Simple preparation of baicalin from Scutellariae Radix

A simple, rapid and reproducible method was developed to isolate high-purity baicalin from Scutellariae Radix, the dried roots of Scutellaria baicalensis Georgi. The method involves partition/recrystallization steps without repeated column chromatography or special instruments. Isolated baicalin was characterized by comparisons of TLC, HPLC, IR, MS, and NMR data with an authentic sample. Moreover, beta-glucuronidase hydrolysis of baicalin sequentially yielded glucuronic acid and baicalein as confirmed by co-TLC with authentic samples. The purity of baicalin was more than 97% with yield ca. 8.7% (w/w). The method presented here appears suitable for commercial application.     

RAMA stain: A fast,sensitive and less protein‐modifying CBB R250 stain

SDS‐PAGE and CBB staining are two of the most popular methods used for protein analysis. Although many reports that describe such staining methods have been published, these conventional protocols require several hours or days for staining and de‐staining. In this study we describe a recently developed, fast and sensitive CBB staining method that utilizes the staining solution of RAMA that consists of the low‐cost reagents: CBB R250, acetic acid, methanol and ammonium sulfate, and the destaining solution of water. Our method dose dependently detects 12 nanograms protein within 60 min and with a wide protein spectrum. Although the features of the dose‐dependent relationship depend upon protein amounts and protein types, for most of the protein samples tested, a linear relationship was observed in the region from 12 to 330 ng. Moreover, through further washing, the detection sensitivity of protein is enhanced and reaches a maximum at 1.4 ng and then gradually decreases in the de‐staining process. It has been shown recently through MS analyses that the sensitive colloidal CBB staining methods frequently result in artifactual methylations due to the strong acid and long contact during staining and the destaining processes. Such artifacts were reported to be reduced by the replacement of strong inorganic acid with acetic acid and because RAMA utilizes acetic acid and is in contact with the proteins for a short time during staining and de‐staining, it is expected that in vitro artifacts will be reduced. Finally, MS analyses of RAMA‐stained protein bands were revealed not to have been methylated.     

Sensitive determination of 4-(4-chlorophenyl)-4-hydroxypiperidine, a metabolite of haloperidol, in a rat biological sample by HPLC with fluorescence detection after pre-column derivatization using 4-fluoro-7-nitro-2,1,3-benzoxadiazole

4-(4-Chlorophenyl)-4-hydroxypiperidine (CPHP), one of the metabolites of haloperidol, is considered to exhibit brain toxicity. CPHP concentrations in plasma and tissue homogenates (each 200 microL) from rats were analyzed by HPLC fluorescence detection after pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F). After basic extraction of the samples with benzene, the derivatization with NBD-F was conducted in borate buffer (pH 8.0) at 60 degrees C for 3 min. Mexiletine was carried through the procedure as an internal standard. The regression equation for CPHP showed a good linearity in the range of 0.03-1 microg/mL with a detection limit of 0.008 microg/mL. The coefficient of variation was less than 11.6%. Plasma concentration-time courses of CPHP after intraperitoneal or per oral administration of CPHP, haloperidol or reduced haloperidol were examined, and the pharmacokinetic parameters were estimated. Additionally, CPHP levels in various tissues at 8 h after intraperitoneal administration of these compounds were compared. The method was simple and sensitive, useful for determination of CPHP in rat biological samples using as little as 200 microL of sample volume and could be applied for pharmacokinetic study.     

Infrared predissociation spectroscopy of ammonia cluster cations (NH3)n+ (n=2-4) produced by vacuum-ultraviolet photoionization

Infrared predissociation spectroscopy of vacuum ultraviolet-pumped ion (IRPDS-VUV-PI) is performed on ammonia cluster cations (NH3)n+ (n=2-4) that are produced by VUV photoionization in supersonic jets. The structures of (NH3)2+ and (NH3)4+ are determined through the observation of infrared spectra and vibrational calculations based on ab initio calculations at the MP2/6-31G** and 6-31++G** levels. (NH3)2+ is found to be of the "hydrogen-transferred" form having the (H3N+-...NH2) composition. In contrast, (NH3)4+ exhibits the "head-to-head" dimer cation (H3...NH3+ core structure, where the positive charge is shared between two ammonia molecules in the core, and two other molecules are hydrogen bonded onto the core. An unequivocal assignment of the infrared spectrum of (NH3)3+ has not been achieved, because the presence of two isomeric structures could be suggested by the observed spectrum and theoretical calculations.     

52 mJ narrow-bandwidth degenerated optical parametric system with a large-aperture periodically poled MgO:LiNbO3 device

We have demonstrated efficient, high-energy, narrow-spectral-bandwidth 2.128 microm pulse generation by use of periodically poled MgO:LiNbO3 devices with a 36 mm length and a 5 mm x 5 mm large aperture. A free-running degenerated optical parametric oscillator (OPO) pumped with a Q-switched 1.064 microm Nd:YAG laser exhibits a high slope efficiency of 75% and an optical-to-optical conversion efficiency of 70% with a broad spectral bandwidth (>100 nm). In a configuration with a spectrally narrowed master oscillator followed by a power amplifier, we have achieved an output pulse energy of 52 mJ with a spectral bandwidth of less than 2 nm at the degeneracy point. The total optical-to-optical conversion efficiency of the system reached 50%.     

