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  • 1
    Electronic Resource
    Electronic Resource
    Stereoselectivity of the 4-hydroxylation of debrisoquine in man, detected by gas chromatography/mass spectrometry1 (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 63-66 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A stable isotope assay for the quantification of debrisoquine (1) and its major urinary metabolite 4-hydroxydebrisoquine (2) is described. The method consists of extractive derivatization of 1 and 2 by use of 1,3-diketones, chiral derivatization of the 4-hydroxy group of 2, and gas chromatography/negative ion chemical ionization mass spectrometry in the presence of deuterated analogues of 1 and 2. In comparison with synthetic R-(-)-2 and S-(+)-2 it is shown that in vivo benzylic 4-hydroxylation of 1 is highly stereoselective, leading predominantly to S-(+)-4-hydroxydebrisoquine (enantiomeric excess ≥90%).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200150202
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  • 2
    Electronic Resource
    Electronic Resource
    Far ultraviolet optical activity of saccharide derivatives. III. Amylose triacetate in the solid state (1973)
    New York : Wiley-Blackwell
    Biopolymers 12 (1973), S. 2189-2193 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bip.1973.360120922
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  • 3
    Electronic Resource
    Electronic Resource
    About the microstructure of PCVD prepared crystal mats of statistical oligo-vinylidene-fluoride-trifluoroethylene in relation to other fluorinated polymers (1995)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 33 (1995), S. 237-246 
    Details
    ISSN: 0887-6266
    Keywords: oriented fluoro-oligomers ; chemical vapor deposition ; ferroelectricity ; glass transition ; Brillouin spectroscopy ; x-ray diffraction ; vinylidene fluoride ; trifluoroethylene ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The room temperature phase of the physical/chemical vapor-deposited statistical co-oligomer VDF/TrFE(70/30) has been characterized by different experimental methods such as small-angle x-ray scattering, wide-angle x-ray diffraction, size-exclusion chromatography, infrared absorption and optical refractometry. The characterization of the elastic properties was carried out using high-performance Brillouin spectroscopy in connection with special scattering geometries. The co-oligomer VDF/TrFE(70/30) was obtained by cracking the parent statistical copolymer and subsequently vapor depositing the shortened chains on highly oriented PTFE substrates (PIA-technique). The room temperature phase of the resulting oriented waxy crystal mats of VDF/TrFE(70/30) is predominantly ferroelectric. The physical properties are very different to those of similarly PIA-prepared n-alkanes, perfluoroalkanes, and blockfluoroalkanes. The microstructure of VDF/TrFE(70/30) is interpreted in terms of partially crystalline nano-sized structures giving rise to a marked freezing process below room temperature. © 1995 John wiley & Sons, Inc.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1995.090330208
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  • 4
    Electronic Resource
    Electronic Resource
    Simultaneous determination of 6-oxo-prosta-glandin F1α and 2,3-dinor-6-oxo-prostaglandin F1α in biological fluids by stable isotope dilution and negative ion chemical ionization mass spectrometry (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1985), S. 399-404 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A stable isotope dilution assay for the simultaneous determination of two metabolites of prostacyclin (1), 6-oxoprostaglandin F1α (2a) and 2,3-dinor-6-oxo-prostaglandin F1α (3a), in human seminal fluid and human urine is described. A new chemical total synthesis of deuterated internal standard, 18,18,19,19-(2H4)-2,3-dinor-6-oxo-PGF1α (3b), is presented and enables specific and sensitive quantification based on negative ion chemical ionization mass spectrometry. 2a and 3a were analysed as their methoxime pentafluorobenzyl ester tris(trimethylsilyl) ether derivatives in the selected ion monitoring mode registrating the [M-181]- fragments with a detection limit for both prostanoids of 10 pg per injection. The two metabolites occur in human seminal fluid in very low concentrations (2a: 2.8 ng ml-1; 3a: 1.7 ng ml-1) and cannot contribute significantly to the urinary metabolite levels which are in the range of 108-265 ng/24 h for 3a and 124-574 ng/24 h for 2a.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200120808
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  • 5
    Electronic Resource
    Electronic Resource
    Measurement of thromboxane B2 in human urine by isotope dilution and negative ion chemical ionization mass spectrometry (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1985), S. 554-559 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific assay for the quantification of thromboxane B2 (TXB2) (1) in human urine is described. The method is based on the use of low-blank (1H≤0.2%) tetradeuterated internal standard 2 (18, 18, 19, 19-2H4-thromboxane B2), whose chemical synthesis is reported. After purification and high-performance liquid chromatography (HPLC) samples are derivatized to give an open-chain derivative of thromboxane B2, the methoxime pentafluorobenzyl ester tris(trimethylsilyl) ether (TXB2-MO-PFB-TMS3), most suitable for negative ion chemical ionization mass spectrometry. In the selected ion monitoring mode limits of detection per injection for pure standards and biological samples of 10 pg and 30 pg, respectively, are established. Normal urinary excretion of 1 in humans is 37-112 ng/24 h (n = 12).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200120919
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  • 6
    Electronic Resource
    Electronic Resource
