Monolithic spin column: a new extraction device for analysis of drugs in urine and serum by GC/MS and HPLC/MS

A monolithic spin column was developed for the extraction of analytes from biological materials. This column was constructed by packing a monolithic silica disk into a spin column. Sample loading, washing, and elution of the target drugs were accomplished simply by centrifugation of the column. Opiates and benzodiazepines are abused throughout the world. Identification and quantification of these drugs is very important to solve crimes or the cause of death. Three opiates (morphine, codeine, and dihydrocodeine) were extracted from urine and serum by using the column. After conversion to trimethylsilyl derivatives of the opiates by vigorous mixing with the derivatizing reagent, the solution was subjected to GC/MS. A linear curve was observed for opiates from 10 to 2500 ng/mL in urine and 5 to 1200 ng/mL in serum, respectively (correlation coefficient > 0.996). For benzodiazepines, the hydroxyl metabolites of triazolam and etizolam were extracted from urine using the column, and the eluate was directly analyzed by HPLC/MS without evaporation. The LOD values were at the ppb level, with RSD values lower than 15%. The proposed methods were successfully applied to clinical and forensic cases, and good agreement of results was obtained compared to conventional methods.     

Isokinetic trunk and knee muscle strengths and gait performance in walking patients with T-cell lymphotropic virus type 1-associated myelopathy/ tropical spastic paraparesis (HAM/TSP)

The aim of this study was to investigate the isokinetic trunk and knee muscle strengths, and examine the clinical relevance of dynamic muscle strengths and gait performance in walking patients with human T-cell lymphotropic virus type 1-associated myelopathy/ tropical spastic paraparesis (HAM/TSP). Thirteen patients with HAM/TSP (8 females and 5 males, aged 38–76) and 13 sex- and age-matched healthy control subjects participated in the study. We assessed gait speed, stride length, cadence; and maximal isokinetic torque of trunk and knee extensors and flexors at 30°/s, 60°/s and 90°/s using a Biodex System 3 dynamometer. Furthermore, we calculated the isokinetic trunk extensor/flexor (E/F) and hamstrings/quadriceps (H/Q) strength ratios (parameter of the muscle strength balance about the trunk and knee joint). Compared with the age-matched controls, the patients with HAM/TSP had significantly reduced gait speed, stride length and cadence (P < 0.05). Peak torque values related to body weight (PTBW) were significantly reduced, especially for the knee flexors (P < 0.05). For the knee extensors, the PTBW values were significantly reduced at an increased angular velocity (P < 0.05). The PTBW of knee flexors was positively correlated with gait speed and cadence in the patients with HAM/TSP. The H/Q ratio but not E/F ratio was significantly decreased compared with the control. Our results indicated that the isokinetic trunk and knee muscle performance had reduced from the ambulatory stage, and suggested the deterioration in knee muscle performance to be associated with gait disturbance in walking HAM/TSP patients.     

High-energy, broadly tunable, narrow-bandwidth mid-infrared optical parametric system pumped by quasi-phase-matched devices

We have developed a tunable, narrow-bandwidth (<2 cm(-1)) mid-infrared (MIR) optical parametric system with a large-aperture periodically poled Mg-doped LiNbO(3) (LA-PPMgLN)-based high-energy pump source. The system has a continuously tunable tuning range from 4.6 to 11.2 mum and produces a maximum output energy of 2.0 mJ at 5.1 mum. Practical use of the MIR source is demonstrated by MIR-UV double-resonance spectroscopy of jet-cooled acetanilide.     

Control of tribological properties of diamond-like carbon films with femtosecond-laser-induced nanostructuring

This paper reports tribological properties of diamond-like carbon (DLC) films nanostructured by femtosecond (fs) laser ablation. The nanostructure was formed in an area of more than 15 mm × 15 mm on the DLC surface, using a precise target-scan system developed for the fs-laser processing. The frictional properties of the DLC film are greatly improved by coating a MoS₂ layer on the nanostructured surface, while the friction coefficient can be increased by surface texturing of the nanostructured zone in a net-like patterning. The results demonstrate that the tribological properties of a DLC surface can be controlled using fs-laser-induced nanostructuring.     

Evolutionary Algorithm Directed Synthesis of Mixed Anion Compounds LaF2X (X=Br,I) and LaFI2

Mixed-anion compounds have attracted growing attentions, but their synthesis is challenging, making a rational search desirable. Here, we explored LaF₃-LaX₃ (X=Cl, Br, I) system using ab initio structure searches based on evolutionary algorithms, and predicted LaF₂X and LaFX₂ (X=Br, I), which are respectively isostructural with LaHBr₂ and YH₂I, consisting of layered La-F blocks with single and double ordered honeycomb lattices, separated by van der Waals gaps. We successfully synthesized these compounds: LaF₂Br and LaFI₂ crystallize in the predicted structure, while LaF₂I is similar to the predicted one but with different layer stacking. LaF₂I exhibits fluoride ion conductivity comparable to that of non-doped LaF₃, and has the potential to show better ionic conductivity upon appropriate doping, given the theoretically lower diffusion energy barrier and the presence of soft iodine anions. This study shows the structure prediction using evolutionary algorithms will accelerate the discovery of mixed-anion compounds in future, in particular those with an ordered anion arrangement.     

Biodegradable polymeric films based on microbial poly(3-hydroxybutyrate). Effect of gamma-radiation on mechanical properties and biodegradability

Two samples of microbial poly(3-hydroxybutyrate) (PHB) having different molecular weight were used for the preparation of films to be exposed to gamma radiation. The effect of radiation on those samples with high molecular weight increased the fragility of the film. Biodegradability increased with time and reached about 95% after 18 days. Weight-loss of both samples (irradiated and non-irradiated) after 23 days were 100%, for those films with molecular weight of 265 kD.     

Charge–discharge performances of Li–S battery using NaI–NaBH4–LiI solid electrolyte

Journal of Solid State Electrochemistry - In this study, Li–S batteries were fabricated using 9(15NaI∙NaBH4)∙LiI as the solid electrolyte, and their charge–discharge...     

Crystallization Control of Molten Ba(B0.9Al0.1)2O4 from Supercooled Pendant Drop

Crystallization process of molten Ba(B_0.9Al_0.1)₂O₄ from supercooled pendant drop was investigated on a viewpoint of a supercooling and a solid phase formation. Molten pendant drop was crystallized by a rod touching at an crystallization temperature under an adequate degree of supercooling. Three kinds of rods were used. Each rod was made of Pt, hBN and graphite which had different wettability to the molten drop. There were three kinds of phases on a solid Ba(B_0.9Al_0.1)₂O₄, such as a high temperature crystal phase, a low temperature crystal phase and a glass phase. All phases could be formed by the present method.