ZIB

1

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Masthead (1982)

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982)

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010101

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2

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Mass spectrometry of amino steroids and steroidal alkaloids (1982)

Budzikiewicz, Herbert

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982), S. 125-168

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Additional Material: 9 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010203

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3

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Field desorption mass spectrometry: Applications (1982)

Wood, G. W.

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982), S. 63-102

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Additional Material: 13 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010106

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4

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Announcement (1982)

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982), S. 199-199

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010205

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5

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Mass spectral studies of lipid topology in biological membranes (1982)

Costello, Catherine E.

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982), S. 169-198

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Additional Material: 12 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010204

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6

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Determination of drug bioavailability by mass spectrometry (1982)

Vink, Jan

New York, NY [u.a.] : Wiley-Blackwell

Mass Spectrometry Reviews 1 (1982), S. 349-393

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ISSN: 0277-7037

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology , Physics

Additional Material: 21 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/mas.1280010403

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7

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Biotransformation of epomediol. I - isolation and identification of main metabolites in the rat (1982)

Ventura, Paolo ; Selva, Antonio

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 18-21

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The identification of biotransformation products of the new choleretic drug epomediol in rat has been performed by means of mass spectral, proton magnetic resonance and infrared techniques. The drug was administered perorally or intravenously; urine, bile and faeces were collected and the metabolites isolated. In urine, three metabolites were found in addition to the unchanged drug, namely: 1,3,3-trimethyl-2-oxabicyclo[2.2.2]octan-6-hydroxy-7-one, 1,3-dimethyl-2-oxabicyclo[2.2.2]octan-6,7-hydroxy-10-methanol and 1,3,3-trimethyl-2-oxabicyclo[2.2.2.]octan-6-β-glucuronide-7-ol. In bile only the glucuronide and the unchanged drug were found. Analogously, in faeces the glucuronide and the drug were also identified, but only in trace amounts. This fact may suggest the presence of an enterohepatic circulation of the drug.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090105

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8

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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ISSN: 0306-042X

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.1200090101

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9

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The identification of (E)-2-methylglutaconic acid, a new isoleucine metabolite, in the urine of patients with β-ketothiolase deficiency, propionic acidaemia and methylmalonic acidaemia (1982)

Duran, M. ; Bruinvis, L. ; Ketting, D. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 1-5

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The identification of (E)-2-methylglutaconic acid, a ‘new’ metabolite of isoleucine, is described. The substance was detected in urine samples from patients with propionic acidaemia, methylmalonic acidaemia and so-called β-ketothiolase deficiency; in the majority of cases together with N-tiglylglycine. (E)-2-Methylglutaconic acid is thought to be the end product of the 3-methylcrotonyl-CoA carboxylase-catalysed carboxylation of tiglyl-CoA. Prerequisites for the quantitative gas chromatographic analysis of the unstable 2- (and 3-) methylglutaconic acid ditrimethylsilyl ester are given.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090102

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10

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Single dose kinetics of deuterium labelled Δ1-tetrahydrocannabinol in heavy and light cannabis users (1982)

Ohlsson, Agneta ; Lindgren, Jan-Erik ; Wahlén, Anita ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 6-10

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Deuterium labelled Δ1-tetrahydrocannabinol was administered intravenously (5.0 mg) and by smoking (10.0 mg) to five heavy and four light marihuana users. All subjects smoked an estimated amount of 8.6-9.9 mg Δ1-tetrahydrocannabinol. The plasma levels of Δ1-tetrahydrocannabinol were followed for 48 hours and in two subjects for 72 hours after administration. The systemic availability after inhalation calculated from the area under curve values was in the range of 27±10% for the heavy users and 14±1% for the light users. There was little difference between the groups with regard to the amount of smoked Δ1-tetrahydrocannabinol or plasma levels and area under curve values obtained after i.v. administration. Thus, it seems likely that the statistically significant difference in systemic availability of smoked Δ1-tetrahydrocannabinol was due to a more efficient smoking by the heavy users. It is also indicated that heavy users prefer slightly higher Δ1-tetrahydrocannabinol plasma levels than light users. Based on the area under curve values after i.v. administration, a plasma clearance of 760-1190 ml min-1 was calculated. The elimination half-life of Δ1-tetrahydrocannabinol is more than 20 hours. The present results do not suggest that tolerance or sensitivity to Δ1-tetrahydrocannabinol in heavy users is readily achieved.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090103

