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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010201

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Interpretation of mass spectra, 2nd Edition, by F. W. McLafferty. W. A. Benjamin Inc., Reading, Massachusetts, 1973. $15.00 (cloth) $7.50 (paper) (1974)

Millard, Brian J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xiv

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200010118

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Qualitative and quantitative mass spectrometry of some noncatecholic biogenic amines and related compounds as their dansyl derivatives (1974)

Durden, D. A. ; Davis, B. A. ; Boulton, A. A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 83-95

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The use of the integrated ion current technique for the analysis of biogenic amines and phenols as their 1-dimethylaminonaphthalene-5-sulphonyl (dansyl) derivatives is described, particularly as regards to the linearity and sensitivity of detection. The mono derivatized amines gave a linear response over the range 10-9 to 10-14 mol, with a few being detected in quantities as small as 5 × 10-15 mol. The bisdansyl derivatives have a lower sensitivity and the response is linear over a more restricted range, terminating at 10-13 mol. Deuterated analogues of some of the amines were prepared and the feasibility of their use as internal standards was investigated. In this way, the problems associated with quantitative biochemical analyses caused by losses during extractions, chromatographic separations and thermal decomposition in the mass spectrometer lon source are overcome. The differentiation of isomers of biogenic amines as their dansyl derivatives has been accomplished by fractional sublimation and by examination of differences in their fragmentation patterns.

Additional Material: 7 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010202

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Amino acid mixture analysis by mass spectrometry in the form of their dimethylaminomethylene methyl esters (1974)

Horman, I. ; Hesford, F. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 115-119

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The amino acids, arginine, citrulline, cysteine, cystine, histidine, hydroxyproline, methionine, ornithine, proline, serine, threonine, tryptophan and tyrosine, have been analysed in the form of their N-(N′, N′-dimethylaminomethylene) methyl esters. formed in a single step by reaction of the free amino acid or its hydrochloride with N,N-dimethylformamide dimethylacetal in acetonitrile/methanol (2:1). A reaction time of 15 minutes at 100 °C ensures complete derivatization, the derivatives being volatile at source temperatures below 150 °C, and giving electron impact spectra characterized by abundant (or moderately abundant) peaks at or near the mass of the molecular ion.The analysis of amino acid mixtures by mass fragmentography on characteristic high mass peaks of their N-(N′,N′-dimethylaminoethylene) methyl ester derivatives, introduced on a direct insertion probe and volatilized during temperature programming of the source, is qescribed. The method is applied to the analysis of a mixture containing arginine, citrulline, cystine, histidine and tryptophan, traditionally difficult to analyse by other methods.

Additional Material: 6 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010206

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Observations on the mechanism of hydroxylation of cyclophosphamide by rat liver microsomes: The metabolism of cyclophosphamide-4-d2 (1974)

Connors, T. A. ; Cox, P. J. ; Farmer, P. B. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 130-136

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The metabolism of cyclophosphamide-4-d2 (2-[bis(2-chloroethyl)amino]-tetrahydro-4,4-dideuterio-2H-1,3,2-oxazaphosphorine 2-oxide), was studied. The first detectable metabolite was a hydroxy derivative which was trapped with ethanol. Mass spectrometry of the resulting two ethoxy derivatives and of the deuterated acrolein 2,4-dinitrophenylhydrazones formed therefrom via reaction with acidic 2,4-dinitrophenylhydrazine, afforded evidence that the ethoxy substituents were at C-4, which was therefore the position of the original hydroxy substituent. The mass spectrum of the deuterated acrolein 2,4-dinitrophenylhydrazone obtained from the total reactive metabolites was used to estimate the ratio of 4- to 6-hydroxylation. The rate of metabolism and the antitumour activity of cyclophosphamide and its 4-d2 analogue were compared.

Additional Material: 3 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010209

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Mass spectral studies of airborne particulates and possible pollution sourcesWork supported in part by EPA under Agreement No. EPA-IAG-0217(D) entitled ‘Correlation of Hazardous Compound Composition of Coal, Ash, Fly-Ash, and Other Emissions from Combustion’. (1974)

Shultz, J. L. ; Sharkey, A. G. ; Friedel, R. A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 137-141

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The organic material in airborne particulate matter is being studied by high resolution mass spectrometry to determine if hydrocarbons typical of major sources of pollution can be detected. Carbon number distributions and hydrogen-to-carbon ratios of components found in airborne particulate samples and the corresponding data for compounds detected in fuel combustion products show great similarity. Samples collected near large power stations and major airports were compared with typical urban particulate samples. Particulates collected from jet engine exhaust and a condensate from the stack effluent from a coal-fired combustion system were studied. Mass spectral data were obtained for an auto exhaust tar, a coal tar pitch and several fuels. The mass spectra of two total particulate samples, compared to the spectrum of an ether extract of the organic matter, indicate that direct vaporization can be used and extraction is not essential for qualitative mass spectral studies.

Additional Material: 7 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010210

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Analysis of intact phospholipids by field desorption mass spectrometry (1974)

Wood, Gordon W. ; Lau, Pui-Yan

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 154-155

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The first application of field desorption mass spectrometry to the analysis of intact diacyl glycerophosphorylcholines (lecithins) has led to the detection of prominent molecular ions. This technique enables positive identification of the components of a mixture of phosphatidylcholines, which will provide valuable information on the phospholipid composition of biological fluids.

Additional Material: 1 Tab.

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URL: http://dx.doi.org/10.1002/bms.1200010213

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Mass spectrometry of pesticides and pollutants, by S. Safe and O. Hutzinger. CRC Press Inc., Cleveland, Ohio, 1973. pp. 220, $32.00 (1974)

Sharkey, A. G.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 157-157

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010215

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xi

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010216

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Detection and quantitative analysis of amphetamine (1974)

Danielson, Terry J. ; Boulton, Alan A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 159-162

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The high resolution mass spectrometric integrated ion current procedure has been used to identify and quantitate amphetamine, isolated as its dansyl derivative, as it is found after addition to urine and in tissues of the rat following intraperitoneal injection. A linear relationship between amphetamine and ion current response has been established at least in the range 5 × 10-12 to 5 × 10-7 g, and as little as 8 × 10-13 mol of amphetamine in urine may be detected.

