Synthesis and properties of new materials with banana-shaped achiral cores and chiral end groups

New chiral bent-core mesogens, derivatives of 1,3-phenylene bis[4-(alkanyloxyphenyliminomethyl)benzoate], were synthesized with variation of a substituent (X=F, Cl); their antiferroelectric properties are described. The mesomorphic and switching properties were characterized by differential scanning calorimetry, polarizing optical microscopy, triangular wave method, and X-ray diffractometry in the small and wide angle regions. The presence of chiral tails at the terminals of side wings in the bent-core molecules induced a decrease in transition temperature and formation of the switchable SmC* phase in the melt. In addition, the introduction of a lateral halogen substituent in the Schiff's base moiety prevented the regular stacking of the molecules, resulting in the formation of very complex optical textures. The smectic phase with F-substituted PBFDOB and Cl-substituted PBCDOB showed layer spacings of 39 and 38.5?Å, respectively, corresponding to the end-to-end distance of molecules with a bent conformation. Significantly, the smectic phases of PBFDOB and PBCDOB exhibited a period of 179.5 and 131?Å, respectively, compatible with a helical structure with periodicity about 4.6 and 3.4 times the layer spacings.     

尿素法合成高结晶度类水滑石

尿素的高温分解特性被用于控制层状化合物合成过程中的pH值。室温下尿素可与硝酸盐形成均一溶液，当其高温分解时可以保证溶液内部各点的pH值始终一致，因而可获得高结晶度的水滑石样品。利用该法可合成出Mg-Al、Zn-Al及Ni-Al类水滑石，但难以合成出Co-Al，Mn-Al及Co-Cr类水滑石，相信这与不同金属离子发生沉淀时所需的pH值有关。     

Effect of heat treatment on ZrO2-embedded electrospun carbon fibers used for efficient electromagnetic interference shielding

ZrO₂-embedded carbon fibers were prepared for use as an electromagnetic interference (EMI) shielding material by electrospinning and heat treatment methods. Structural changes were observed in the ZrO₂ and in the carbon structures by XRD and Raman spectroscopy, respectively. During heat treatment, XRD analysis results revealed a transition from a monoclinic structure to a tetragonal structure in ZrO₂ and a graphitization in the structural formation of carbon fibers was observed by Raman spectroscopy. It was observed that these structural changes in the ZrO₂ and the carbon fibers improved the real and imaginary permittivities by a factor of more than 3.5. The EMI shielding efficiency (SE) improved along with the permittivity with higher treatment temperatures and greater amounts of embedded ZrO₂; the highest average EMI SE achieved was 31.79 dB in 800-8500 MHz. The heat treatment played an important role in the improvements in the permittivity and in the EMI SE because of the heat-induced structural changes of the ZrO₂-embedded electrospun carbon fibers. We suggest that the EMI shielding of the fibers is primarily due to the absorption of electromagnetic waves, which prevents secondary EMI by reflection of electromagnetic waves.     

A Sensitive and Selective LC-MS Method for the Determination of Lurasidone in Rat Plasma,Bile, and Urine

A liquid chromatography-mass spectrometry (LC-MS) assay was developed and validated for the quantification of lurasidone, an atypical antipsychotic drug, in rat plasma, bile, and urine. Rat plasma, bile, or urine samples were processed by liquid–liquid extraction and injected onto an LC-MS system for the quantification of lurasidone and ziprasidone (an internal standard). Lurasidone and ziprasidone were separated from endogenous substances using a Gemini C6-Phenyl column with mixture of acetonitrile and 0.1 % formic acid (80:20, v/v) as the mobile phase. Quantification was performed using the selected ion monitoring mode at m/z 493 for lurasidone and m/z 413 for the IS. The detector response was specific and linear for lurasidone in the concentration range 5–5,000 ng mL⁻¹ The intra- and inter-day accuracy and precision of the method were determined to be within the acceptable criteria for assay validation guidelines. In addition, lurasidone was stable under a variety of processing and handling conditions. Lurasidone concentrations could be readily measured in rat plasma, bile, and urine samples up to 24 h after an intravenous or oral administration, suggesting that the assay can be used in pharmacokinetic studies of lurasidone in rats.

     

Analysis of a queueing system with a general service scheduling function,with applications to telecommunication network traffic control

In this paper we analyze a queueing system with a general service scheduling function. There are two types of customer with different service requirements. The service order for customers of each type is determined by the service scheduling function α_k(i, j) where α_k(i, j) is the probability for type-k customer to be selected when there are i type-1 and j type-2 customers. This model is motivated by traffic control to support traffic streams with different traffic characteristics in telecommunication networks (in particular, ATM networks). By using the embedded Markov chain and supplementary variable methods, we obtain the queue-length distribution as well as the loss probability and the mean waiting time for each type of customer. We also apply our model to traffic control to support diverse traffics in telecommunication networks. Finally, the performance measures of the existing diverse scheduling policies are compared. We expect to help the system designers select appropriate scheduling policy for their systems.     