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11

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The use of hexamethylenetetramine for nitrogen-15 isotope abundance measurements with an organic mass spectrometer (1982)

Cottrell, R. C. ; Young, P. J. ; Purchase, R. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 43-44

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A method has been developed which utilizes an organic mass spectrometer for the measurement of 15N isotope enrichment in ammonia, based on conversion into hexamethylenetetramine. Commercially available equipment and minimal computing facilities were required. Ion current ratios were measured with a precision of 3% or better over a wide dynamic range by automatic voltage switching and the use of a single (retractable) Faraday Cup detector linked, with a preamplifier and the standard instrument main amplifier, to a digital voltmeter. Enrichment of 0.01 atom % above natural abundance was detected with 90% confidence, using only five replicate determinations.

Additional Material: 1 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090109

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12

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Identification and quantitation of methotrexate and methotrexate metabolites in clinical high-dose therapy by high-pressure liquid chromatography and field desorption mass spectrometryPresented in part at the American Society for Mass Spectrometry, 28th Annual Meeting on Mass Spectrometry and Allied Topics, New York (1980). (1982)

Przybylski, Michael ; Preiß, Joachim ; Dennebaum, Reiner ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 22-32

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: High-pressure liquid chromatography in combination with field desorption mass spectrometry as techniques of high specificity and sensitivity have been applied to the identification and quantitation of the anticancer drug methotrexate and its metabolites which occur in clinical high-dose therapy. Field desorption mass spectra of methotrexate and several methotrexate and folic acid derivatives, when investigated as free acids or ammonium salts, yield abundant protonated molecular ions and a consistent pattern of structurally significant fragments. High-pressure liquid chromatographic separation of methotrexate metabolites was performed on reverse-phase, C-18 columns using a volatile, ammonium bicarbonate/acetate containing mobile phase that was especially suited for the field desorption mass spectral analysis of isolated metabolites, and provided the definite identification of 7-hydroxymethotrexate and 4-[[2,4-diamino-6-pteridinyl]methylmethylamino]-benzoic acid in serum and urine of patients treated with high-dose methotrexate. The high intensity and stability of the [MH]+ ions was found suitable for the quantitation of methotrexate and related folate analogues by field desorption mass spectrometry. A synthetic methotrexate derivative, methotrexate-γ-(2-hydroxy)ethylamide was used as internal standard for the quantitative determination of methotrexate in serum and urine. In a study to comparatively assess the potential of specific quantitation methods, serum and urine levels of methotrexate and its major metabolite, 7-hydroxymethotrexate were determined by (i) an enzyme immunoassay, (ii) reverse phase high-pressure liquid chromatography and (iii) field desorption mass spectrometry. Results obtained from four patients with osteogenic sarcoma receiving high-dose methotrexate/leucovorin rescue therapy consistently show the sustained elimination of 7-hydroxymethotrexate over several days, thus indicating the utility of specifically monitoring this nephrotoxic metabolite, at massive methotrexate doses.

Additional Material: 10 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090106

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13

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Sequence determination of a peptide with 55 amino acid residues by Edman degradation and field desorption mass spectrometry (1982)

Katakuse, Itsuo ; Matsuo, Takekiyo ; Matsuda, Hisashi ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 64-68

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The amino acid sequence of a polypeptide was determined by a new method combined with field desorption (FD) mass spectrometry and Edman degradation. The polypeptide, N-terminal BrCN fragment of Streptomyces erythraeus lysozyme with 55 amino acid residues, was cleaved specifically into several peptide fragments by trypsin and chymotrypsin. The molecular weights of subpeptides were determined by FD mass spectrometry. Peptide mixtures were subjected to Edman degradation successively and PTH amino acids released were measured by high performance liquid chromatography. The amino acid sequence was calculated by a computer program from molecular weights of subpeptides and PTH amino acids.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090204