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URL: http://dx.doi.org/10.1002/bms.1200010302

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Thin-layer chromatography-mass spectrometry for the identification of sapogenins from Digitalis species (1974)

Evans, F. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 166-168

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A method is described for the identification of the sapogenins of several Digitalis species. The steroids are separated by repeated development thin-layer chromatography and identified by means of high resolution mass spectrometry. The spectra of tigogenin, gitogenin, digalogenin and digitogenin are recorded. These spectra are of particular use in establishing the position of extra hydroxy moieties in the steroid nuclei. Several species of Digitalis were screened for their sapogenin content. D. purpurea, D. mertonensis and D. lutea were found to contain tigogenin and digitogenin in small amounts, the principal steroid being gitogenin, whilst D. ambigua and D. lanata contained all four steroids.

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URL: http://dx.doi.org/10.1002/bms.1200010304

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Intramolecular isotopic order in biologically produced acetic acid (1974)

Meinschein, W. G. ; Rinaldi, G. G. L. ; Hayes, J. M. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 172-174

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Acetic acid isolated from cider vinegar and inorganically synthesized glacial acetic acid have markedly different intramolecular isotopic distributions of the stable carbon isotopes. Carbon-12 is concentrated in the methyl group relative to the carboxyl group in the biologically produced acid. The reverse distribution is observed in the particular sample of glacial acetic acid examined here.

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URL: http://dx.doi.org/10.1002/bms.1200010306

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Identification of some organic smog components based on rain water analysis (1974)

Saunders, R. A. ; Griffith, J. R. ; Saalfeld, F. E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 192-194

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: An analysis has been made of a sample of rain water collected in Washington, D.C. following a sustained photo-oxidant smog alert which was accompanied by haze and low visibility. The analysis was effected by purging the organic content from the water with helium gas and identifying the constituents by means of gas chromatography - mass spectrometry. The predominant compound was found to be 3-methylfuran, a possible intermediate or end product of the atmospheric decomposition of terpenoid hydrocarbons. The analysis suggests that the smog resulted from the air oxidation of hydrocarbons evolved from Appalachian forestation rather than from manassociated activities.

Additional Material: 3 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010309

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Source of the carboxamide nitrogen atom in 2-carboxamido-5-isopropoxycarbonylaminobenzimidazole, a metabolite of cambendazole (1974)

Vandenheuvel, W. J. A. ; Carlin, J. R. ; Ellsworth, R. L. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 190-191

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Combined gas chromatography-mass spectrometry and isotope labeling techniques have been employed to demonstrate that the carboxamide nitrogen atom in 2-carboxamido-5-isopropoxycarbonylaminobenzimidazole, a metabolite of 2-thiazolyl-5-isopropoxycarbonylaminobenzimidazole (cambendazole), is derived wholly from the parent drug. [15N] Thiazole-labeled cambendazole was administered to a rat and the metabolite isolated from urine. Trideutero-2-carboxamido-5-isopropoxycarbonylaminobenzimidazole was employed as a carrier to isolate the metabolite in sufficient purity for isotope ratio measurements using multiple ion detection. The metabolite was converted to its tetramethyl derivative by on-column reaction with trimethylanilium hydroxide to permit satisfactory gas chromatography.

Additional Material: 1 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010308

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Workshop reports (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 206-207

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010312

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xiii

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010314

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The mass spectral fragmentation of partially ethylated alditol acetates, a derivative used in determining the glycosly linkage composition of polysaccharidesSupported in part by AEC Contract No. AT(11-1)-1426.Abbreviations: PEGS = poly-(ethylene glycol succinate); PEGA = poly-(ethylene glycol adipate). (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010401

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Evaluation of bilirubin derivatives for mass spectral analysis (1974)

Salmon, Manuel ; Fenselau, Catherine

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 219-222

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Twelve derivatives of bilirubin were evaluated from the point of view of providing intense molecular ion peaks on electron impact and unambiguous molecular weights. The tetrakis-(trimethylsilyl) derivative of bilirubin was judged to be the most suitable because its molecular ion carries 22% of the total ion current and is the base peak in the spectrum. Molecular ions were found to carry 10% of the total ion current in the spectrum of the trimethylsilylated methyl ester of the phenylazo derivative of bilirubin. Fragmentation patterns of these two compounds were studied using deuterium labeling.

Additional Material: 3 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010404

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The use of Edman degradation in peptide mixture analysis by mass spectrometryA preliminary report including some of the data presented in this paper has been given at the 6th International Mass Spectrometry Conference, Edinburgh, Scotland, September 1973. (1974)

Roepstorff, P. ; Kristiansen, K.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 231-236

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Mass spectrometric analysis of peptide mixtures may lead to ambiguous results when it is possible to change from one peptide chain to another during the interpretation of the spectra. This kind of ambiguity can be eliminated by submission of part of the sample to one cycle of Edman degradation, followed by comparison of the results obtained for this preparation with those obtained for the nondegraded sample. Combination of this procedure with the use of deuterated derivatives has allowed an unambiguous interpretation for two mixtures of synthetic peptides.

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URL: http://dx.doi.org/10.1002/bms.1200010406

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Field desorption mass spectrometry of ten medicinal carbamates (1974)

Rouse, Doris J. ; Brent, David A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 256-262

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The field desorption mass spectra of ten medicinal carbamates - meprobamate, mebutamate, carisoprodol, emylcamate, bethanechol chloride, styramate, hydroxyphenamate, mephenesin carbamate, methocarbamol and chlorphenesin carbamate - were run and compared with their published electron impact spectra. Of the ten compounds run only emylcamate did not give a field desorption mass spectrum. All others gave abundant molecular ions, with the exception of bethanechol chloride which has a quarternary ammonium group and gave a field desorption spectrum characteristic of compounds possessing such a functional group. No general characteristic fragmentation was attributed to the carbamate function in the field desorption mode. However, the ease of obtaining abundant molecular ions or quasimolecular ions makes the field desorption method a valuable complementary technique to electron impact studies of carbamates.

