Electrochemical reduction of Bi2Sr2Ca1Cu2O8 superconductor single crystals

Single crystals and polycrystalline pellets of the high-temperature cuprate superconductor Bi₂Sr₂Ca₁Cu₂O₈ were doped at room temperature by electrochemical reduction at > 95% Coulombic efficiency using lithium dopant ions in propylene carbonate electrolyte. Cyclic voltammetry and potential step measurements on single crystals suggest an unusual reduction mechanism, with a diffusion coefficient for Li⁺ in the c-axis direction of bulk superconductor of ca. 3 × 10⁻¹¹ cm²s⁻¹. Sintered pellets of polycrystalline powder could be doped more rapidly, with an apparent diffusion coefficient of 7 × 10⁻⁸ cm²s⁻¹. X-ray susceptibility analysis show extensive disordering occurs on heavy Li doping, with a first-order transition from a crystalline/superconducting to an amorphous/non-superconducting phase. Single, crystals of Bi₂Sr₂Ca₁Cu₂O₈ exhibited a color change on reduction from metallic gray to golden bronze. The reduced material was highly air-sensitive, forming a hydroxide surface film on exposure to ambient atmosphere.     

1H and 13C NMR signal assignment of cucurbitacin derivatives from Citrullus colocynthis (L.) Schrader and Ecballium elaterium L. (Cucurbitaceae)

2D NMR-derived 1H and 13C NMR signal assignments of six structurally closely related cucurbitacin derivatives are presented. The investigated 2-O-beta-D-glucopyranosylcucurbitacins I, J, K, and L were obtained from Citrullus colocynthis (L.) Schrader whereas the aglyca cucurbitacin E and I were isolated from Ecballium elaterium L.     

Aglairubine: Structure Revision of a Chemotaxonomically Interesting Bisamide in Aglaia (Meliaceae)

 The bisamide aglairubine was isolated from different Aglaia species. The original structure was revised on the basis of FDMS and 2D-NMR data. Since all isolates were obtained from species belonging to the section Amoora of the genus Aglaia, aglairubine might serve as a taxonomic marker.     

Eine Sicherheitspipette

Analytical and Bioanalytical Chemistry -     

Characterization and optimization of liquid electrodes for lateral dielectrophoresis

Using the concept of insulator-based "electrodeless" dielectrophoresis, we present a novel geometry for shaping electric fields to achieve lateral deviation of particles in liquid flows. The field is generated by lateral planar metal electrodes and is guided along access channels to the active area in the main channel. The equipotential surfaces at the apertures of the access channels behave as vertical "liquid" electrodes injecting the current into the main channel. The field between a pair of adjacent liquid electrodes generates the lateral dielectrophoretic force necessary for particle manipulation. We use this force for high-speed deviation of particles. By adding a second pair of liquid electrodes, we focus a particle stream. The position of the focused stream can be swept across the channel by adjusting the ratio of the voltages applied to the two pairs. Based on conformal mapping, we provide an analytical model for estimating the potential at the liquid electrodes and the field distribution in the main channel. We show that the simulated particle trajectories agree with observations. Finally, we show that the model can be used to optimize the device geometry in different applications.     

Conventional sample enrichment strategies combined with high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance analysis allows analyte identification from a single minuscule Corydalis solida plant tuber

Identification of putative biomarker molecules within the genus Corydalis (Papaveraceae) was pursued by combining conventional off-line sample enrichment with high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance (HPLC-SPE-NMR) based structure elucidation. Off-line reversed phase solid phase extraction (SPE) was used to enrich the desired analytes from a methanolic extract (93 mg dry weight) of a miniscule single tuber (233 mg dry weight) of C. solida. An aliquot of the SPE fraction (2.1 mg) was subjected to separation in the HPLC-SPE-NMR hyphenation. Chromatographic peaks bearing the metabolites under investigation were trapped in the SPE device in a single experiment and transferred to a 600 MHz NMR spectrometer equipped with a 30 microl cryofit insert fed into a 3 mm cryoprobe. Recorded homo- and heteronuclear 1D and 2D NMR data allowed the identification of the three analytes under investigation as protopine, allocryptopine, and N-methyl-laudanidinium acetate. The latter is a rare alkaloid, which has been isolated only once before.