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14

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Studies on the metabolism of procarbazine by mass spectrometry (1982)

Kuttab, Simon H. ; Tanglertpaibul, S. ; Vouros, Paul

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 78-84

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectrometric properties of procarbazine and some of its breakdown products were examined using isotopic labeling and high resolution mass spectrometry. A specific intramolecular methyl group transfer, induced by electron impact, was used diagnosticaliy to distinguish between two isomeric derivatives. The mass spectrometric information was used for identification of the in vivo metabolites of procarbazine in rat. Minimum sample manipulation was used due to the inherent instability of the suspected metabolites. The azo compound, N-isopropyl-α-(2-methylazo)-p-toluamide was identified as the principal circulating metabolite of procarbazine.

Additional Material: 6 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090208

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15

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Hydroxypolychlorodibenzofurans in technical pentachlorophenol: Electron capture negative ion chemical ionization mass spectra of alkoxypolychlorodibenzofurans (1982)

Deinzer, M. ; Griffin, D. ; Miller, T. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 85-90

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A mixture of hydroxypolychlorodibenzofurans was isolated from technical pentachlorophenol. The alkyl ethers were prepared, and analyzed by fused silica capillary column gas chromatography electron capture negative ion chemical ionization mass spectrometry. The appearance of intense molecular ion peaks for the alkyl ethers apparently depends on the ring position of alkoxy substitution. Loss of chlorine atoms from the ring, followed by protonation of the resultant anion as the alkyl group is eliminated, is postulated on the basis of deuterium labeling experlments. Evidence is also presented for the presence of a hydroxyheptachlorodibenzodioxin in technical pentáchlorophenol.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090209

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16

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Benzo[a]pyrene glucuronide and sulfate conjugate characterization by field desorption mass spectrometry (1982)

Deutsch, Joseph ; Gelboin, Harry V.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 99-102

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The field desorption mass spectral behaviour of benzo[a]pyrene metabolites were studied. Each of the phenol, diol, quinone and diol-epoxide metabolites of benzo[a]pyrene showed a single peak corresponding to the molecular ion. The water soluble glucuronides and sulfate conjugated metabolites showed protonated and cationized molecular ions. With the glucuronides, three peaks were observed and the abundance of these peaks may be indicators for characterization of the three isomeric glucuronides.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090304

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17

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Quantitative determination of nitroglycerin in human plasma by capillary gas chromatography negative ion chemical ionization mass spectrometry (1982)

Ottoila, Pekka ; Taskinen, Jyrki ; Sothmann, Aslak

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 108-110

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A quantitative method for determination of nitroglycerin in human plasma was developed. Nitroglycerin and the internal standard (butane-1,2,4-triyl trinitrate) were extracted from plasma with pentane. The extracts were analysed by gas chromatography mass spectrometry using fused silica capillary columns and electron capture negative ion chemical ionization. The quantitation limit of the method was about 50 pg ml-1. Linear calibration curves were obtained in the range of 50-1600 pg ml-1. Precision at the level of 100 pg ml-1 was 4%.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090306

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Deuteromethylation of dimethylxanthines: A gas chromatographic mass spectrometric method for confirmatory analysis in horse urine extracts (1982)

Houghton, E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 103-107

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The methylated xanthines caffeine and/or theobromine are commonly encountered in drug-positive samples from racehorses and their metabolism and excretion in the horse and their analysis in urinary extracts has been of particular interest in this laboratory. Due to their polar nature the dimethylxanthines theobromine, theophylline and paraxanthine give unsatisfactory gas chromatographic performance and require derivatization prior to analysis by gas chromatography mass spectrometry. The present paper describes a simple deuteromethylation procedure to render the compounds amenable to analysis by gas chromatography mass spectrometry. Characteristic ions in the mass spectra of the isomeric monotrideunteromethyl-dimethylxanthines provide a means of distinguishing between them. The discriminatory evidence provided by mass spectrometric analysis of the deuteromethylated products is compared to that obtained by gas chromatographic mass spectrometric analysis of the butylated products.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090305

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19

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Secondary ion mass spectra of the neuropeptides leucine-enkephalin and methionine-enkephalin (1982)

