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  • Analytical Chemistry and Spectroscopy  (23)
  • Physics  (5)
  • Wiley-Blackwell  (28)
  • American Institute of Physics
  • American Institute of Physics (AIP)
  • 1
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermospray LC/MS methods with internal standardization were developed for the quantification of the antimalarial arteether and six of its metabolites at the 1-10 μg/ml level in liver microsome preparations without the use of solvent extraction. The thermospray mass spectra of arteether and most of its metabolites exhibited strong [M + NH4]+ and [M - OR]+ peaks arising from the molecular ion adduct and the loss of the alkoxy or hydroxy group of the side chain. In addition to the six metabolites for which authentic reference standards were available, three additional metabolites were detected. The major metabolites of arteether were found to be dihydroartemisinin, deoxydihydroartemisinin, 3-hydroxydeoxydihydroartemisinin, two isomers of hydroxyarteether, and 3-hydroxydeoxyarteether. Deoxyartheether was not found at significant concentrations in the microsome preparation.
    Additional Material: 11 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 5 (1982), S. 150-150 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 959-968 
    ISSN: 0887-6266
    Keywords: PTMSP ; cross-linking ; membranes ; permeability ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Cross-linkable poly[1-(trimethylsilyl)-1-propyne] (PTMSP) films were cast from toluene solutions containing PTMSP and either 4,4′-diazidobenzophenone or 4,4′-(hexafluoroisopropylidene)diphenyl azide. The composite films were clear and homogeneous and were cross-linked by UV irradiation at room temperature or thermal annealing at 180°C. Low levels of the bis(aryl azide) (1-5 wt %) were effective in rendering the films insoluble in toluene and THF, both good solvents for PTMSP. The process is simple and effective, and thus PTMSP can be readily converted to mechanically stable membranes with permeabilities and separation factors comparable or higher than those of poly(dimethylsiloxane). The films were characterized by measuring their density, their permeability toward O2 and N2, and their spectroscopic properties. Compared to PTMSP, films containing bis(aryl azide) cross-linkers had lower permeabilities and higher separation factors, consistent with a reduction in free volume. When the films were cross-linked photochemically, the permeabilities declined further and the separation factor increased. Films cross-linked thermally had permeabilities comparable to their PTMSP/azide precursors, and density and swelling measurements suggest that higher free volumes are obtained in thermally cross-linked films. All films stored in air suffered from a slow decline in permeability which may reflect slow surface oxidation of the films. When stored in vacuum, cross-linked films were stable and showed no loss in permeability, but the permeability of uncross-linked PTMSP films stored under the same conditions fell to 70% of their original value in 1 month. We attribute the permeability decline to densification accelerated by impurities and solvents. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 959-968, 1998
    Additional Material: 5 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 2787-2793 
    ISSN: 0887-6266
    Keywords: gel ; arborol ; dendrimer ; freeze-fracture electron microscopy ; small-angle X-ray scattering ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Reversible gels of two-directional cascade polymers with hydrophilic groups covalently attached by an hydrophobic center chain were studied by light and small-angle X-ray scattering, differential scanning calorimetry, and freeze-fracture transmission electron microscopy. The long, self-assembled fibers interact side-by-side over extended regions to form bundles. A given fiber may participate in several bundles, thus forming a three-dimensional gel network. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 2787-2793, 1997
    Additional Material: 8 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1990), S. 793-806 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Studies on the metabolism of the tricyclic antidepressant trimipramine, 5-(3-dimethylamino-2-methylpropyl)-10, 11-dihydro-5H-dibenz[b, f] azepine, in the rat are described. Many metabolites of trimipramine (TMP) were isolated from rat urine after enzymatic hydrolysis and their structures were identified by a gas chromatographic/mass spectrometric method, before and after appropriate chemical derivatization. Besides unchanged TMP, 20 metabolites were characterized (underivatized, and after acetylation), of which 12 had undergone alicyclic (C10 or C11) oxidation. This is a hitherto unreported metabolic pathway for TMP in the rat.