Static magnetic order in metallic K0.49CoO2

By means of muon-spin spectroscopy, we have found that K0.49CoO2 crystals undergo successive magnetic transitions from a high-T paramagnetic state to a magnetic ordered state below 60 K and then to a second ordered state below 16 K, even though K0.49CoO2 is metallic at least down to 4 K. An isotropic magnetic behavior and wide internal-field distributions suggest the formation of a commensurate helical spin density wave (SDW) state below 16 K, while a linear SDW state is likely to exist above 16 K. It was also found that exhibits a further transition at 150 K presumably due to a change in the spin state of the Co ions. Since the dependence of the internal-field below 60 K was similar to that for Na0.5CoO2, this suggests that magnetic order is more strongly affected by the Co valence than by the interlayer distance or interaction and/or the charge ordering.     

Size and viscoelasticity of spatially confined multilamellar vesicles

We studied viscoelastic properties and scaling behavior of multilamellar vesicles (MLVs) confined between two parallel plates as a function of the shear rate and sample thickness (gap size between parallel plates). The rheological properties are classified into two regimes; the shear-thinning regime at high shear rates and the shear-thickening regime at low shear rates. In the former, the MLV radius results from the mechanical balance between the effective surface tension σ_eff and viscous stress force. The MLV radius is independent of the gap size. σ_eff estimated by van der Linden model is 2.1 ±0.15 ×10^-4 Nm^-1 corresponding to the same value obtained by SANS measurement. Power law exponents for the steady state viscosity and yield stress against pre-shear rate ( , ) well agree with prediction based on the layering of membranes. Therefore, viscoelastic properties in this regime could be modeled by assuming that the dynamics of MLVs are driven by layering of MLV polydomains, which could be accompanied by the viscous dissipation, i.e., the stress relaxation on the MLV, induced by continuous sequence of yields of MLVs. The flow curve is empirically explained by the assumption of a relaxation time for the MLV shape. In the latter, however, scaling laws observed in the shear-thinning regime break down. The MLV radius increases when the gap size is reduced below the threshold value and MLV is no longer formed at very small gap sizes. Different dynamics from the shear-thinning regime seem to dominate the viscoelasticity.     

Investigation of uterine peristalsis diurnal variation

BACKGROUND: In women of reproductive age, wavelike movements of the subendometrial myometrium, which is called uterine peristalsis, is considered to be related with fertility and menstrual problems. This is because the direction and frequency of peristalsis is known to be different among menstrual cycle phases. However, nothing is known as regarding diurnal variations. This study was designed to evaluate for the presence of a diurnal variation in uterine peristalsis. MATERIALS AND METHODS: MR studies were performed on 12 volunteers of reproductive age using a 1.5-T magnet, four times per day (at 0800, 1300, 1800 and 2300 h) during three (periovulatory, luteal and menstrual) phases of one menstrual cycle. Sixty images were obtained by half-Fourier acquisition single-shot turbo spin echo every 2 s and displayed on cine mode. Semiautomated software was utilized to discern the presence of peristaltic waves, as well as peristaltic frequency and direction. The presence of sustained contractions was visually determined. RESULTS: There was no statistically significant difference during the daytime for frequency and direction of uterine peristalsis for all menstrual cycle phases. Nonetheless, peristaltic frequency and direction fluctuated during each cycle. Statistically significant peristaltic suppression was observed in association with sustained contractions during the periovulatory phase. CONCLUSIONS: A diurnal variation was not observed for uterine peristalsis. Sporadic changes in peristaltic frequency were observed and appear to be closely related to sustained uterine contractions.     

Cerium isotope effects in Ce(III) malate and lactate complex formation studied by long-distance displacement chromatography

Isotope effects of cerium were observed in malate and lactate complex formations during the long-distance displacement chromatographic processes at 313 K. Heavier isotopes were found fractionated in the frontal edges of the Ce adsorption bands in both the systems, registering a preference of the heavier isotopes for the Ce(III) complexes in the solution phase over the simply hydrated Ce(III) ions in the resin phase. The fractionation coefficients epsilon for the 136Ce/140Ce, 138Ce/140Ce and 142Ce/140Ce isotopic pairs were 7.1 x 10(-6), 5.2 x 10(-6) and -2.1 x 10(-6) for the malate system, and 4.8 x 10(-6), 4.5 x 10(-6) and-2.6 x 10(-6) for the lactate system, respectively. They all show the mass-dependent law if the deviation of epsilon for the 138Ce/140Ce pair was considered merely due to the isobaric interference in Ce isotopic ratio measurements, suggesting the molecular vibration, rather than the nuclear field shift, mainly contributes to the Ce isotope effects in the complex formation systems. The absolute values of epsilon between the two systems are comparable, suggesting no instinct difference in structural properties between Ce malate and lactate complexes involved.     

Preparation of single-crystalline ZnO films on ZnO-buffered a-plane sapphire by chemical bath deposition

High-quality zinc oxide (ZnO) films were successfully grown on ZnO-buffered a-plane sapphire (Al₂O₃ (1 1 2¯ 0)) substrates by controlling temperature for lateral growth using chemical bath deposition (CBD) at a low temperature of 60 °C. X-ray diffraction analysis and transmission electron microscopy micrographs showed that the ZnO films had a single-crystalline wurtzite structure with c-axis orientation. Rocking curves (ω-scans) of the (0 0 0 2) reflections showed a narrow peak with full width at half maximum value of 0.50° for the ZnO film. A reciprocal space map indicated that the lattice parameters of the ZnO film (a=0.3250 nm and c=0.5207 nm) were very close to those of the wurtzite-type ZnO. The ZnO film on the ZnO-buffered Al₂O₃ (1 1 2¯ 0) substrate exhibited n-type conduction, with a carrier concentration of 1.9×10¹⁹ cm⁻³ and high carrier mobility of 22.6 cm² V⁻¹ s⁻¹.