Westmore, J. B. ; Ens, W. ; Standing, K. G.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 119-124

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Positive and negative secondary ion mass spectra obtained by bombardment of thin films of leucine-enkephalin and methionine-enkephalin with a pulsed beam of Cs+ ions of energy 5-15 keV were recorded using a time-of-flight mass spectrometer. Many of the secondary ions are metastable. The spectra contain a wealth of information, including the following important features: (i) ions characteristic of the intact molecule, from which the molecular weight may be deduced; (ii) ions diagnostic of the amino acid composition of the peptide; (iii) ions diagnostic of the sequence of amino acids in the peptide.

Additional Material: 5 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090309

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Pyrolysis field ionization mass spectrometry of pharmaceutical plant mucilages (1982)

Schulten, H.-R. ; Bahr, U. ; Wagner, H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 115-118

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The combination of pyrolysis and field ionization (Fl) mass spectrometry is used to characterize and identify mucous polysaccharides isolated from plant material (crude drugs). Oven pyrolysis is simply performed inside the ion source using a commercial direct introduction system. About 20μg of sample is thermally degraded by heating linearly from 50°C to 600°C at a rate of 0.4°C s-1.The thermal evaporation profiles and FI mass spectra of the pyrolysates of five pharmaceutically used plant mucilages were recorded and found to differ significantly from one another. The mass spectra show almost exclusively peaks corresponding to molecular ions of pyrolysis products which are characteristic for polysaccharides and demonstrate the presence of aldohexoses, aldopentoses and deoxyhexoses. The ratios of the characteristic signals of the dehydration products of these three groups of sugar subunits give semiquantitative information on the composition of these polysaccharides. The relative abundances of the key signals were compared with quantitative data obtained by classical methods, e.g. gas chromatography, and found to be a useful, indicative value.Comparison of the FI spectra of the mucilage pyrolysates with spectra of reference samples of mono- and oligosaccharides allows the identification of subunits in the sugar polymers. This is supported by the occurrence of their typical pyrolysis products which were assigned in previous pyrolysis studies.

Additional Material: 6 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090308

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Dealkylation during electron impact mass spectrometric analysis of N- monoalkylated porphyrin methyl esters (1982)

Smith, Andrew G. ; Farmer, Peter B.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 111-114

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The N-monoethylated, N-monoethylated and N-mono-1-propylated homologues of mesoporphyrin IX dimethyl ester and the corresponding methylated and 1-propylated homologues of coproporphyrin III tetramethyl ester have been prepared. Substituted porphyrins in a series could be distinguished from each other and from the parent porphyrin by their dication absorption spectra. All compounds gave molecular ions of varying intensities during electron impact mass spectrometry but thermal N-dealkylation to mesoporphyrin IX or coproporphyrin III methyl esters occurred readily and it was difficult to obtain spectra not showing fragmentation ions derived from this process. The compounds serve as models for the ‘green pigments’ produced in vivo by the action of some drugs and illustrate the problem of dealkylation during their analysis by electron impact mass spectrometry.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090307

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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ISSN: 0306-042X

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.1200090401

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The use of gas chromatography mass spectrometry in the evaluation of the synthesis of 3-dimethylaminomethyl-2-(3′, 4′-dichlorophenyl)bicyclo[2.2.2.] octane. A novel drug with potential antidepressant activity (1982)

Mallen, David N. B. ; Smith, Julie M.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 125-129

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Gas chromatography mass spectrometry was used to characterize compounds observed throughout the synthesis of a cis-fused 3′,4′-dichlorophenyl bicyclo-octane, a potential CNS acting drug substance. An ortho chloro-effect identified the isomeric 2′,4′-dichlorophenyl impurities.

