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1.
HPLC with fluorescence detection assay of perampanel,a novel AMPA receptor antagonist,in human plasma for clinical pharmacokinetic studies
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Perampanel (Fycompa®), a novel α‐amino‐3‐hydroxy‐5‐methyl‐4‐isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥12 years) with refractory partial‐onset seizures. To support therapeutic drug monitoring, a simple high‐performance liquid chromatography (HPLC) assay with fluorescence detection was developed to determine perampanel concentrations in human plasma and validated to support clinical trials. Human plasma samples (1.0 mL) were processed by liquid extraction using diethyl ether, followed by chromatographic separation on a YMC Pack Pro C18 column (150 × 4.6 mm i.d., 5 µm) with isocratic elution of acetonitrile–water–acetic acid–sodium acetate (840:560:3:1.8, v/v/v/w) at a flow rate of 1.0 mL/min. Column eluent was monitored at excitation and emission wavelengths of 290 and 430 nm, respectively. The assay was linear (range 1.0–500 ng/mL) and this could be extended to 25 µg/mL by 50‐fold dilution integrity. No endogenous peaks were detected in the elution of analytes in drug‐free blank human plasma from six individuals and no interference was observed with co‐medications tested. Intra‐ and inter‐batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria of bioanalytical guidelines. Validation data demonstrated that our assay is simple, selective, reproducible and suitable for therapeutic drug monitoring of perampanel. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
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Kohji Masaki Shin-ichi Ohkawara Tomohiro Hirano Makiko Seno Tsuneyuki Sato 《Journal of polymer science. Part A, Polymer chemistry》2004,42(17):4437-4447
The crosslinking reaction of 1,2-polybutadiene (1,2-PB) with dicumyl peroxide (DCPO) in dioxane was kinetically studied by means of Fourier transform near-infrared spectroscopy (FTNIR). The crosslinking reaction was followed in situ by the monitoring of the disappearance of the pendant vinyl group of 1,2-PB with FTNIR. The initial disappearance rate (R0) of the vinyl group was expressed by R0 = k[DCPO]0.8[vinyl group]−0.2 (120 °C). The overall activation energy of the reaction was estimated to be 38.3 kcal/mol. The unusual rate equation was explained in terms of the polymerization of the pendant vinyl group as an allyl monomer involving degradative chain transfer to the monomer. The reaction mixture involved electron spin resonance (ESR)-observable polymer radicals, of which the concentration rapidly increased with time owing to a progress of crosslinking after an induction period of 200 min. The crosslinking reaction of 1,2-PB with DCPO was also examined in the presence of vinyl acetate (VAc), which was regarded as a copolymerization of the vinyl group with VAc. The vinyl group of 1,2-PB was found to show a reactivity much higher than 1-octene and 3-methyl-1-hexene as model compounds in the copolymerization with VAc. This unexpectedly high reactivity of the vinyl group suggested that an intramolecular polymerization process proceeds between the pendant vinyl groups located on the same polymer chain, possibly leading to the formation of block-like polymer. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 4437–4447, 2004 相似文献
4.
Squier (1987) showed that if a monoid is defined by a finite complete rewriting system, then it satisfies the homological
finiteness condition FP3, and using this fact he gave monoids (groups) which have solvable word problems but cannot be presented by finite complete
systems. In the present paper we show that a monoid cannot have a finite complete presentation if it contains certain special
elements. This observation enables us to construct monoids without finite complete presentation in a direct and elementary
way. We give a finitely presented monoid which has (1) a word problem solvable in linear time and (2) linear growth but (3)
no finite complete presentation. We also give a finitely presented monoid which has (1) a word problem solvable in linear
time, (2) finite derivation type in the sense of Squier and (3) the property FP∞, but (4) no finite complete presentation. 相似文献
5.
Sohei Okazaki Noriaki Okazaki Hidetaka Sugaya Ryota Takahashi Yuji Matsumoto Hideomi Koinuma Tetsuya Hasegawa 《Applied Surface Science》2006,252(7):2615-2621
We developed a scanning microwave microscope (SμM) designed for high-throughput electric-property screening as well as for rapid construction of electronic phase diagrams at low temperatures. As a sensor probe, we used a high-Qλ/4 coaxial cavity resonator to which a thin needle with ball-tip end was attached. The sensor module was mounted on the low-temperature XYZ stage, which allowed us to map out the change of resonance frequency and quality factor due to the local tip-sample interaction at low temperatures. From the measurements of combinatorial thin films, such as Ti1−xCoxO2−δ and Nd0.9Ca0.1Ba2Cu3O7−δ (NCBCO), it was demonstrated that this SμM system has enough performance for the high-throughput characterization of sample conductance under variable temperature conditions. 相似文献
6.
