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  • Analytical Chemistry and Spectroscopy  (60)
  • Humans
  • 1975-1979  (60)
  • 1977  (60)
  • 1
    Digitale Medien
    Digitale Medien
    In vivo metabolism of cannabinol by the mouse and rat and a comparison with the metabolism of Δ1-tetrahydrocannabinol and cannabidiolAbbreviations: THC = tetrahydrocannabinol; CBD = cannabidiol; CBN = cannabinol. (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 364-370 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The in vivo liver metabolism of cannabinol has been studied in the mouse and rat by combined gas chromatography and mass spectrometry. Cannabinol glucuronide was the major metabolite of cannabinol in the mouse and was accompanied by relatively large amounts of 7-hydroxycannabinol, cannabinol-7-oic acid and their corresponding glucuronide conjugates. Lower concentrations of glucuronides were found in the rat. Two series of disubstituted metabolites were found containing either a 7-hydroxyl or a 7-carboxylic acid group and a second hydroxyl group in the 1″-4″ positions of the sidechain. These were of low concentration in the mouse but higher in the rat; 1″-hydroxy metabolites were particularly abundant in the latter species. Also found in the rat livers were small amounts of sidechain monohydroxy metabolites and larger quantities of 4″,5″-bisnorcannabinol-3″-oic acid; these were absent in the mouse. The metabolites were identified using the trimethylsilyl (TMS),[2H9]TMS and methyl ester-TMS derivatives, and by reduction of acid metabolites with lithium aluminium deuteride to the corresponding alcohols.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040608
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  • 2
    Digitale Medien
    Digitale Medien
    The measurement of acetanilide in plasma by spectrophotometric and selected ion monitoring methods (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 255-257 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Plasma samples from volunteers who had received an oral dose of acetanilide have been analysed by gas chromatography mass spectrometry and ultraviolet absorption techniques. The gas chromatography mass spectrometry method involved extraction of the plasma and analysis of the acetanilide using selected ion monitoring with a deuterated internal standard. In the ultraviolet method the plasma was hydrolysed with acid to convert the acetanilide to aniline, and this compound was diazotized and coupled with N-1-naphthylethylene-diamine. The absorbance of the resulting complex was read at 550 nm. Acetanilide levels in plasma determined by the selected ion monitoring method were significantly lower than those measured by spectrophotometry. Pharmacokinetic data calculated from the results obtained using these two assays are very different and illustrate the need for an accurate and specific method of analysis. The major metabolites of acetanilide are shown not to interfere with these assays and the results suggest the possible presence of a new metabolite of acetanilide.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040412
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  • 3
    Digitale Medien
    Digitale Medien
    Cyclic alkylboronates as derivatives for the characterization of cannabinolic acids by combined gas chromatography and mass spectrometryAbbreviations: BSTFA = N, O-bis-(trimethylsilyl)trifluoroacetamide; TMCS = trimethylchlorosilane; THC-tetrahydrocannabinol; CBN = cannabinol; CBD = cannabidiol. (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 88-93 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Stable cyclic methyl-and n-butylboronates were prepared from the cannabinolic acids and used as derivatives for the characterization of these compounds by combined gas chromatography mass spectrometry. Retention times of the methylboronates were comparable with those of the trimethylsilyl derivatives. The mass spectra of these derivatives were more characteristic of the cannabinoid skeleton than were the spectra of the trimethylsilyl derivatives where fragmentation was associated with the trimethylsilyl groups. Molecular weights were lower and abundant molecular ions were obtained. These derivatives also offered the possibility of distinguishing between isomeric cannabinolic acids where only isomers possessing adjacent phenolic and carboxylic functions form cyclic boronates.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040206
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  • 4
    Digitale Medien
    Digitale Medien
    Peptide sequencing: The utility of chemical ionization mass spectrometry (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 159-171 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Chemical ionization mass spectrometry is used at low resolution to determine the sequences of permethylated acetyl peptides. The method has been tested with 45 peptides, between 2 and 5 residues long, including examples of all of the common amino acids except cysteine and N-terminal asparagine. The isobutane chemical ionization spectra contain three principal types of N-terminal sequence ion and one type of C-terminal sequence ion. The redundant information available from these four types of sequence ion increases the reliability of the sequence determination. In prospect, isobutane chemical ionization mass spectrometry seems to be a useful technique for peptide sequence determination, and may have advantages in some cases.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040308
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  • 5
    Digitale Medien
    Digitale Medien
    High performance liquid chromatographic and mass spectrometric identification of dimethylxanthine metabolites of caffeine in human plasma (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 172-177 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: High performance liquid chromatography and mass spectrometry were used to isolate and identify theophylline, theobromine and 1,7-dimethylxanthine (paraxanthine) in plasma of human volunteers following administration of 300 mg caffeine to methylxanthine-free volunteers. Plasma from these subjects was extracted and the dimethylxanthines were separated from each other and caffeine by high performance liquid chromatography. The effluents at the chromatographic peaks corresponding to the dimethylxanthine metabolites were collected, rechromatographed in a second system and the dried residues were subjected to mass spectrometry. By comparison of their retention times and mass spectra with those of authentic compounds, theophylline, theobromine and paraxanthine were positively identified as metabolic products of caffeine.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040309
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  • 6
    Digitale Medien
    Digitale Medien
