Important Requirements for the Selection of Internal Standards during the Development of Desorption/Ionization Assays for Drug Quantification in Biological Matrices—A Practical Example

Desorption/ionization mass spectrometry (DI-MS) approaches allow for the rapid quantification of drugs in biological matrices using assays that can be validated according to regulatory guidelines. However, specific adaptations must be applied to create reliable quantification methods, depending on the approach and instrumentation used. In the present article, we demonstrate the importance of the molecular weight, the fragmentation pattern, and the purity of the internal standard for the development of matrix-assisted laser desorption/ionization (MALDI)-ion mobility (IM)-tandem MS and MS/MS methods. We present preliminary results of method development for the quantification of selinexor in microdialysis fluids with a stable isotopically labeled internal standard. In addition, we discuss the selection of internal standards for MALDI-MS assays using different instrumentations.     

Diffusion of Gold Nanoparticles in Inverse Opals Probed by Heterodyne Dynamic Light Scattering

The diffusive behavior of nanoparticles inside porous materials is attracting a lot of interest in the context of understanding, modeling, and optimization of many technical processes. A very powerful technique for characterizing the diffusive behavior of particles in free media is dynamic light scattering (DLS). The applicability of the method in porous media is considered, however, to be rather difficult due to the presence of multiple sources of scattering. In contrast to most of the previous approaches, the DLS method was applied without ensuring matching refractive indices of solvent and porous matrix in the present study. To test the capabilities of the method, the diffusion of spherical gold nanoparticles within the interconnected, periodic nanopores of inverse opals was analyzed. Despite the complexity of this system, which involves many interfaces and different refractive indices, a clear signal related to the motion of particles inside the porous media was obtained. As expected, the diffusive process inside the porous sample slowed down compared to the particle diffusion in free media. The obtained effective diffusion coefficients were found to be wave vector-dependent. They increased linearly with increasing spatial extension of the probed particle concentration fluctuations. On average, the slowing-down factor measured in this work agrees within combined uncertainties with literature data.

     

HILITE—A tool to investigate interactions of matter and light

Detailed investigations of laser–ion interactions require well-defined ion targets and detection techniques for high-sensitivity measurements of reaction educts and products. To this end, we have designed and built the High-Intensity Laser-Ion Trap Experiment Penning trap setup, which features various ion-target preparation techniques including selection, cooling, compression, and positioning as well as destructive and non-destructive measurement techniques to determine the number of stored ions for all charge states individually and simultaneously. We have recently performed first commissioning experiments of ion deceleration and dynamic ion capture with highly charged ion bunches from an electron beam ion source. We have characterized our single-pass non-destructive ion counter in detail and were able to determine the ion velocity as well as the number of ions from the signals acquired.     

Isotope Effect on Diffusion in Nafion Studied by NMR Diffusometry

Applied Magnetic Resonance - The isotope effect H → D on diffusion in proton-exchange membrane Nafion 212 is investigated using 1H and 2H nuclear magnetic resonance (NMR)...     

Crystal Growth in Gels at Elevated Pressures: The Upper Limit of Temperature for Metastable Formation of Aragonite

Both rapid precipitation and diffusion controlled gel growth were applied to crystallize calcium carbonate at temperatures in the range of 100 °C to 270 °C. The amount of aragonite was determined by means of X-ray diffraction data. The morphology of the aragonite crystals are described. Metastable formation of aragonite was observed only at temperatures below 270 °C.     

Raman spectroscopy in high polymer research and production

The mechanism of RAMAN scattering depends on molecular polarizability changes and therefore this method is especially useful for the study of non-polar bonds. This is shown by reviewing some analytical applications. Knowledge on polymer structure was especially promoted by studies of the lowest-frequency bending modes, of correlation splittings in case of crystallinity, and by measurements on depolarization of the laser light. RAMAN spectroscopy has possibilities for in-situ and multi-method measurements. Newer developments serving the polymer sciences are surface enhanced RAMAN scattering and the RAMAN spectroscopy of electroconducting polymers.     

Calculation of one-dimensional temperatures profiles in a crystal growth furnace with special respect to germanium

In the paper a one-dimensional method of calculation for temperature profiles in crystal growth furnaces is described. It is characterized by high flexibility. The model applied to our own calculations is based on heat balances in segments of a multi-zone furnace and presupposes the availability of experimental data which allow the coefficients to be derived which are necessary to carry out the calculations. — The results of numerical calculations demonstrate the applicability of an existing furnace unit to directional crystallization of germanium.