Cellulose dimethylphenylcarbamate-bonded carbon-clad zirconia for chiral separation in high performance liquid chromatography.

Porous zirconia particles are very robust material and have received considerable attention as a stationary phase support for HPLC. We prepared cellulose dimethylphenylcarbamate-bonded carbon-clad zirconia (CDMPCCZ) as a chiral stationary phase (CSP) for separation of enantiomers of a set of 14 racemic compounds in normal phase (NP) and reversed-phase (RP) liquid chromatography. Retention and enantioselectivity on CDMPCCZ were compared to those on CDMPC-coated zirconia (CDMPCZ) to see how the change in immobilization method of the chiral selector affects the retention and chiral selectivity. In NPLC, retention was longer and the number of resolved racemates was smaller on CDMPCCZ than on CDMPCZ. However, chiral selectivity factors for some resolved racemates were better on CDMPCCZ than on CDMPCZ. The longer retention on CDMPCCZ is likely due to strong, non-chiral discriminating interactions with the carbon layer on CDMPCZ. In RPLC only two racemates were resolved on CDMPCCZ, but retention times were shorter than, and resolutions were comparable to, those in NPLC, indicating a potential for improving chromatographic performance of the CDMPCCZ column in RPLC with optimized column preparation and separation conditions.     

A precision measurement of the hyperfine structure of87Sr+

The ground state hyperfine splitting of⁸⁷Sr⁺ was measured with a precision of 1×10^–8. The experiments were performed with an RF ion trap connected to an ISOL (isotope separator on-line), where all the possible transitions between Zeeman sublevels were observed by a laser-microwave double resonance method. The magnetic dipole hyperfine constant was determined to beA=–1 000 473.673 (11) kHz.     

Validation of a method for predicting the precision, limit of detection and range of quantitation in competitive ELISA.

The mathematical model for predicting the precision, limit of detection (LOD) and range of quantitation (ROQ) in a competitive enzyme-linked immunosorbent assay (ELISA) proposed by Hayashi et al. (Anal. Chem., 2004, 76, 1295) was validated. The model describes the relative standard deviation (RSD) of concentration estimates by the RSDs of pipetting volumes of analyte, enzyme-conjugated antigen, antibody and substrate solutions, and the standard deviation (SD) of inherent absorbances between the wells in an ELISA plate. For 6 kinds of direct competitive ELISA kits, the LOD and ROQ predicted by the model agreed well with those obtained by experiments with real samples. It was also confirmed that the model is applicable to the prediction of uncertainty that depends on the pipetting error of the viscous antiserum solution. The model was demonstrated to be useful for estimating the LOD and ROQ of competitive ELISA.     

Dicationic ((−)-sparteine)palladium-catalyzed enantioselective aldol reaction of aldehydes with 1-phenyl-1-trimethylsilyloxyethene, proceeding via a palladium enolate

A dicationic ((−)-sparteine)palladium complex underwent a superior catalytic enantioselective aldol reaction of aldehydes with 1-phenyl-1-trimethylsilyloxyethene performing satisfactorily, starting with ((−)-sparteine)PdCl₂ and AgSbF₆ as catalyst precursors (1 mol % loading) in the presence of 3 Å molecular sieves over the reaction.     

Laser spectroscopy of trapped 7Be and 10Be at a prototype slow RI-beam facility of RIKEN

A next-generation slow radioactive nuclear ion beam facility (SLOWRI) which provides slow, high-purity and small emittance ion beams of all elements is being build as one of the principal facilities at the RIKEN RI-beam factory (RIBF). High energy radioactive ion beams from the projectile fragment separator BigRIPS are thermalized in a large gas catcher cell. The thermalized ions in the gas cell are guided and extracted to a vacuum environment by a combination of dc electric fields and inhomogeneous rf fields (rf carpet ion guide). From there the slow ion beam is delivered via a mass separator and a switchyard to various devices: such as an ion trap, a collinear fast beam apparatus, and a multi-reflection time of flight mass spectrometer. In the R&D works at the present RIKEN facility, an overall efficiency of 5% for a 100A MeV ⁸Li ion beam from the present projectile fragment separator RIPS was achieved and the dependence of the efficiency on the ion beam intensity was investigated. Recently our first spectroscopy experiment at the prototype SLOWI was performed on Be isotopes. Energetic ions of ¹⁰Be and ⁷Be from the RIPS were trapped and laser cooled in a linear rf trap and the specific mass shifts of these isotopes were measured for the first time.     

Schottky metal library for ZNO-based UV photodiode fabricated by the combinatorial ion beam-assisted deposition

A binary alloy Schottky barrier diode on zinc oxide (ZnO) was developed using the combinatorial ion beam-assisted deposition system. The compositional fraction of the binary alloy was continuously varied using the composition-spread technique, to control the Schottky barrier height. After metal deposition, patterned Schottky diodes were fabricated on a ZnO single-crystal substrate. Pt-Ru alloy was selected from the work function viewpoint. Our experiments showed that the compositional fraction of the Schottky binary alloys changed continuously as designed and the Schottky barrier heights measured by current-voltage (I-V) measurements increased with increasing Pt content. Maximum barrier height difference for ZnO was 137 meV. Using ion beam deposition in parallel with the combinatorial system showed that the Schottky barrier heights for ZnO can be controlled by binary metal alloying.     

Mesomorphic properties of orthopalladated complexes of laterally substituted azobenzene derivatives, 2-alkoxycarbonyl-4-(4-ethoxyphenylazo)phenyl 4-methoxybenzoates

Homologous series of 2-alkoxycarbonyl-4-(4-ethoxyphenylazo)phenyl 4-methoxybenzoates (L) and their orthopalladated μ-chloro dimers (Pd₂Cl₂L₂) have been synthesized and their thermotropic phase transition behaviour has been characterized. The ligands, L, are three-ring nematogens with their central rings substituted in the 2-position by n-alkyl chains of varied length. The thermal stability of the nematic phases decreases rapidly with increasing side chain length and then levels off as the series is ascended. In every case the mesomorphic phase appears only over a small temperature range (less than 20° C). The orthopalladated species also proved to be nematogenic. Melting and clearing points rise on the average by 87° C and 126° C, respectively, and thus the temperature ranges of the nematic phases are enlarged considerably upon metallation. In relation to the observed stabilization of the nematic phases, particularly of higher homologues, a lath-like molecular structure, in which the side chains of the ligands fill up the clefts of the core part, has been deduced for a Pd2Cl2L2 homologue from its solution ¹H-NMR spectrum.     

Illuminating Molecular Processes in Living Cells

Lately, scientists have explored approaches to developing fluorescent and/or bioluminescent indicators to pinpoint cellular processes in single living cells. These analytical methods have become a key technology for visualizing and detecting what was otherwise unseen in live cells. The target signaling included second messengers, protein phosphorylations, protein–protein interactions, and protein localizations.     

Electrical conductance of solutions of lithium nitrate in 1,3-diaminopropane

Electrical conductances and densities of the LiNO₃-1,3-diaminopropane system have been measured as a function of composition and temperature. The results suggest that the solvent molecules may act as bridges between Li⁺ ions at higher concentration of LiNO₃.