Additional Material: 9 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200010409

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The determination of sequence information in homologously related proteins by mass spectrometry (1974)

Dell, Anne ; Morris, Howard R. ; Williams, Dudley H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 269-273

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: An azurin, a small respiratory copper protein from the bacterium Pseudomonas fluorescens biotype G, has been studied by mass spectrometry to determine sequence information. The study of homologously related proteins by mass spectiometry is particularly attractive, since the correct nature of major parts of the deduced sequences can be confirmed by comparison with the sequences of the protein from related organisms. An oxidized tryptohan residue has been identified amongst the products from a cyanogen bromide digest of this wild type azurin. In the same digest, a product is also found to arise from cleavage of the peptide chain at the C-terminal side of the same tryptophan residue. These results are rationalized.

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URL: http://dx.doi.org/10.1002/bms.1200010411

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Sweet, David P. ; Shapiro, Robert H. ; Albersheim, Peter

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 263-268

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectral data for the primary fragmentation of partially ethylated alditol acetates have been tabulated in order to allow easy reference for the identification of these polysaccharide derivatives. Sodium borodeuteride is used in all the aldose to alditol reductions, since the presence of a single deuterium label on C-1 greatly increases the information available in the mass spectrum and allows some identifications to be made which would not otherwise be possible. The primary fragmentations of these derivatives are analogous to those of the partially methylated alditol acetates, with each fragment shifted to a higher m/e value by fourteen mass units for each ether linkage contained in the fragment. The secondary fragmentation is also very similar, being characterized by the loss of acetic acid or ketene, or, less frequently, by the loss of ethanol or acetaldehyde. Coupled with the chromatographic retention time data for the partially ethylated alditol acetates tabulated elsewhere, the unambiguous mass spectral identification makes this derivative an excellent choice as a complementary derivative to the partially methylated alditol acetates for polysaccharide analysis. The utility of the partially ethylated alditol as a routine analytical derivative is further enhanced by the almost identical procedures required for synthesis of the ethyl and methyl derivatives. Through the combined use of these derivatives, most of the possible linkage isomers of the seven common aldoses of plant cell wall polysaccharides can be resolved, identified and quantitated.

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URL: http://dx.doi.org/10.1002/bms.1200010410

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Characterization of cytosine nucleosides by mass spectrometry (1974)

Liehr, J. G. ; von Minden, D. L. ; Hattox, S. E. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 281-285

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectra of most nucleosides of cytosine exhibit molecular ions of low abundance, rearranged ions base + 2H in greater abundance than the companion species base + H, and a characteristic and abundant ion which corresponds to base + C2HO from the sugar. Deuterium, oxygen-18 and substituent labeling showed the presence of C-1′, 2′, H-2′ and O-4′ in the latter ion, which led to a proposed mechanism of formation involving opening of the sugar ring and recyclization between O2 and C-2′ with expulsion of water. Primary driving force for the reaction is due to resonance stabilization promoted by unshared electrons from N4, which results in diminished abundance in the case of imino isomers and derivatives which contain electron-withdrawing groups at N4, and enhanced abundance resulting from methylation at N4. Data for 24 nucleosides are presented and discussed in terms of the determination of nucleoside structure.

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URL: http://dx.doi.org/10.1002/bms.1200010413

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. ix

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010417

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Metabolism of branched medium chain length fatty acid: I - ω-oxidation of sodium dipropylacetate in ratsAbbreviations: DPA = dipropylacetate; BSA = N,O-bis-(trimethylsil)acetamide; TMCS = trimethylchlorosilane. (1974)

Kuhara, Tomiko ; Matsumoto, Isamu

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 291-294

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The metabolism of sodium dipropylacetate (a newly developed anticonvulsant) was investigated in rats, and two metabolites were found in urine of rats which received dipropylacetate. The metabolites were identified as 2-n-propyl-5-hydroxypentanoic acid and 2-n-propylglutaric acid, respectively, by low and high resolution mass spectrometry. Synthetic 2-n-propylglutaric acid, when administered to rats, was not oxidized further and was excreted intact in urine. These data clearly show that ω-oxidation is involved in the metabolism of sodium dipropylacetate and that 2-n-propylglutaric acid, the end product of ω-oxidation, does not serve as a substrate for β-oxidation.

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Limits of detection of carbon-13 labelled drugs and their metabolites in human urineAbbreviation used: PDB = Belemnitella americana (‘Peedee Belemnite’). (1974)

von Unruh, Gerd E. ; Hauber, David J. ; Schoeller, Dale A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 345-349

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The precise isotopic analysis of carbon by means of differential comparison of CO2 samples is applied to neutral, acid c and basic extract fractions of human urine. It is shown that the standard deviation of the analytical procedure, including sample preparation steps, is about 1% or 0.001 atom % excess carbon-13, but depends some what on the fraction considered. Day to day variations (expressed as standard deviations) in the isotopic composition of the urine fractions are generally less than 2.8%, 1.4% and 3.9% for the neutral, acidica and basic fractions, respectively, although the effect of unusual dietary inputs can be recognized. The ingestion of 23 μg excess carbon-13 in the form of isotopically labelled aspirin is shown to perturb significantly the isotopic composition of the acidic urine fraction which, for a 24 hour collection period, had a mass of 570 mg C. Because only 0.01% of the fraction was consumed by isotopic analysis, further extensive analysis would be possible. It is concluded that carbon-13 tracer experiments generally should be arranged to provide at least 5 × 10-5 g excess 13C/g carbon in any fraction which is to be used for lable detection.

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A method of analysis of dansylamides in mixtures by mass spectrometryAbbreviation: Dansyl = dimethylaminonaphthalene-5-sulphonyl. (1974)

Addeo, F. ; Malorni, A. ; Marino, G. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 363-364

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: The mass spectra of a mixture twenty dansyl derivatives of biogenic amines were run using low energy electron impact. This method appears to be useful for the analysis of amines present in biological materials.

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

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Topics: Chemistry and Pharmacology

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Mass spectrometric studies of thyroxine and related compounds. Trimethylsilyl derivatives (1974)

Lawson, A. M. ; Ramsden, D. B. ; Raw, P. J. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 374-380

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Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: The mass spectra of the trimethylsilyl derivatives of thyroxine and sixteen related compounds are reported. In addition to deiodinated analogues and iodinated tyrosines, the latter include a series of thyroacetic and thyropropionic acids and one thyroformic acid compound. Their spectra are discussed in terms of their fragmentation and utility for qualitative and quantitative estimation by gas chromatography - mass spectrometry.