Asymptotic behaviors for partial sum processes of a Gaussian sequence

We establish some large increment results for partial sum processes of a dependent stationary Gaussian sequence via estimating upper bounds of large deviation probabilities on suprema of the Gaussian sequence.     

Spreader-CDR system for efficient,reproducible, and frugal western blot

Efficient antibody incubation is a vital step for successful western blot. During the incubation, a thin antibody-depleted layer is created around the blotting membrane, which limits antibody binding. Although the conventional batch shaking method is ineffective against it, this layer can be easily disrupted by cyclic draining and replenishing (CDR) of the antibody solution during membrane incubation. Previously, we introduced a closed and rotating cylindrical chamber as a tool to implement CDR for western blots (rCDR). A new open bucket-style chamber was devised for easier operation and the possibility of process automation. Instead of rotation as in rCDR, rocking it back and forth achieved the CDR antibody incubation (R-CDR). The chamber was then equipped with a spreader-rod to facilitate the uniform movement of the antibody solution across the membrane surface. Hence, it was named spreader CDR (S-CDR). Compared to the batch incubation method, both the S-CDR and R-CDR devices produced significantly enhanced signals and developed faster results. There were several additional benefits of using the spreader-rod, which included uniform antibody binding across the membrane, reduced usage of antibodies, and the ability to recover results even from mishandled, creased membranes. The S-CDR device ensures better blots and can be easily implemented in existing western blot protocols.     

Flow injection microbial trichloroethylene sensor

A flow type microbial biosensor for direct measurement of trichloroethylene (TCE) was developed. The unique features of this novel microbial sensor were the use of the TCE degrading bacterium Pseudomonas aeruginosa JI104, the electrical detection of the chloride ion released by microbial degradation, and flow cell made of glass. Glass cell was used in order to suppress adsorption of TCE and made a closed reaction cell. Vaporization of TCE during the measurement was prevented using closed flow cell. The performance of the sensor was evaluated from following aspects; such as pH of the carrier solution, amount of the immobilized microbe, flow rate and injection volume. The sensor signals were linearly proportional to the concentration of TCE in the range from 0.03 to 2 mgl(-1), which is suitable for the determination of suspected samples to be drinkable water or not. The sensor performance was checked on the real sample, and this system showed good response in ground water, indicating its applicability for the on line monitoring at TCE contaminated areas or hazardous sites.     

Quantification of lurasidone, an atypical antipsychotic drug, in rat plasma with high-performance liquid chromatography with tandem mass spectrometry

A liquid chromatography–tandem mass spectrometric (LC/MS/MS) method was developed for the determination of an atypical antipsychotic drug, lurasidone, in rat plasma. The method involves the addition of acetonitrile and ziprasidone (internal standard) solution to plasma samples, followed by centrifugation. An aliquot of the supernatant was diluted with water and directly injected into the LC/MS/MS system. The separations were performed on a column packed with octadecylsilica (5 μm, 2.0 × 50 mm) with 0.1% formic acid and 0.1% formic acid in acetonitrile as mobile phase and the detection was performed using tandem mass spectrometry by multiple‐reaction monitoring via an electrospray ionization source. The standard curve was linear (r = 0.9982) over the concentration range 0.002–1 μg/mL. The intra‐ and inter‐assay precisions were 1.7 and 8.6%, respectively. The accuracy range was from 90.3 to 101.8%. The lower limit of quantification was 2.0 ng/mL using 50 μL of rat plasma sample. The developed analytical method was successfully applied to the pharmacokinetic study of lurasidone in rats. Copyright © 2011 John Wiley & Sons, Ltd.     

Synthesis and mesomorphic properties of banana-shaped achiral molecules with central and lateral halogen substituents

Three banana-shaped achiral compounds, derivatives of 4-chloro-1,3-phenylene bis[4-(4-n-decanyloxyphenyliminomethyl)benzoate], were synthesized with variation of a substituent (X=H, F, or Cl); their antiferroelectric properties are described. The mesomorphic and switching properties were characterized by polarizing optical microscopy, differential scanning calorimetry, triangular wave method, and X-ray diffraction. The introduction of a lateral halogen substituent in the Schiff's base moiety prevents the regular stacking of the molecules, resulting in a decrease of melting temperature and leads to formation of the switchable SmC* phase in the melt. All of the compounds showed antiferroelectric switching, and their values of spontaneous polarization on reversal of an applied electric field were 260, 480, and 300 nC cm^-2, respectively, for X=H, F and Cl.