optimum temperature for the thermal decomposition of the precursor materials to NiTiO3 with fairly high crystallinity was also determined and discussed.
The gas chromatographic analysis of the reaction products of the partial isobutene oxidation as a two-phase processHelmholtz-Zentrum Dresden-RossendorfGermany
Thomas Willms obtained his PhD at the University of Greifswald in 1999 and completed postdoctoral studies at the Helmholtz-Zentrum Dresden Rossendorf and in industry in Paris. In 2007, he joined the GRS Brunswiek and then moved to Helmholtz-Zentrum Dresden Rossendorf. Dr. Willms‘s group currently investigates the oxidation of hydrocarbons with the aim to improve the energy efficiency. His main responsibilities are improving processes and analytics including radical reactions, hydroperoxides and peroxides to reduce product losses.
The partial oxidation of isobutane to t-butyl hydroperoxide (TBHP) has been studied analytically for the first time as a two-phase process in a capillary micro reactor. In order to obtain detailed information on products, yield, selectivity and reaction pathways, the products have been analysed by GC-MS. An Rxi-05-ms column and a PTV-injector have been used to separate the liquid products. The liquid products identified by MS were TBHP, di-t-butyl peroxide (DTBP), t-butanol (TBA), and propanone as main products as well as further by-pro¬ducts e.g. methanal, isopropanol, isobutanol and isobutanal in minor quantities. The liquid products have been obtained by quenching the reaction and vaporizing the isobutane afterwards by pressure reduction using a mass flow controller allowing a constant mass flow. The gaseous phase has been also analysed. Apart from the educts, isobutene has been found.