    Additional Material: 5 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1988), S. 211-213 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of octafluorotoluene (OFT) as a versatile gas chromatographic/mass spectrometric derivatizing agent for steroids containing alcoholic, phenolic or α,β-unsaturated keto functions, is described. Two distinct derivatizing schemes can be utilized, involving (method 1) a phase-transfer reaction, employing a two-phase system of CH2Cl2 and N NaOH with n-Bu4NHSO4 as catalyst (suitable for alcoholic and phenolic steroids) and (method 2) a reaction conducted in anhydrous dimethylformamide at 155°C with CsF as base (appropriate for α,β-unsaturated keto steroids). Perfluorotolyl (PFT) ethers and/or enol ethers have thus been generated. The electron impact spectra display abundant high-mass molecular ions where derivatization has occurred at a phenolic or enolic function. An extraction, derivatization and gas chromatographic/mass spectrometric scheme has been devised involving method 2 for the analysis of steroids in human plasma. A preliminary quantitative investigation of the levels of testosterone in plasma has been carried out employing these methods. The anomalously high level found is explained in terms of the presence in plasma of lipid-soluble derivatives of testosterone (probably fatty acid esters) which generate the testosterone bis-OFT derivative under the reaction conditions employed.
    Additional Material: 2 Ill.
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  • 7
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An assay for the determination of the neuromuscular blocking agents pancuronium bromide and vecuronium bromide in plasma or urine has been developed. This method is based on syringe application of sample extracts to the moving belt surface and single metastable transition monitoring of the elimination of acetic acid from the ion of m/z 543 during chemical ionization. The analysis shows good linearity over three orders of magnitude and is capable of analyzing for the compounds below the 5 ng ml-1 level. The assay has been used in preliminary pharmacokinetic studies of the biological fluids of surgical patients. The utility of the method for simultaneous determination of the deacetylated metabolites of these two drugs has also been investigated.
    Additional Material: 7 Ill.
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  • 8
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermospray mass spectra of arteether and 16 of its potential metabolites all showed strong [M + NH4]+ ions and with only a few exceptions these compounds also showed spectral peaks corresponding to [M + NH4 - HOR]+ and [M + H - HOR]+, where OR represents the alkoxy or hydroxy group at the 12-position. A method for quantifying the metabolites was developed in which the plasma was spiked with an internal standard (the propyl ether analog of arteether), extracted using a C-18 solid-phase cartridge, then subjected to thermospray high-performance liquid chromatographic/mass spectrometric analysis using selected ion monitoring and a C-18 reversed-phase analytical column. Following the intravenous administration of arteether (11.6 mg kg-1), the plasma was found to contain 12 metabolites of arteether in the 10-1000 ng ml-1 range 15 min post-injection, and within 60 min two of these metabolites attained higher concentrations than that of the parent compound, while several other of the metabolites attained concentrations similar to the parent compound. The pseudo-first-order half-life of arteether was found to be 10.0 ± 0.6 min, while the apparent half-lives of most of the metabolites were in the 15-30 min range. Nine of these metabolites were identified by comparison to authentic reference standards and the structures of three remaining metabolites were tentatively assigned from their spectral and chromatographic properties. The metabolic pathways leading to these 12 metabolites was a rather complex, multiple-step process, but most of the metabolites arose from an enzymatic oxidation at one of three sites; 3α, 9α, or the CH2 of the side-chain. Conversion of the endoperoxide group to an cyclic ether was not a major pathway. The in vitro antimalarial activity of reference standards of several of the metabolites was determined and all of those tested were found to be active in the low nanogram per milliliter range.
    Additional Material: 14 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 9 (1995), S. 1087-1094 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A pneumatically assisted electrospray liquid chromatography/mass spectrometry interface has been modified for use with open-tubular supercritical fluid chromatography (SFC). The modified interface houses the SFC flow restrictor within the spray device. A sheath-flow liquid of methanol or methanol/water containing ammonium acetate flows coaxially to the restrictor. The addition of the sheath-flow liquid results in the ionization of analytes known to be in a neutral charge state during the chromatographic separation. The sheath-flow liquid also allows for the independent operation of the chromatograph and the mass spectrometer. Both could be operated under optimum conditions. The operation of the interface was optimized using a solution of poly(dimethylsiloxane) in CO2 introduced by continuous infusion. We also report the application of the modified instrument to samples containing amines and propoxylated alcohols.
    Additional Material: 8 Ill.
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  • 10
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The sequences of synthetically prepared methylphosphonate oligodeoxyribonucleotides have been verified using ionspray tandem mass spectrometry with sample introduction via flow injection. The technique involves the use of product-ion scans from multiply protonated (4+ and 5+) precursors. Among the ions detected are several series of fragments of different charge states that indicate the base sequence of the intact molecule. Oligomers as large as 18 bases have been successfully characterized.
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