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Mass spectrometry of the methyl ethers of isomeric hydroxychlorobiphenyls - potential metabolites of chlorobiphenyls (1974)

Jansson, B. ; Sundström, G.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 386-392

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: The mass spectra of synthetic methoxychlorobiphenyls have been investigated. These substances are of interest as reference compounds in studies of the metabolism of chlorobiphenyls. Some characteristic fragmentation patterns have been found, useful for differentiation between the 2-, 3- and 4-methoxychlorobiphenyl isomers. Thus, mass spectra of 2-methoxychlorobiphenyls show large fragments at [M - CH3Cl]+., while those of 4-methoxy compounds differ from 3-methoxy isomers by the presence of significant [M - CH3]+ fragments in the former.

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Identification of explosives by chemical ionization mass spectrometry using water as reagentAbbreviations: HMX (Octogen) = 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane; RDX (Hexogen, Cyclonite) = 1,3,5-Trinitro-1,3,5-triazacyclohexane; PETN = Pentaerythrytoltetranitrate. (1974)

Yinon, Jehuda

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 393-396

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Notes: Chemical ionization mass spectra of four explosive compounds have been obtained by using water as reagent gas. The compounds are 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane, 1,3,5-trinitor-1,3,5-triazacyclohexane, pentaerythritol tetranitrate, and an explosive which has been used in letter bombs, containing the two latter compounds and a plasticizer. The chemical ionization H2O mass spectra were recorded at an ion source temperature range of 170 to 225°C, a probe temperature range of 160 to 265°C and a reagent gas (H2O) pressure range of 0.07 to 0.10 Torr. Unlike in chemical ionization using methane or isobutane, chemical ionization H2O spectrum of these compounds provides a method for obtaining quasimolecular peaks. Adduct ion peaks like [M + H3O]+, [M + H5O2]+, [M + NO]+ and [M + NO2]+ are also observed in the chemical ionization H2O mass spectra of these compounds. Chemical ionization H2O mass spectra provide thus a better means of explosive identification.

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Carbon isotopic fractionations associated with acetic acid production by Acetobacter suboxydans (1974)

Rinaldi, Gianfranco ; Meinschein, W. G. ; Hayes, J. M.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 412-414

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Acetobacter suboxydans, strain 8.3, was grown using ethanol, made by the hydration of ethylene, as the sole energy source. After the microorganism had oxidized some of the ethanol to acetic acid, the unassimilated alcohol and produced acetic acid were isolated from the supernatant. Carbon isotopic analyses of these compounds and the starting ethanol show: (1) the methyl carbon of the starting alcohol is enriched in carbon-13 by 4.6% relative to the hydroxyl carbon, (2) the starting alcohol contains 2% less carbon-13 than the unassimilated ethanol and (3) the carboxyl carbon of the acetic acid excreted by the A. suboxydans is enriched by 3.8% in carbon-13 relative to the methyl carbon. These results support earlier findings which indicate that organisms preferentially utilize compounds enriched in carbon-12 and tend to concentrate carbon-12 in the reduced carbons relative to the oxidized carbons of metabolic products.

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Comparison of the field desorption, chemical ionization and electron impact mass spectra of some steroids (1974)

Haskins, N. J. ; Games, D. E. ; Taylor, K. T.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 423-424

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The electron impact, chemical ionization and field desorption mass spectra of seven steroids showing varying stability to electron impact have been compared.

Additional Material: 1 Ill.

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Mass spectra of compounds of biological interest, Volume 1 to 3, edited and compiled by S. P. Markey, W. G. Urban and S. P. Levine. USAEC TID-26553-P1, 2, 3. National Technical Information Service, U.S. Department of Commerce, Springfield, Virginia, 22161. 1974. pp. 1226. $28.80 (paper), $6.75 (microfiche) (1974)

Budde, William L.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 427-428

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URL: http://dx.doi.org/10.1002/bms.1200010613

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News (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. ix

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URL: http://dx.doi.org/10.1002/bms.1200010615

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 428-428

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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URL: http://dx.doi.org/10.1002/bms.1200010101

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Editorial (1974)

Millard, Brian J. ; Fenselau, Catherine

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xi

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URL: http://dx.doi.org/10.1002/bms.1200010102

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Separation and characterization of isomeric substituted nucleosides by gas chromatography and mass spectrometryAbbreviations used: TMS (trimethylsilyl); TFA (trifluoroacetyl); TBDMS (t-butyldimethylsilyl). (1974)

Quilliam, M. A. ; Ogilvie, K. K. ; Westmore, J. B.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 78-79

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Notes: The 3′- and 5′-O-t-butyldimethylsilyl derivatives of thymidine and deoxyadenosine have characteristically different mass spectra and can be separated by gas chromatography.

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The collection and analysis of volatile hydrocarbon air pollutants using a timed elution chromatographic technique linked to a computer controlled mass spectrometer (1974)

Perry, R. ; Twibell, J. D.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 73-77

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The difficulty of collecting volatile hydrocarbons, such as benzene, from street air in a form suitable for subsequent analysis is overcome by the use of a time-based elution procedure. By linking this technique to a gas chromatograph-mass spectrometer-data system, a rapid analysis is possible for low concentrations of collected material. Among advantages of this novel sample introduction procedure are the facility for collecting organic materials without interference from water vapour and their subsequent introduction into the g.c.-m.s. system without the use of any auxiliary solvents. Consequently the mass spectrometer can be used continuously on-line enabling the more volatile materials, normally masked by solvents, to be examined. This procedure is illustrated by the measurement of benzene and other hydrocarbon levels in street air (London). Following gas chromatographic separation the hydrocarbons can be identified by library search facilities attached to the mass spectrometer.