    Determination of the enantiomers of flecainide and two major metabolites in man by gas chromatography/mass spectrometry using negative ion chemical ionization and stable isotope labelled internal standards (1990)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1990), S. 256-266 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The class I antiarrhythmic drug flecainide (1) is used clinically as racemate. In order to study the stereochemical disposition and excretion of 1 an analytical method has been developed based on a deuterated analogue of 1 as internal standard and on measurement with gas chromatography/mass spectrometry (GC/MS) using negative ion chemical ionization (NICI). Several diasteromeric derivatives prepared were separated on an achiral capillary column. All derivatives exhibited negative ion properties forming characteristic fragments: [M — CH2CF3]- and [M — HF]-., respectively. The limit of detection was 1 pmol ml-1 plasma corresponding to 0.41 ng ml-1 of free base. A more convenient and in particular more precise approach was investigated by separating the pentafluoropropionyl (PFP) derivatives on a chiral phase capillary column monitoring the base peak [M — 20]-. in NICI mode. This method is not only the most sensitive assay of 1 presently available, but also allows for the determination of the enantiomers of flecainide in biological fluids. In addition, the assay could be applied to the dtermination of the enantiomers of one of the major metabolites of flecainide, the meta-O-dealkylated flecainide (MODF), in human urine. Additionally, a non-sterospecific assay was developed and applied to the quantification of the two major metabolites of flecainide, MODF and the meta-O-dealkylated flecainide lactam in human urine. Deuterated analogues were used as internal standards and measurement of the PFP derivatives with GC/MS using NICI was performed.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200190410
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  • 7
    Electronic Resource
    Electronic Resource
    Quantification of nitrendipine by stable isotope dilution and electron-capture negative ion chemical ionization (1986)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 645-650 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron-capture properties of nitrendipine, a 1,4-dihydro-pyridine derivative with antihypertensive activity, have been applied to develop a sensitive and specific assay in biological fluids using capillary column gas chromatography and measurement in negative ion chemical ionization mode. The synthesis of a 13C4-labelled analogue suitable as a biological internal standard for bioavailability studies and of a 2H8-labelled analogue, which serves as internal standard, is described. The electron-capture positive ion chemical ionization and electron-capture negative ion chemical ionization mass spectra of nitrendipine and its isotope-labelled analogues are compared. The assay has a detection limit of 100 pg ml-1 plasma with a coefficient of variation of 10.2% using the selected ion monitoring mode and electron-capture negative ion chemical ionization. The method is specific, sensitive and accurate to determine terminal half-life times after intravenous and oral administration of nitrendipine and its 13C-analogue. From the nearly identical plasma concentration-time profile of nitrendipine and its 13C-labelled analogue, an isotopic effect can be excluded. Thus, the synthesized 13C4-analogue should be well suited as a biological standard for bioavailability studies.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200131202
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  • 8
    Electronic Resource
    Electronic Resource
    Synthese und Constitution des Isophorons (1897)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 297 (1897), S. 185-203 
    Details
    ISSN: 0075-4617
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.18972970110
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  • 9
    Electronic Resource
    Electronic Resource
    A PGE2-derivative for quantitative gas chromatographic mass spectrometric measurement in the selected ion monitoring modePresented in part at the 21st Annual Meeting of the German Pharmacological Society, Mainz, March 1980 (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 114-117 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The quantification of prostaglandin PGE2 by gas chromatography mass spectrometry in the form of an easily prepared derivative is described. After extraction and purification of biological samples the compound was derivatized in two steps to 9-enol-PGE2-methylester-trimethylsilylether, 9-enol-PGE2 -Me-TMS3. The molecular ion at m/z 582 with 40% relative abundance and the fragment ion at m/z 492 with 100% relative abundance permit a specific and sensitive evaluation in the selected ion monitoring mode. The high masses selected lie above the biological background. The calibration curve produced by adding known amounts (10-200 ng) of PGE2 to blank human urine and with (2H4)-deuterated PGE2 as internal standard gave a linear correlation. The separation from biological impurities was obtained on a 50 m glass capillary column and resulted in sharp and symmetrical peaks.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200110304
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  • 10
    Electronic Resource
    Electronic Resource
    A stable isotope method for the quantification of N-acetyl-5-aminosalicylic acid in plasma and urine (1984)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 539-544 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of a number of N-acyl-5-aminosalicylic acids and their derivatives is described. These compounds allow the sensitive and specific mass spectrometric determination of unlabelled or deuterium-labelled N-acetyl-5-aminosalicylic acid in biological samples. An in vivo study shows that the labelled compound, administered to rats, is excreted isotopically unchanged to at least 97%, and that no significant deacety lation/acetylation mechanism exists for this metabolite N-acetyl-5-aminosalicylic acid of salicylazosulphapyridine.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200111009
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