Direct determination of benzamides in serum by column-switching high-performance liquid chromatography.

A column-switching high-performance liquid chromatographic method with fluorescence detection was developed for the simultaneous determination of four benzamide-type anti-psychotic drugs: sulpiride, tiapride, sultopride and metoclopramide in human serum. In this method, a TSKgel Super-ODS column was used as an analytical column, and a TSKgel G 2000SW was prepared as a pretreatment column. Under the optimized analytical conditions, four benzamide-type anti-psychotic drugs were eluted within 18 min. The detection limits (S/N = 3) for sulpiride, tiapride, sultopride and metoclopramide are 1 ng/ml, 4 ng/ml, 2 ng/ml and 0.5 ng/ml, respectively. Finally, the method was applied to the determination of sulpiride in human serum samples obtained after a single oral dose of sulpiride.     

Association Behavior of 4-Acylpyrazolone Derivative and Tertiary Amine of High Molecular Weight in Antagonistic Synergistic Extraction of Palladium

To find an effective extraction and removal method for palladium(II), which is one of the main fission products from an acidic nuclear spent fuel solution, the extraction behavior of palladium(II) from a nitric acid medium by an acidic chelating extractant, 1-phenyl-3-methyl-4-trifluoroacetylpyrazolone-5-one (HPMTP) and a tertiary amine of high molecular weight, tri-n-octylamine (TOA), has been studied by spectrophotometry. A noticeable antagonistic extraction effect was observed in the extraction system under the given conditions. To understand this phenomenon, a preliminary investigation was performed to explain the mechanism of this reaction. According to the theory of corresponding solutions (TCS), the association reaction between HPMTP and TOA is proposed in the organic phase. An associated species, HPMTP·TOA, formed through hydrogen bonding in a chloroform medium might be the main reason why an antagonistic extraction effect occurred. The association constant between HPMTP and TOA was calculated to be 2.86±0.05.     

Acoustic characteristics of Ni–Nb–Zr–H glassy alloys by ultrasonic shear waves

The propagation characteristics of shear horizontally polarized (SH) waves passing through (Ni₄₂Nb₂₈Zr₃₀)_100–x H_x (x = 0–15.2) glassy alloys were investigated as a function of hydrogen content. With an increase in hydrogen content, the propagation time and main frequency of the receiving waves show increase and decrease, respectively, indicating expan‐ sion in average atomic distance which comes from solution of hydrogen. In sharp contrast to crystalline alloys, the decrease in damping ratio and the delay in phase with increasing hydrogen suggest a strong settlement of hydrogen into four‐coordination sites surrounded tetrahedrally by four Zr atoms and the resulting increase in dynamic elasticity, respectively. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Second order evolution equations with time-dependent subdifferentials

We study an abstract second order nonlinear evolution equation in a real Hilbert space. We consider time-dependent convex functions and their subdifferentials operating on the first derivative of the unknown function. Introducing appropriate assumptions on the convex functions and other data, we prove the existence and uniqueness of a strong solution, and give some applications of the abstract theorem to hyperbolic variational inequalities with time-dependent constraints.      

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.     

Synthesis and properties of furo[4,3,2-de][1]benzopyran

A new heterocycle, furo[4,3,2-de][1]benzopyran ( 2 ), was synthesized. A key step in the sequence was the allylic bromination of 3,4-dihydrofuro[4,3,2-de][1]benzopyran ( 8 ) to give 3-bromo-3,4-dihydrofuro[4,3,2-de][1]-benzopyran ( 10 ) using N-bromosuccinimide under irradiation and high dilution conditions. Bromide 10 was dealt with 1,8-diazabicyclo[5.4.0]undec-7-ene to afford compound 2 . Several reactions of 2 were examined. Protonation of 2 in trifluoroacetic acid occurred at the 2-position to form a pyrylium ion 12 . Catalytic hydrogenation of 2 with palladium on charcoal proceeded smoothly to give 8 . Reduction of 2 by sodium and ethanol afforded 3-ethyl-4-hydroxybenzofuran ( 14 ). Electrophilic substitutions of 2 such as formylation, acetylation, and bromination, occurred easily at the 2-position. The above results show that compound 2 has both properties of benzofuran and 4-methylenepyran.     

Structurally isomeric two pyridino macrocycles: complexation and structures

Pyridine-based, structurally isomeric two macrocyclic compounds displayed a remarkably different complexation nature. The cage-type compound has an ideal structure for spherical cations, especially for the NH₄⁺ ion, but the reaction with some transition metals and Ln³⁺ produced its protonated species. On the other hand, its isomer formed complexes with alkali metals and lanthanides (1:1) and also with transition metals. Some structures of the complexes were clarified by crystallographic analyses.