    Single and multiple ion recording techniques for the analysis of diphenylhydantoin and its major metabolite in plasmaAbbreviations: DPH = diphenylhydantoin; HPPH = 5-(p-hydroxyphenyl)-5-phenylhydantoin; TMAH = trimethylanilinium hydroxide; BSA = N, O-bis-(trimethylsilyl)acetamide. (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 36-41 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method has been developed for single ion monitoring of diphenylhydantoin and its major metabolite 5-(p-hydroxyphenyl)-5-phenylhydantoin in plasma. A plasma extract is reacted with N, O-bis(trimethylsilyl)acetamide and single ion recording is carried out using a gas chromatograph mass spectrometer system. The mass value selected, m/e 254, is common to the TMS ethers of diphenylhydantoin and its principal metabolite 5-(p-hydroxyphenyl)-5-phenylhydantoin. The results indicate that one cause of an adverse reaction to diphenylhydantoin could be a reduced ability to hydroxylate the drug. Quantitative methods for the analysis of the drug and its major metabolite have also been developed. Diphenylhydantoin and 5-(p-hydroxyphenyl)-5-phenylhydantoin can be analysed in plasma after addition of deuterium labelled internal standards and conversion to volatile derivatives for mass fragmentographic analysis. Diphenylhydantoin and its internal standard are analysed as the N, N-dimethyl derivative, and the hydroxylated metabolite and its internal standard are converted to a pertrimetylsilyl compound by reaction with N, O-bis-(trimethylsilyl)acetamide.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040104
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  • 7
    Digitale Medien
    Digitale Medien
    Organic structural analysis. J. B. Lambert, H. F. Shurvell, L. Berbit, R. G. Cooks, G. H. Stout, Macmillan Publishing Co. Inc., New York, N. Y., 1976. 596 pp. $22.95 (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. vii 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040612
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  • 8
    Digitale Medien
    Digitale Medien
    Allyldimethylsilyl ethers as derivatives for the characterization of steroids and cannabinoids by combined gas chromatography and mass spectrometryAbbreviations: BSTFA = N, O-bis-trimethylsilyltrifluoroacetamide; THC = tetrahydrocannabinol; CBN = cannabinol; CBD = cannabidiol. (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 265-274 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The allyldimethylsilyl ethers of thirteen mono- and dihydroxy steroids and eleven cannabinoids were examined by combined gas chromatography mass spectrometry and their properties compared with those of the corresponding trimethylsilyl and t-butyldimethylsilyl ethers. The spectra of the allyldimethylsilyl derivatives of the steroids exhibited abundant ions produced by elimination of the larger (allyl) silyl substituent and were thus found to be useful for single ion monitoring studies. Ion currents carried by the [M-allyl]+ ions were slightly less than those carried by the [M-t-butyl]+ ions from the t-butyldimethylsilyl derivatives, but the spectra exhibited more abundant molecular ions and ions characteristic of the presence of specific functional groups such as a Δ5-3β-hydroxy structure. In addition they produced a lower molecular weight increase than the t-butyldimethylsilyl derivatives and had shorter retention times. The mass spectral fragmentations shown by the corresponding derivatives of the cannabinoids were very similar to those of the trimethylsilyl derivatives with the addition of abundant ions resulting from loss of the allyl or t-butylsilyl radical. However, these ions did not carry such high ion currents as the corresponding ions in the steroid spectra and were thus of limited use for single ion studies. The allyldimethylsilyl derivatives of the cannabinoid metabolites produced more abundant molecular ions than either the trimethylsilyl or t-butyldimethylsilyl derivatives. Fragmentation pathways involving elimination of C3H6 were found to be specific for the allyldimethylsilyl derivatives.
    Zusätzliches Material: 12 Tab.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040414
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  • 9
    Digitale Medien
    Digitale Medien
    Precise measurement of total body water using trace quantities of deuterium oxide (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 4 (1977), S. 82-87 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: This study was undertaken to investigate the possibility of measuring total body water in human subjects to better than ±0.5%. Accurate serial estimates of total body water were required to complement densitometric and anthropometric measurements used to monitor body compositional changes in obese patients undergoing dietary or surgical weight reduction therapy. The method required the oral administration of 1-2 g of deuterium oxide and the analysis of pre-dose and respective equilibrated samples of urine, plasma or saliva. The sample size required for analysis was 5 μl and the conversion of gaseous phase was accomplished using a uranium reduction furnace. Isotopic erichment of samples was measured using a mass spectrometer incorporating several features designed to cope with problems inherent in H2/H2H isootopic analysis. Reproducibility of sample preparation and accuracy of the mass spectrometer were tested using international standards and shown to give an overall sensitivity of 2 parts in 107 for the determination of deuterium in H2O/H2HO mixtures. This precision has enabled us to demonstrate that isotopic fractionation of deuterium with respect to hydrogen occurs within the body and expands the potential use of this isotope for quantitative biochemical studies in the human subject.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200040205
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  • 10
    Digitale Medien
    Digitale Medien
    Electron impact and chemical ionization mass spectra of alkyldiphenylphosphine oxides (1977)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1977), S. 33-36 
    Details
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In the 70 e V electron impact mass spectra of a series of alkyldiphenylphosphine oxides (Rφ2PO, R = Me, Et, n-Pr, i-Pr, n-Bu, i-Bu, t-Bu, neopentyl, n-decyl), molecular ions of low abundance are observed and [M + H]+ ions are formed to a small extent at high sample pressures. The major ions include [φ2PO]+, [φ2POH]+; [φ2CH2PO]+ and [φ2CH2POH]+ which are formed by rearrangement and cleavage processes. The chemical ionization mass spectra obtained with methane and isobutane reagents consist of [M + H]+ ions. The proton affinity of Rφ2PO was found to be 219 ± 2.5 kcal mol-1.
    Zusätzliches Material: 4 Tab.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/oms.1210120110
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