Determination of netilmicin in serum by thin-layer densitometry and fluorescence polarization immunoassay

Summary A newly developed thin-layer chromatographic method (TLC) for the quantitative determination of netilmicin in serum is described and compared with fluorescence polarization immunoassay (FPIA). The TLC procedure involves solid-phase extraction of the aminoglycoside from serum and chromatography on reversed-phase thin layer. Post-chromatographic derivatization is carried out using 2,2-diphenyl-1-oxa-3-oxonia-2-boratanaphthalene (DOOB) as fluorescence reagent. The calibration curve for netilmicin in serum is linear in the range 1.0–5.0 g/ml and the detection limit is about 0.2 g/ml (correlation coefficient r=0.9963, mean coefficient of variation V_XO=±5.3 %). A total of 25 serum samples from patients treated with netilmicin was measured by TLC and the results were compared with those of FPIA (Abbott TDx). There is no statistically significant difference between the two procedures (y=–0.35+1.094·x, Passing/Bablok). Thus the TLC-procedure is an alternative for the determination of netilmicin in serum, that possesses the necessary sensitivity of other comparable methods.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday.     

Zur Kenntnis des Dianthryls

Ohne ZusammenfassungErste Mitteilung: Hans Meyer, Monatshefte für Chemie,30, 165 (1909). — Zweite Mitteilung: Hans Meyer, R. Bondy und A. Eckert, Monatshefte für Chemie,33, 1447 (1912).     

Eine neue Synthese des Phenazins

Ohne Zusammenfassung     

Copper deposition and dissolution in seemingly parallel electric and magnetic fields: Lorentz force distributions and flow configurations

In two different cylindrical electrochemical cells, copper deposition and dissolution in the presence of a magnetic field mostly parallel to the electric field was investigated. Particle image velocimetry measurements show that even under such a field configuration where Lorentz forces are often a priori neglected may in fact dominate the flow. Further, depending on the electrode radius, a reversal of the secondary flow was found. This feature can be explained by the different Lorentz force configurations calculated from the magnetic field and the primary current distributions. The components of the magnetic field were determined by means of a traversed Hall probe and were calculated by a commercial finite element package. Experimentally and numerically determined field distributions match very well. A good agreement between the measured and calculated velocity distributions was also found, suggesting that in the present case the effect of the Lorentz force alone is sufficient to explain the magnetic field influence on the flow. Contribution to the special issue “Magnetic field effects in Electrochemistry”     

Three level atom optics in dipole traps and waveguides

An analogy is explored between a setup of three atomic traps coupled via tunneling and an internal atomic three-level system interacting with two laser fields. Within this scenario we describe a STIRAP like process which allows to move an atom between the ground states of two trapping potentials and analyze its robustness. This analogy is extended to other robust and coherent transport schemes and to systems of more than a single atom. Finally it is applied to manipulate external degrees of freedom of atomic wave packets propagating in waveguides.     

Solid-State Nuclear Magnetic Resonance Techniques for the Structural Characterization of Geminal Alane-Phosphane Frustrated Lewis Pairs and Secondary Adducts

The first comprehensive solid-state nuclear magnetic resonance (NMR) characterization of geminal alane-phosphane frustrated Lewis pairs (Al/P FLPs) is reported. Their relevant NMR parameters (isotropic chemical shifts, direct and indirect ²⁷Al-³¹P spin-spin coupling constants, and ²⁷Al nuclear electric quadrupole coupling tensor components) have been determined by numerical analysis of the experimental NMR line shapes and compared with values computed from the known crystal structures by using density functional theory (DFT) methods. Our work demonstrates that the ³¹P NMR chemical shifts for the studied Al/P FLPs are very sensitive to slight structural inequivalences. The ²⁷Al NMR central transition signals are spread out over a broad frequency range (>200 kHz), owing to the presence of strong nuclear electric quadrupolar interactions that can be well-reproduced by the static ²⁷Al wideband uniform rate smooth truncation (WURST) Carr-Purcell-Meiboom-Gill (WCPMG) NMR experiment. ²⁷Al chemical shifts and quadrupole tensor components offer a facile and clear distinction between three- and four-coordinate aluminum environments. For measuring internuclear Al⋅⋅⋅P distances a new resonance-echo saturation-pulse double-resonance (RESPDOR) experiment was developed by using efficient saturation via frequency-swept WURST pulses. The successful implementation of this widely applicable technique indicates that internuclear Al⋅⋅⋅P distances in these compounds can be measured within a precision of ±0.1 Å.