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Forthcoming events (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xiv

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URL: http://dx.doi.org/10.1002/bms.1200010119

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Mass spectrometry of 16,16′-O-permethylated 17-ketosteroidsAbbreviations used: A (androsterone); EA (epiandrosterone); E (etiocholanolone); DHA (dehydroandrosterone); DHEA (dehydroepiandrosterone); 11 OH-A (11 β-hydroxyandrosterone); 11 OH-E (11 β-hydroxyetiocholanolone). (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. xv

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URL: http://dx.doi.org/10.1002/bms.1200010120

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Reagent gases for G.C.-M.S. analyses (1974)

Jelus, Barbara L. ; Munson, Burnaby ; Fenselau, Catherine

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 96-102

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Notes: Several reagent gases and mixed reagent gases for high pressure ion-molecule reaction ionization of samples have been investigated for use in gas chromatography-mass spectrometry analyses. The common g.c. carrier gases and their mixtures with other gases such as isobutane, ammonia, tetramethylsilane, hexafluoroacetone and nitric oxide, were studied. These reagents were used to enhance the molecular ion intensity and to simplify the spectra of steroidal alcohols and the trimethylsilyl ethers of biologically important compounds.

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Studies in organic mass spectrometry: XVSande, C. Van de; Vandewalle, M. Bull. Soc. Chim. Belges 1973, 82, 775. - mass fragmentographic identification of epinine in adrenal medulla and as a product of an in vitro enzymic methylation (1974)

Claeys, M. ; Verzele, M. ; Vandewalle, M. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 103-108

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Notes: The presence of epinine in adrenal medulla and in reaction mixtures of enzymic in vitro experiments is proven by mass fragmentography. Derivatization of catecholamines, suitable for gas chromatographic analysis is discussed. The perfluoropropionates were selected for mass fragmentography.

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Leclercq, P. A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 109-114

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Notes: Using methylsulphinyl carbanion as base. methylation of 17-ketosteroids with methyl iodide not only converts hydroxy into methoxy groups, but also replaces both C-16 hydrogen atoms by methyl groups. These permethyl derivatives are very stable, have excellent properties for gas chromatographic separation and fragment characteristically upor electron impact. The mass spectra of a number of these derivatives are discussed.

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High resolution field desorption mass spectrometry: II - glycosides (1974)

Schulten, H-R. ; Games, D. E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 120-123

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The high resolution field desorption mass spectra of a number of glycosides are described. In all cases the spectra enabled molecular weights and elemental formulae to be established, and the presence of fragment ions due to cleavage of the sugar groups provides considerable assistance in the identification of sugar and aglycone moieties. The [M + 23Na]+ ion was the base peak in the spectrum of the sodium salt of testosterone glucuronide, and the presence [M + 39K]+, [M + 41K]+ and [M + 23Na]+ ions in the spectra of other glycosides are attributed to the presence of their sodium or potassium salts as impurities.

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Direct (non-chromatographic) quantification of drugs and their metabolites from human plasma utilizing chemical lonization mass spectrometry and stable isotope labeling: Quinidine and lidocaineAbbreviations: MEGX = monoethylglycinexylidide; GX = glycinexylidide. (1974)

Garland, W. A. ; Trager, W. F. ; Nelson, S. D.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 124-129

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Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: Preliminary results are reported for the quantitative determination of the antiarrhythmic agents quinidine and lidocaine in human plasma by combined isobutane chemical ionization mass spectrometry and stable isotope labeling. The concentration of monoethylglycinexylidide, a known metabolite of lidocaine, was also determined using this method. In the procedure used, stable isotope analogs of the materials to be determined were added to serial plasma samples. The plasma was then made basic and extracted with benzene. The residue after evaporation of the solvent was placed directly into the mass spectrometer via the direct insertion probe and the spectrum determined. In this manner the above named compounds could readily be quantitated without recourse to either derivitization or further purification.

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Mass spectrometric determination of butobarbitone and its metabolites in man (1974)

Gilbert, J. N. T. ; Powell, J. W.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 142-144

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

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Notes: The urinary excretion of butobarbitone and its metabolites has been studied quantitatively using combined gas chromatography-mass fragmentography, tuned to ions at m/e 169 and 184. After a single oral dose (200 mg) to healthy male volunteers, unchanged drug (7 to 9%), 3′-hydroxybutobarbitone (22 to 27%), 3′-oxobutobarbitone (14 to 18%) and the 3′-carboxylic acid (4 to 8%), were found. In all cases, the maximum rate of excretion was in or near the third 12 hour urine.

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Watson, J. Throck ; Falkner, Fred C. ; Sweetman, Brian J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 156-157

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Source: Wiley InterScience Backfile Collection 1832-2000

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URL: http://dx.doi.org/10.1002/bms.1200010214

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Chemical ionization and high resolution electron impact mass spectra of 1,6-anhydro-3,4-O-isopropylidene-β-D-talopyranosePart of a series Specific Isotropic Labeling of Sugars: Applications in Mass-Spectral Analysis. For the previous report in this series. see Ref. 1. (1974)

Horton, Derek ; Jewell, Jon S. ; Just, Ernst K. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 145-153

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Notes: The high resolution, electron impact mass spectrum of 1,6-anhydro-3,4-O-isopropylidene-β-D-talopyranose, together with those of its derivatives having specific deuterium substitution at C-2, at C-3, at C-2 and C-3, and in the isopropylidene group, is considered in detail and compared with the ammonia and isobutane mediated chemical ionization spectra of these five compounds. From the elemental compositions of the fragment ions and mass number shifts upon deuterium incorporation, the origin of the hydrogen atoms in each of the fragments is traced, and a detailed scheme of the main fragmentation. pathways is presented.

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Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200010301

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High resolution mass spectroscopic analysis of methylated tolbutomide derivatives (1974)

Sabih, Khalid

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 163-165

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Notes: The methyl derivative of tolbutamide, obtained by the action of dimethyl sulfate, has been subjected to g.c.-m.s. at high resolution. From the mass spectrum it is deduced that methylation of the sulfonamide nitrogen atom has occurred. During the loss of SO2 from the molecular ion, aryl rearrangement to both oxygen and nitrogen occurs in the ratio of 1:2.

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Field desorption mass spectrometry of the B vitamins: Pyridoxal, pyridoxamine, their phosphates, and thiamine (1974)

Sammons, Martin C. ; Bursey, Maurice M. ; Brent, David A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 169-171

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: Characterization of the B vitamins. pyridoxal, pyridoxamine, their phosphates and thiamine salts by electron impact mass spectrometry is difficult. A new technique, field desorption, is applied in ionizing these molecules for mass spectrometric analysis Characterization of these compounds by field desorption has the advantage that in each case the most intense peak in the spectrum is formed without fragmentation.

