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51.
Hohyun Kim Hyeongjin Roh Seung-Bock Yeom Hee Joo Lee Sang Beom Han 《Chromatographia》2003,58(3-4):235-240
Summary A sensitive and selective liquid chromatographic method coupled with electrospray ionization tandem mass spectrometry (LC–ESI–MS–MS) has been developed for quantification of felodipine in human and dog plasma. Compounds were separated on a 2.0 mm × 150 mm, 5.0 m particle, C8 column with 1 m m ammonium acetate–acetonitrile, 20:80, pH 6.0, as mobile phase at a flow rate of 200 L min–1. Nifedipine was used as internal standard. Plasma samples were extracted with diethyl ether, the centrifuged upper layer was evaporated, the residue was reconstituted with mobile phase, and the reconstituted samples were injected. The analytical column lasted for at least 1000 injections. By use of multiple reaction monitoring (MRM) mode in MS–MS felodipine and nifedipine were detected without severe interference from the human or dog plasma matrix. Felodipine produced a protonated precursor ion ([M + H]+) at m/z 384 and a corresponding product ion at m/z 338. And internal standard (nifedipine) produced a protonated precursor ion ([M + H]+) at m/z 347 and a corresponding product ion at m/z 315. Detection of felodipine in human and dog plasma was accurate and precise, with a limit of quantification of 0.05 ng mL–1. The method has been successfully applied to preliminary pharmacokinetic study of felodipine in human and dog plasma. 相似文献
52.
Devendra Kumar Uday Razdan Alka D. Gupta 《Journal of polymer science. Part A, Polymer chemistry》1992,30(7):1477-1487
Various melt-polymerizable bisimido-bisphthalonitrile polymer precursors were synthesized by the reaction of 4-aminophthalonitrile (4-APN) with bis(3,4-dicarboxyphenyl) dimethylsilane dianhydride (SIDA), 4,4′-hexafluoroisopropylidene diphthalic anhydride (6FDA), bis(3,4-dicarboxyphenyl)ether dianhydride (ODPA), and 3,3′, 4,4′-tetracarboxylichenzophen+ne dianhydride (BTDA) in an aprotic solvent. The synthesized monomers showed crystalline melting at 269 and 271°C. Elemental analysis, differential thermal analysis (DTA), infrared (IR), nuclear magnetic resonance (1H-NMR) and mass spectral studies were carried out to characterize the synthesized monomers. Thermogravimetric analysis (TGA) of the synthesized monomers showed their thermal stability at 410–400°C. A detailed study and NMR investigation of the first step of condensation reaction was carried out and indicated the formation of a transient charge transfer complex. Thermal cyclization of the formed intermediate, however, gave the required monomers. A preliminary study demonstrated that melt-polymerization of the synthesized monomers gave thermallystable, tough polymers. 相似文献
53.
Joris Van Loco Maureen Moerenhout Hedwig Beernaert 《Accreditation and quality assurance》2003,8(2):61-67
A GLP study can be performed at more than one site. This is called a multi-site study. Although, the study is performed at
different sites, it is still one study and must completely comply with the GLP principles. The fact that different activities
are conducted at different sites implies that the planning, the organization and the communication are crucial for the success
of the study. This means that all the staff involved should know their responsibilities and should have the knowledge and
skills to realize all the phases of the study according to the GLP principles. To achieve a well managed multi-site study,
several strategies for setting up such a study can be followed. This paper focuses on the responsibilities, communication,
and collaboration of the personnel, which are involved in a multi-site study. Several case studies are highlighted, and we
concluded that the basic communication triangle in a single-site GLP study between test facility management, study director,
and the quality assurance unit should be extended to the communication among test facility and test site management, study
director, principle investigator(s), and the quality assurance units at the test sites.
Introduction
Received: 14 August 2002 Accepted: 26 November 2002 相似文献
54.
Krishna Bisetty Francesc J. Corcho Josep Canto Hendrik G. Kruger Juan J. Perez 《Journal of Molecular Structure》2006,770(1-3):221-228
In this paper, we report on the conformational profile of the pentacyclo-undecane (PCU) cage tripeptide carried out by molecular dynamics (MD) simulation using water as an explicit solvent. The MD solution phase studies carried on the model peptide analogues (A)=Ac–Ala–Ala–Ala–NHMe; (B)=Ac–Cage–Cage–Cage–NHMe; (C)=Ac–Ala–Cage–Ala–NHMe and (D)=Ac–Ala–Pro–Ala–NHMe, are used as a complimentary technique to the corresponding gas phase simulated annealing (SA) study previously carried out in our laboratory. No significant structural changes were observed over the MD trajectories. However, the results reported here provide further evidence that the (PCU) cage amino acid exhibits C7eq, C7aq, R and L conformations, and the theoretical results suggest that the PCU cage amino acid is a strong β-turn inducer. These results support the prediction that when the PCU cage residues are in the (i) and (i+2) positions, the β-turn can be extended in either direction to form anti-parallel β-pleated sheets, thereby forming the basis of the mechanism for the folding back of the chain in a cross-β-turn structure. 相似文献
55.