High-performance liquid chromatography was used to determine cyclosporin A (CsA) concentrations in the serum of kidney transplant patients by rapid-flow fractionation (RFF) followed by silica gel normal-phase high-performance liquid chromatography (HPLC). The extraction of CsA from serum was achieved by RFF using a short diatomaceous earth column eluted with diethyl ether-n-hexane (50:50, v/v). The recovery was more than 80% at concentrations of 50-150 micrograms/l. The concentration of this compound was determined by HPLC using a conventional silica gel column with 3.3 M ammonia solution-ethanol-n-hexane (0.31:10.69:89, v/v) as eluent. Concentration calibration was made on the basis of the peak-height ratio of CsA to CsD as the internal standard. The coefficient of variation of this assay was less than 6.5% and the results were used for the therapeutic drug monitoring of CsA administered to kidney transplant patients. Measurements of the CsA concentrations in 160 serum specimens were also made by conventional radioimmunoassay (RIA) using commercial kits. The data obtained by RIA were on average 2.5 times those obtained by HPLC. Higher values in RIA were observed characteristically with patients with severe disfunction resulting from CsA hepatotoxicity. From the results, it appeared that HPLC rather than RIA provides more precise and reliable values for the concentration of this drug. 相似文献
7.
The effect of the cation concentration, hydrolysis temperature, and composition in the CeO2–ZrO2 system on the direct precipitation of ceria–zirconia solid solutions and the structure of the precipitates from acidic aqueous solutions of (NH4)2Ce(NO3)6 and ZrOCl2 by hydrolysis under hydrothermal conditions were investigated. Nanometer-sized (8–10 nm) ceria–zirconia solid solution particles in a composition range of 0 to 60 mol% ZrO2 were directly precipitated from the solutions with total metal cation concentration less than 0.2 mol/dm3 by simultaneous thermal hydrolysis at 150–240°C. The crystalline phase of the precipitates gradually changed from cubic and/or tetragonal to monoclinic with increasing the cation concentration of the solution from 0.2 to 0.8 mol/dm3 at the starting composition of 50 mol% ZrO2 under hydrolysis condition of 150°C for 48 h, which was attributed to decrease in the supply of hydrolyzed Ce component caused by decrease in the hydrolysis ratio of (NH4)2Ce(NO3)6. Ceria–zirconia solid solutions containing large amount of ZrO2 maintained high specific surface area and small-sized crystallite after heat-treatment at 900–1000°C for 1 h. 相似文献
8.
Low-loss and rugged distal tips for CO2 laser have been proposed and fabricated based on a commercially available stainless steel (St) pipe. A method of smoothening the inner surface of the St pipe with a rough inner surface is put forward. Fabrication parameters, transmission properties, and mechanical strength of the cyclic olefin polymer-coated silver hollow St distal tip are experimentally discussed. 相似文献
9.
Polyethylene oxide (PEO) based polymer electrolytes with BaTiO3 as filler and Li(C2F5SO2)2N as salt have been examined in lithium polymer batteries. The aluminum disolution potential in PEO-Li(C2F5SO2)2N was estimated to be 4.1 V vs. Li/Li+ at 80 °C, which was compared to that of 3.8 V vs. Li/Li+ in PEO-Li(CF3SO2)2N. The electrical conductivity of the system was measured as a function of O/Li ratio. The highest conductivity was observed
in O/Li=8. The conductivity was 1.65×10−3 S/cm at 80 °C and 1.5×10−5 S/cm at 25 °C. The interfacial resistance of Li/polymer electrolyte/Li annealed at 80 °C for 15 days was lower than 100 Ωcm2.
Paper presented at the 8th EuroConference on Ionics, Carvoeiro, Algarve, Portugal, Sept. 16 – 22, 2001. 相似文献
10.
Oxide heterojunctions made of p-type La0.8Sr0.2MnO3 (LSMO) and niobium-doped n-type SrTiO3 (STO:Nb) have been fabricated by the pulsed laser deposition (PLD) technique and characterized under UV light irradiation by measuring the current-voltage, photovoltaic properties and the junction capacitance. It is shown that the heterojunctions work as an efficient UV photodiode, in which photogenerated holes in the STO:Nb substrate are injected to the LSMO film. The maximum surface hole density Q/e and external quantum efficiency γ are estimated to be 8.3×1012 cm−2 and 11% at room temperature, respectively. They are improved significantly in a p-i-n junction of LSMO/STO/STO:Nb, where Q/e and γ are 3.0×1013 cm−2 and 27%, respectively. 相似文献