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Mass spectrometry of synthetic oligopeptides N, O-permethylated, N-acetylated derivativesAbbreviation: DMF = dimethylformamide. (1974)

Haegele, K. D. ; Holzer, G. ; Parr, W. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 175-189

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Mass spectra of a series of stable isotope derivatives aided a structure elucidation study of an amino acid amide (Tyr-NH2) and the following family of synthetic oligopeptides: Gly-Tyr-NH2, Gly-Gly-Tyr-NH2, Gln-Gly-Gly-Tyr-NH2, Gln-Gln-Gly-Gly-Tyr-NH2, Ala-Gln-Gln-Gly-Gly-Tyr-NH2, Ser-Ala-Gln-Gln-Gly-Gly-Tyr-NH2 and Lys-Ser-Ala-Gln-Gln-Gly-Gly-Tyr-NH2. This series of peptides was synthesized by classical methods. N,O-permethylated, N-acetylated derivatives were synthesized to provide sufficient volatility for mass spectrometry. Various combinations of stable isotope derivatives (CH3CO + CH3, CD3CO + CH3, CH3CO + CD3, CD3CO + CD3) confirmed proposed fragmentation pathways and corroborated hypothetical ion structures. This family of oligopeptides corresponds to the C-terminus of scotophobin.

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Phospholipids in pulmonary alveolar proteinosis (1974)

Einolf, W. Noel ; Fenselau, Catherine

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 195-198

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Gas chromatography-mass spectrometry has been used to identify the phosphate diester backbones of two classes of phospholipids previously unrecognized in washings from human lungs. Washings were analyzed from two patients with pulmonary alveolar proteinosis and also from two pairs of normal lungs washed postmortem. α-Glycerophosphorylglycerol and α-glycerophosphorylinositol were identified in all four cases following hydrolysis of the fatty acid esters and treatment with trimethylsilylating reagent.

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The amino acid sequences of the tryptic peptides of the cowpea strain of tobacco mosaic virus proteinThe following abbreviations are used in the text: CPA = carboxypeptidase A; CPB = carboxypeptidase B-DFP.The following additional abbreviations and symbols are used in the diagrams: Th = thermolytic peptide; C = chymotryptic peptide; ⇀ = amino acids determined by the Edman degradation procedure; ⇁ = amino acids determined by mass spectrometry; ↽ = amino acids determined by carboxypeptidase A or B; → = amino acids determined by partial acid hydrolysis. (1974)

Heller, Stephen R. ; Fales, Henry M. ; Milne, G. W. A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 207-208

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010313

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Studies of O-substituted oxime-trimethylsilyl ester derivatives of some metabolically-important oxocarboxylic acidsAbbreviations: BO-TMS, EO-TMS and MO-TMS are respectively the benzyl, ethyl and methyl O-substituted oximes; BSA = N, O-(trimethylsilyl)acetamide. (1974)

Lawson, A. M. ; Chalmers, R. A. ; Watts, R. W. E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 199-205

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectra of the methyl-, ethyl- and benzyl-oxime trimethylsilyl ester derivatives of sixteen oxocarboxylic acids are reported. They are discussed both in terms of their fragmentation and their utility for use in studies of inborn errors of metabolism. Several applications where these derivatives have proved of value are presented.

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Organic contaminants in the District of Columbia water supply (1974)

Scheiman, M. A. ; Saunders, R. A. ; Saalfeld, F. E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 209-211

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Thirty-two organic contaminants have been identified in District of Columbia drinking water. These contaminants include aliphatic and aromatic hydrocarbons, chlorocarbons, bromine-containing compounds, alcohols and ketones. The concentration of each constituent identified was less than one part per million. The organic contaminants were extracted from the water samples with a 1:1 mixture of carbon disulfide (CS2) and methylene chloride (CH2Cl2). Each constituent was identified by its gas chromatographic retention time and by its mass spectrum.

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Characterization of dipeptides by electron impact and chemical ionization mass spectrometryAbbreviation : ACA = acetylacetone. (1974)

Schier, G. M. ; Halpern, B. ; Milne, G. W. A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 212-218

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The components of mixtures of dipeptides can be identified from the electron ionization and chemical ionization mass spectra of their N-acetylacetonyl methyl ester derivatives without prior separation. The pyrolytic conversion of peptide trimethylanilinium salts to their methyl esters in the direct insertion probe of a mass spectrometer was found to be most suitable for the derivatization of dipeptides in mixtures.

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Field desorption mass spectrometry of metabolites of the anticancer drug cyclophosphamide (1974)

Schulten, H.-R.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 223-230

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Some of the known and important metabolites of cyclophosphamide and the parent drug itself were investigated by low and high resolution field desorption mass spectrometry. The potential of the relatively new analytical method for the determination of the molecular weight and elemental formulae of drugs and drug metabolites was exemplified. This holds for pure, synthetic compounds as well as for contaminated extracts from biological sources. In addition, by thermally-/field-induced fragmentation, diagnostic fragment ions could be produced, providing valuable structural information. Further, an indication on how to distinguish [M]+. and [M + H]+ ions in field desorption mass spectrometry is given. The ability to identify these ions unambiguously is critical for interpretation. Finally, the potential of the method as applied to drug and drug metabolite mixtures is evaluated. The results indicate that field desorption mass spectrometry is a promising tool in metabolism studies.

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Gas chromatographic and high resolution mass spectrometric determination of phenylbutazone in blood (1974)

Sabih, Khalid

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 252-255

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: High resolution mass spectrometry has been used to identify phenylbutanone in plasma extracts. Concentrations of 5 μg/ml of the drug in plasma have been determined by a gas chromatographic method with a standard deviation of ±0.3%.

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Rees, M. W. ; Short, Margaret N. ; Self, R. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 237-251

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The amino acid sequences of the thirteen tryptic peptides of the cowpea strain of tobacco mosaic virus (Cowpea TMV) protein were determined by a combination of the mass spectrometric and Edman degradation procedures. In order to complete the amino acid sequences, a number of the tryptic peptides were further digested with chymotrypsin, thermolysin and carboxypeptidases A and B. The peptide fragments were separated and purified by the use of ion exchange chromatography. Sephadex chromatography and paper electrophoresis.The total number of amino acid residues in the Cowpea TMV protein was found to be 161 as opposed to the 158 found for the type TMV protein, and asparaginyl-arginine was the only tryptic peptide common to both proteins. All peptides used for mass spectrometry were first N-acetylated and then permethylated using methyl iodide and methyl sulphinyl carbanion or potassium t-butoxide dissolved in dimethyl sulphoxide.