A complete assignment of the 1H, 13C and 19F NMR spectra of 1,1,4,4-tetrafluoro-2-propylidene-3-methyl-6-tert-butyl-1,4-disila-5-cyclohexene 3, the product of the cycloaddition reaction between tetrafluorodisilacyclobutene 1 and cis, trans-2,4-hexadiene mediated by (n5-C5H5)Mn(CO)3, has been made by means of various 2D NMR chemical shift correlation methods and selective heteronuclear decoupling techniques. An analysis of the three bond 13C-1H coupling constants and two bond 13C-19F coupling constants and the molecular modeling results enabled the determination of the conformation and configuration of compound 3. The conformation of 3 provides insight into mechanistic details of the Mn-mediated cycloaddition. 相似文献
56.
S. N. Dmitrieva N. I. Sidorenko A. I. Vedernikov L. G. Kuz’mina J. A. K. Howard T. M. Buslaeva S. P. Gromov 《Russian Chemical Bulletin》2007,56(5):993-1002
The condensation reaction of 1,2-bis(2-haloethoxy)-4-nitrobenzenes with acyclic α,ω-(oxa)alkanedithiols in the presence of
alkali metal carbonates produced a series of nitrobenzodithiacrown ethers with macrocycles of different size. The structures
of three ethers were established by X-ray diffraction. A new method was developed for the synthesis of nitrobenzomonothia-15-crown-5
ether. Nitro derivatives of benzodithiacrown ethers were tested as reagents for extraction of palladium(II), platinum(IV), and rhodium(III) from hydrochloric acid solutions. Extraction of PdII salts was found to be highly selective compared to that of PtIV and RhIII salts. Benzodithia-15-crown-5 ether is the most efficient extractant for palladium(II). Reduction of nitrobenzothiacrown ethers with hydrazine hydrate in the presence of a platinum catalyst afforded their amino
derivatives.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 958–966, May, 2007. 相似文献
57.
Z. A. Starikova A. I. Yanovsky Yu. T. Struchkov S. V. Zubkov I. I. Seifullina 《Russian Chemical Bulletin》1996,45(9):2157-2162
The crystal structure of the product of the condensation of (salicylideneamino)nitroguanidine with salicylaldehyde on a Ni2+ ion template, K[Ni(C15H10N5O4)] · DMF, has been studied. It was established that a planar Ni complex, consisting of isolated [NiL]– anions and solvated [K+ · DMF] cations, is formed. The negative charge of the anion is localized mainly on the O atoms of the nitro group. The nitroguanidine fragment of the ligand occurs in the tautomeric form, which was not reported previously.Deceased in 1995Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 2273–2277, September, 1996. 相似文献
58.
Improved separations of the isomers of olefinic aliphatic insect pheromones were obtained on cholesteryl cinnamate glass capillary columns by operating in the supercooled temperature range of the liquid crystal. Capillary columns were prepared with varying film thickness of the stationary phase; choice of the correct film thickness ensured optimum retention for a wide range of compounds within the most effective temperature range of the liquid crystal. The deactivation procedures described made the liquid crystal columns suitable for separation of the geometric isomers of polar and nonpolar compounds. 相似文献
59.
A novel series of the formula NdSrNi1−xCuxO4−δ were synthesized for various values of x ranging from 0 to 1 in 1 atm of O2 gas flow using conventional solid-state methods and were characterized by powder X-ray diffraction and electrical resistivity measurements. The compounds have been shown to adopt the K2NiF4-type structure. The oxygen stoichiometry of the compounds was determined from thermo-gravimetric analysis (TGA). An analysis of the micro-structure of the neodymium strontium nickel copper oxide is described. All the samples were semi-conducting from room temperature down to 77 K. The effect of Cu2+ incorporation on the structural and electrical properties of NdSrNi1−xCuxO4−δ, 0?x?1, are discussed in terms of Jahn-Teller distortion of the (Ni/Cu)O6 octahedra and mixed valence character of copper. 相似文献
60.
灭多威的光催化降解动力学研究 总被引:19,自引:3,他引:19
研究了农药灭多威在TiO2光催化下的降解产物,反应动力学及影响降解速度的因素,灭多威在TiO2催化下10min内可被完全转换为无机物而失去毒害作用,IR研究表明,灭多威的分解产物NH^+4,SO^2-4和CO2,其分争过程中准一级反应,除铜和氯离子体低浓度时有促进作用,而高浓度为阻碍作用外,大部分阴,阳离子对降解均有不利影响。 相似文献