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G A van't Klooster F M Woutersen-van Nijnanten H J Kolker J Noordhoek A S van Miert 《Journal of chromatography. A》1992,579(1):158-164
Ethylmorphine N-demethylation is used as a marker pathway in studies of rat cytochrome P450 3A and 2C11 biotransformations. At present, microsomal activities are generally measured by a colorimetric determination of the formed formaldehyde. In the present study, a high-performance liquid chromatographic method of separating and quantifying both the N-demethylated (norethylmorphine) and the O-de-ethylated (morphine) metabolites is described. Either samples are extracted with ethyl acetate or proteins are precipitated with zinc sulphate-barium hydroxide. Separation is achieved on a CN reversed-phase column, using a mobile phase of phosphate buffer (pH 4.5)-acetonitrile (90:10, v/v). At a flow-rate of 1.5 ml/min, the analysis time is 30 min. The limit of detection (ultraviolet, 210 nm) for ethylmorphine and its metabolites is 0.5 micrograms/ml. 相似文献
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G A van 't Klooster H J Kolker F M Woutersen-van Nijnanten J Noordhoek A S van Miert 《Journal of chromatography. A》1992,579(2):354-360
A high-performance liquid chromatographic method is presented for the determination of trimethoprim (TMP), 3'-hydroxy-TMP, 4'-hydroxy-TMP, alpha-hydroxy-TMP and two TMP N-oxides. The last two metabolites appear to decompose on liquid extraction. TMP and its oxidative metabolites are separated using a C18 radial-compression column and quantified by UV detection at 230 nm. Calibration curves are linear from 0.5 to at least 50 microM. The limit of detection is 0.05-0.15 micrograms/ml. In in vitro rat liver metabolism studies. 3'- and 4'-hydroxylation of TMP appear to be important metabolic pathways whereas TMP N-oxides are minor metabolites. 相似文献
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An accurate structure refinement of the deuterated analog of the cesium lithium acid sulfate, formerly identified as ‘Cs1.5Li1.5H(SO4)2’, has been carried out using neutron diffraction methods. Like the protonated material reported earlier (Merinov et al., Solid State Ionics 69 (1994) 53), the compound is cubic, , however, the correct stoichiometry is Cs3Li(DSO4)4. There are four formula units per unit cell and six atoms in the asymmetric unit. The lattice constant measured in this work is a=11.743(2) Å, comparable to the earlier results. The structure contains one disordered hydrogen bond, formed between O(2) atoms and located on two of the edges of the single LiO4 tetrahedron. The Li site occupancy is , as is that of the deuterium site. This level of site occupancies is consistent with a structure in which hydrogen bonds are formed only when the lithium site is unoccupied, and explains the otherwise close proximity of the Li and D atoms, 1.394(10) Å. This unusual structural feature furthermore leads to a fixed stoichiometry, as confirmed here by chemical analysis of both the deuterated and protonated materials, despite the partial occupancy of the lithium and deuterium (hydrogen) atom sites. 相似文献
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A procedure has been developed for estimating the information content of retrieval systems with binary-coded mass spectra, as well as mass spectra coded by other methods, from the statistical properties of a reference file. For a reference file, binary-coded with a threshold of 1% of the intensity of the base peak, this results typically in an estimated information content of about 50 bits for 200 selected values. It is shown that, because of errors occurring in the binary-coded spectra, the actual information content is only about 12 bits. This explains the poor performance observed for retrieval systems with binary-coded mass spectra. 相似文献
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White DB Tippens WB Abegg R Baldisseri A Boudard A Briscoe W Fabbro B Garçon M Hermes EA Jacobs WW Kessler RS Lytkin L Mayer B Nefkens BM Niebuhr C Petrov AM Poitou J Saudinos J Tomasi-Gustafsson E van der Schaaf A van Oers WT Vigdor SE Wang M 《Physical review D: Particles and fields》1996,53(11):6658-6661
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Dr. Riccardo Bonsignore Sophie R. Thomas Dr. Wim T. Klooster Dr. Simon J. Coles Dr. Robert L. Jenkins Dr. Didier Bourissou Prof. Giampaolo Barone Prof. Angela Casini 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(19):4226-4231
With the aim of exploiting new organometallic species for cross-coupling reactions, we report here on the AuIII-mediated Caryl−P bond formation occurring upon reaction of C^N cyclometalated AuIII complexes with phosphines. The [Au(C^N)Cl2] complex 1 featuring the bidentate 2-benzoylpyridine (CCON) scaffold was found to react with PTA (1,3,5-triaza-7-phosphaadamantane) under mild conditions, including in water, to afford the corresponding phosphonium 5 through C−P reductive elimination. A mechanism is proposed for the title reaction based on in situ 31P{1H} NMR and HR-ESI-MS analyses combined with DFT calculations. The C−P coupling has been generalized to other C^N cyclometalated AuIII complexes and other tertiary phosphines. Overall, this work provides new insights into the reactivity of cyclometalated AuIII compounds and establishes initial structure–activity relationships to develop AuIII-mediated C−P cross-coupling reactions. 相似文献
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