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Gas phase analytical resolution of enantiomeric amines as diastereomeric amides. Gas chromatography-mass spectrometry of α-phenylbutyramides, α-phenylpropionamides and α-chlorophenylacetamides (1974)

Gilbert, Mary T. ; Gilbert, John D. ; Brooks, Charles J. W.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 274-280

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Representative phenylalkylamines (six enantiomeric pairs) and amino acid methyl esters (five enantiomeric pairs) have been examined by gas chromatography-mass spectrometry, in the form of their N-(R)-α-phenylbutyryl, N-(S)-α-phenylpropionyl- and N-(R)-α-chlorophenylacetyl derivatives. In most cases, satisfactory gas chromatographic resolution of the diastereomeric amides has been achieved on both SE-30 and OV-17 stationary phases. The phenylbutyramides and phenylpropionamides gave the more informative mass spectra (for characterization of the amines) but molecular ions were observed in all instances.

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Fales, H. M. ; Heller, S. R. ; Milne, G. W. A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 295-295

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200010416

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Identification of nitrosophenols by mass spectrometryAbbreviations: SCOT = support-coated open tubular columns; BSTFA = N, O-bis-(trimethylsilyl) trifluroacetamide. (1974)

Knowles, M. E. ; Gilbert, J. ; McWeeny, D. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 286-290

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Characteristic mass spectroscopic data for the identification of ten nitrosophenols is presented. The use of TMS derivatives for gas chromatography-mass spectrometry of 4-nitrosophenols is discussed, together with the use of copper chelates for obtaining direct insertion spectra of 2-nitrosophenols. The fragmentations of nitrosopher ols also show ions derived from their quinonemonoxime tautomers, even under gas chromatography-mass spectrometry conditions, indicating that isomerization occurs in the mass spectrometer. An anomalous elimination of nitrogen from these nitrosophenols has been shown to be a facile reduction of the nitroso moiety which takes place in the ion source of the mass spectrometer.

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Recent advances in pyrolysis mass spectrometry of complex biological materialsThe research reported in this paper is supported by the Foundation for Fundamental Research on Matter (F.O.M.) and the Ministry of Health and Environmental Hygiene in the Netherlands, and has been presented in part at the 2nd International Symposium on Mass Spectrometry in Biochemistry and Medicine, Milan, Italy, 24th to 26th June 1974. (1974)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974)

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200010501

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Mass fragmentography of morphine and 6-monoacetylmorphine in blood with a stable isotope internal standardAbbreviations used: 6-MAM = 6-monoacetylmorphine; TFA = trifluoroacetyl; TFAA = trifluoroacetic anhydride. (1974)

Ebbighausen, W. O. R. ; Mowat, J. H. ; Stearns, H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 305-311

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A mass fragmentographic method for the estimation of the estimation of free and bound morphine and free 6-monoacetylmorphine in blood has been developed. It uses stable isotope internal standards and has a sensitivity of about 1 ng per ml or about 100 times better than ordinary gas chromatography. The focusing on specific high molecular fragments of the molecules gives high specificity to the assay and the stable isotope internal standards allow correction for losses occuring in the preparative steps of the analysis. A sensitive, specific method for monoacetylmorphine is particularly valuable since this compound seems to be a specific metabolite of heroin.

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Meuzelaar, Henk L. C. ; Kistemaker, Piet G. ; Posthumus, Maarten A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 312-319

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Nonvolatile biological materials, such as biopolymers or even whole cells, can be made accessible to mass spectrometric analysis by pyrolysis techniques. In principle, this enables differentiation, classification and identification of these materials. Moreover, pyrolysis mass spectrometry can provide a general picture of the chemical composition and structure of the sample analysed. During the past few years we have investigated several pyrolysis techniques in combination with different mass spectrometric methods. These investigations included Curie point pyrolysis, infrared laser pyrolysis, low voltage electron impact ionization, field ionizationIn co-operation with Professor Dr H. D. Beckey and Dr H.-R. Schulten, University of Bonn, Germany. and pyrolysis field desorption. Pyrolysis reactions were performed either at the gas inlet or directly at the ion source. The relative merits of these different experimental approaches are discussed. Additionally, examples of various applications, such as computer identification of bacteria and qualitative analyses of biopolymers, are given.

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The use of solid probe chemical ionization mass spectrometry and gas chromatography-chemical ionization mass spectrometry in quantitation of drugs in biological fluids. Determination of tolbutamide and its metabolites in human plasmaAbbreviations used: T = tolbutamide; OHT = 1-p-hydroxymethylbenzenesulfonyl-3-butylurea; COOHT = 1-p-carboxyphenylsulfonyl-3-butylurea. (1974)

Matin, Shaikh B. ; Knight, James B.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 323-328

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Quantitative methods based on chemical ionization mass spectrometry are described for the determination of tolbutamide, a sulfonylurea, and its metabolites from human plasma. The sulfonylureas are extracted from the acidified plasma and then N-1 methylated with diazomethane. The methylated compounds can be subjected to gas chromatography where they are partially cleaved to the corresponding N-1 methylated sulfonamides. Alternatively, the methylated compounds can be introduced into the ion source by means of a solid sampler. The sulfonylureas upon evaporation from the solid sampler or the formed sulfonamide and the parent sulfonylurea upon elution from the gas chromatographic column are subjected to chemical ionization with methane as the reactant gas. The [M + H]+ ions formed are measured quantitatively with respect to the deuterium substituted internal standards. It is suggested that the technique of introducing biological extracts into the ion source via a solid probe may be applied for the quantification of compounds that are unstable under gas-liquid chromatographic conditions. Both the gas chromatographic and the non gas chromatographic methods provided excellent and comparable results. The plasma level-time profile of tolbutamide and its metabolites in a diabetic patient following the administration of 1.0 g tolbutamide intravenously is presented.

