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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
2.
Takashi Yoshitake Ryuji Iizuka Kaoru Fujino Osamu Inoue Kenji Yamagata Hitoshi Nohta Masatoshi Yamaguchi 《Analytical sciences》2004,20(12):1687-1690
An improved high-performance liquid-chromatographic (HPLC) assay for the simultaneous determination of serotonin (5-HT) and 5-hydroxyindole-3-acetic acid (5-HIAA) in human urine is reported. Following the automated precolumn derivatization of urinary 5-HT and 5-HIAA with benzylamine, the derivatives are separated by isocratic elution on a reversed-phase C18 semi-microbore column, and are fluorometrically detected at an excitation wavelength of 345 nm and an emission wavelength of 480 nm. The detection limits of 5-HT and 5-HIAA are 7 and 5 nmol/l in urine (0.7 and 0.5 fmol/20-microl injection). The proposed automatic method permits a highly selective and sensitive determination of 5-HT and 5-HIAA in human urine without any sample purification. 相似文献
3.
G. M. Luke L. P. Le B. J. Sternlieb Y. J. Uemura J. H. Brewer R. Kadono R. F. Kiefl S. R. Kreitzman T. M. Riseman C. E. Stronach M. Davis S. Uchida H. Takagi Y. Tokura Y. Hidaka T. Murakami E. A. Early J. T. Markert M. B. Maple C. L. Seaman 《Hyperfine Interactions》1991,63(1-4):311-317
We report muon spin relaxation/rotation measurements on sintered powder samples of Nd2−x
Ce
x
CuO4−y
and a large single crystal of Nd2CuO4−y
. We find an electronic phase diagram which is quite similar to that of hole-doped superconductors such as La2−x
Sr
x
CuO4−y
, although the doping of electrons into the system is less efficient in destroying the static moments on the copper spins.
Static magnetic order in Nd2CuO4−y
appears below about 250 K, and two spin reorientations are seen atT=75 K andT=35 K. Measurements of the magnetic field penetration depth have been unsuccessful due to the rare-earth paramagnetism of
these materials. 相似文献
4.
G. M. Luke L. P. Le B. J. Sternlieb Y. J. Uemura J. H. Brewer R. Kadono R. F. Kiefl S. R. Kreitzman T. M. Riseman C. L. Seaman Y. Dalichaouch M. B. Maple J. D. Garrett 《Hyperfine Interactions》1991,64(1-4):517-522
We have performed both zero field and high transverse field measurements at dilution refrigerator temperatures on a number of heavy electron systems, examining the superconducting and magnetic properties of these interesting materials. Among the materials studied to date are UBe13, URu2Si2 and U6Fe. The magnetic field penetration depth in the superconducting state of UBe13 is greater than 10000 Å, as no increase in the transverse field relaxation rate is observed belowT c . A sharp increase in the precession frequency is seen, starting atT c . This frequency shift shows little temperature dependence at low temperature; we found no clear evidence for unconventional superconductivity in this material. Zero field measurements in URu2Si2 show the weak antiferromagnetic transition at 17.5 K. Finally, we we found no clear evidence for unconventional superconductivity in this material. Zero field measurements in URu2Si2 show the weak antiferromagnetic transition at 17.5 K. Finally, we have observed relaxation in high transverse field due to the formation of a flux lattice in U6Fe, a material where the electron effective mass is rather lighter than in other heavy fermion systems. The relaxation exhibits a sharp onset atT c=3.9 K, and is flat at low temperatures as expected for a conventional superconductor. 相似文献
5.
6.
7.
Osamu Kobayashi 《Mathematische Zeitschrift》1989,200(2):273-277
Financial support from the FRD is gratefully acknowledged 相似文献
8.
9.
Mark P. WattersonAlison A. Edwards John A. LeachMartin D. Smith Osamu IchiharaGeorge W.J. Fleet 《Tetrahedron letters》2003,44(31):5853-5857
Efficient syntheses of all diastereomers of methyl 2,5-anhydro-3-deoxy-hexonate from mannono- or gulono-lactones provide precursors for C-nucleosides of 2-deoxyribose and for THF-templated γ- and δ-amino acids. 相似文献
10.
Takafumi Adachi Ichimin Shirotani Junichi Hayashi Osamu Shimomura 《Physics letters. A》1998,250(4-6):389-393
Lanthanide monophosphides LnP (Ln = La, Ce, Pr, Nd, Sm, Gd, Tb, Tm and Yb) with a NaCl-type structure have systematically been prepared at high temperatures. Using synchrotron radiation, X-ray diffractions of LnP have been studied up to 61 GPa at room temperature. The NaCl---CsCl transition for CeP is found at around 25 GPa. First-order phase transitions of LnP (Ln = La, Pr and Nd) with the crystallographic change occur at around 24, 26 and 30 GPa, respectively. The structure of the high pressure phases of these phosphides is a body center tetragonal structure (Ln: 0, 0, 0; P: 1/2, 1/2, 1/2; space group P4/mmm), which can be seen as the distorted CsCl-type structure. The Pr---P distance in the high pressure form of PrP is 2.789 Å. This almost agrees with the sum of covalent radii of Pr and P. The Pr---P bond has the covalent character at very high pressures. Similar results are also obtained for LaP and NdP. The pressure-induced phase transitions of SmP, GdP, TbP, TmP and YbP occur at around 35, 40, 38, 53 and 51 GPa, respectively. The structure of the high pressure phase is unknown. The phase transitions of LnP with many f-electrons are not due to the mechanism of the ordinary NaCl---CsCl transition. The transition pressures of LnP increase with decreasing the lattice constants in the NaCl-type structure, which decrease with increasing atomic number of the lanthanide atoms. 相似文献