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Characterization of the isomeric dialkylbarbituric acids formed by the reaction of barbiturates with diazoalkanes (1974)

Harvey, D. J. ; Nowlin, J. ; Hickert, P. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 340-344

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The reaction of barbituric acids with diazoalkanes (diazomethane and diazoethane) gives the N,N′-dialkylbarbituric acids as the major products. Gas chromatograms of the reaction products show up to four additional peaks. These have been shown by mass and proton magnetic resonance spectrometry to be produced by the two isomeric N,O-dialkylbarbituric acids (1,4- and 1,2-dialkylbarbituric acids) and the two O,O′-dialkyl isomers.

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Mass fragmentographic studies of sulfur compounds: The thienylthiaalkanes (1974)

Foster, Norman G. ; Shiu, Diana Wong-Kiu ; Higgins, Robert W.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 297-304

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Fragmentation studies of the mass spectra of 24 high purity compounds of importance in a study of fossil fuels are described. The substances include eleven 1-(2-thienyl)-1-thia-, six1-(2-thienyl)-3-thia, and seven1-(2-thienyl)-4-thiaalkanes in the molecular weight range 158 to 270. Rearrangement peaks are prominent in all spectra and form the base peaks for the 1-thia- and 4-thia- compounds. The 3-thia- compounds are somewhat perverse in exhibiting weaker rearrangement peaks, and large ion intensities, including base peaks, at masses typical of alkyl fragments, alkenyl fragments, or ions more characteristic of the thiaalkanes (aliphatic sulfides). The major fragment ions are discussed and their use in differentiating subclasses is described. Low ionization voltage data is presented in support of suggested mechanisms of fragmentation.

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Determination of phenformin in biological fluids using chemical ionization mass spectrometryAbbreviations used: P = phenformin; PD2 = α-dideuteriophenethyl biguanide. (1974)

Matin, Shaikh B. ; Karam, John H. ; Forsham, Peter H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 320-322

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: A method for the quantification of phenformin, an oral hypoglycemic biguanide, from biological fluids based upon gas chromatography and chemical ionization mass spectrometry, is reported. Phenformin is quantitatively cyclized to the 2-substituted-4-trifluoremethyl-2,6-diamino-1,3,5-S-triazine when acylated with trifluoroacetic anhydride. This cyclized product was measured with respect to the deuterium substituted phenformin. The plasma levels achieved following the administration of a therapeutic dose of phenformin to a diabetic subject are reported.

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Mass spectrometric identification of an N-oxide formed by incubation of N,N-dimethyl-5H-dibenzo[a,d]cycloheptene-Δ5,γ-propylamine with rat liver microsomes (1974)

Belvedere, G. ; Rovei, V. ; Pantarotto, C. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 329-331

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: On incubation with rat liver microsomes, N,N-dimethyl-5H-dibenzo[a,d]cycloheptene-Δ5,γ-propylamine is converted to the N-oxide. The identification of this metabolite has been achieved by the use of gas chromatography, mass spectrometry and thin-layer chromatography.

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Studies on the mass fragmentographic determination of plasma estriol (1974)

Adlercreutz, H. ; Nylander, P. ; Hunneman, D. H.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 332-339

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Three mass fragmentatographic methods for the determination of unconjugated estriol in pregnancy plasma and unconjugated and conjugated estriol in plasma of nonpregnant women after estriol administration were developed and tested as to their reliability and practicability. The methods were found to fulfil appropriate reliability criteria especially with regard to specificity. Unconjugated estriol could be assayed without prior chromatography in late pregnancy plasma, but a chromatographic step was needed for plasmas with a low estriol titre, and both a methylation step and chromatography is needed to achieve the required specificity if plasma conjugated estriol is determined or if assays are carried out following estriol administration. Unconjugated estriol in normal late pregnancy plasma was found in concentrations from 4.3 to 9.3 μg/l. The highest value recorded, 16.3 μg/l, was found in a prediabetic subject with mild hypertension, who delivered a child weighing 4150 g by Cesarean section in the 39th week. Low values were found in severe hypertension and in toxemia, and in general the results from the pathological material investigated seemed to correlate well with the clinical findings. However, only a few samples (five to ten) can be processed so rapidly that the results can be obtained the same day, which in addition to the expensive and complicated instrumentation limits the usefulness of the methods in routine clinical chemistry.

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Identification of an atypical constitutent of a clandestine opiate (1974)

Herman, Gary J. ; Kan, Man-Na N.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 350-351

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: An unusual morphine analog was extracted and separated from an opium-like sample. The high resolution mass spectrum of the unknown substance confirmed the empirical formula as C17H18O2NCl. Mass spectra and retention factor values in thin-layer chromatography of both unknown and authentic standards were compared, which lead to the identification of the unknown as β-chloromorphide.

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Pyrolysis mass spectrometric studies on nucleic acids (1974)

Posthumus, M. A. ; Nibbering, N. M. M. ; Boerboom, A. J. H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 352-357

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ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Two different mass spectrometric techniques have been used to analyse the products resulting from Curie-point pyrolysis of nucleic acids: low voltage ionization quadrupole mass spectrometry and high resolution field ionization mass spectrometry. The spectra obtained with both techniques are in good agreement with one another. As already indicated by the low resolution spectra, the high resolution spectra proved that most of the peaks originate from the carbohydrate moiety of the nucleic acid. Micrograms of DNA/RNA can be distinguished very easily by use of these key fragments, although the bases themselves are not found. Some significant pyrolysis mechanisms are proposed.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010512

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A quantitative method of sample loading for field desorption mass spectrometry (1974)

Olson, Keith L. ; Cook, J. Carter ; Rinehart, Kenneth L.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 1 (1974), S. 358-362

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Details

ISSN: 1052-9306

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A quantitative method for loading nanogram samples onto field desorption emitter wires is described. Sample consumption is reduced and problems with emitter wettability are overcome by freezing microliter droplets onto the emitters. Using this technique, good spectral data are obtained from 10 to 50 ng of material. Field desorption sensitivity measurements are reported for neomycin B, adenosine and cholesterol. Evaluation of the nonquantitative dipping technique previously employed reveals poor and nonreproducible sample loading efficiency.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200010513

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Paper (German National Licenses)

Fulltext

84

Electronic Resource