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090310

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Mass spectra of 1,6:2,3- and 1,6:3,4-dianhydro-β-D-hexopyranose derivatives: Formation of cluster ions assisted by participation of neighbouring acyloxy groups (1982)

Kadentsev, Valentin I. ; Kaymarazov, Alexander G. ; Chizhov, Oleg S. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 130-134

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Chemical ionization and electron impact mass spectra of 1,6:2,3-and 1,6:3,4-dianhydro-β-D-hexopyranose derivatives are reported. The methane and isobutane chemical ionization mass spectra of both positional and configurational isomers differ significantly, while the electron impact mass spectra of stereoisomers are hard to discern. Examination of the isobutane chemical ionization mass spectra indicates that only those isomers containing the acyloxy group and the oxirane ring in the trans position give stable [M+C4H9]+ ions, otherwise these ions are of negligible abundance. This observation is interpreted in terms of participation of the acyloxy group in oxirane ring opening. This feature of the chemical ionization mass spectra can be used for stereochemical assignment.

Additional Material: 3 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200090311

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The amino acid sequences of eleven tryptic peptides of papaya mosaic virus protein by electron ionization mass spectrometry (1982)

Parente, A. ; Short, M. N. ; Self, R. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 141-145

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Eleven of the fourteen tryptic peptides of papaya mosaic virus protein have been sequenced by electron ionization mass spectrometry using chemical and enzymic hydrolyses and mixture analysis as required. Mid-chain cleavages of N—C bonds produced secondary ion series which allowed up to 16 residues to be sequenced without further hydrolysis. Mixture analysis on hydrolysis products enabled a 24 residue tryptic peptide to be sequenced from the data recorded in a single mass spectrum.

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Detection of fragment genesis in the mass spectrometer: Amino acid sequence analysis by DADI/MIKE, linked scan and collisional activation mass spectrometry. 6 - Peptides containing trifunctional amino acids (1982)

Steinauer, René ; Schlunegger, Urs Peter

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 153-157

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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 sequence in tripeptides containing trifunctional amino acids has been analysed by direct analysis of daughter ions/mass analysed ion kinetic energy (DADI/MIKE) and B/E linked scan spectrometry. Collision induced dissociations in the first and second field free regions of a mass spectrometer with reversed geometry were also investigated.

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Gas chromatographic mass spectrometric determination of myo-inositol in humans utilizing a deuterated internal standardA preliminary account of part of the present work was presented at 4th International Conference on Stable Isotopes, Jülich, 23-27 March, 1981. (1982)

Andersen, Jan Rud ; Larsen, Elfinn ; Harbo, Helge ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 135-140

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The isotopic dilution technique was used for determining the content of myo-inositol in human urine, plasma and haemolysed erythrocyte samples. A deuterated myo-inositol, synthesized from inosose-2 by base-catalysed exchange of hydrogens by deuterium, followed by reduction of the inosose with 2H2, was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions selected for monitoring were m/z 210 and m/z 214, which are characteristic and abundant fragment ions from unlabelled and hexadeuterated myo-inositolhexa-acetate, respectively. Calibration curves from water, urine, plasma and haemolysed erythrocytes show parallel, linear responses in the ratio between analyte and internal standard in the area of interest (0.2-2.0).

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Field desorption and fast atom bombardment mass spectrometry of hydroxamate containing siderophores (1982)

Dell, A. ; Hider, R. C. ; Barber, M. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 158-161

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Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: Field desorption and fast atom bombardment mass spectrometric procedures have been applied to the analysis of hydroxamate containing siderophores as their iron (III) complexes. Molecular ion species predominate in both field desorption and fast atom bombardment spectra. The results reported demonstrate the potential of these soft ionization techniques for the characterization of novel siderophores and siderophores metabolites.

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Identification and quantitative determination of m-hydroxyphenylglycol in mammalian urine (1982)

Crowley, Jan R. ; Couch, Margaret W. ; Williams, Clyde M. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 146-152

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Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: m-Hydroxyphenylglycol (MHPG) has been identified in mammalian urine by gas chromatography mass spectrometry selected ion monitoring. (2H0)MHPG and (2H5)MHPG were synthesized for use as authentic sample and internal standard, respectively. After acid hydrolysis or treatment with sulfatase, the glycol was extracted from urine with ethyl acetate, converted to its tris-pentafluoropropionyl (PFP) derivative and identified by comparison of the retention times and relative intensities of the characteristic ions, m/z 592, m/z 428 and m/z 415, with those from the authentic sample. Using the internal standard the following quantitative results were obtained: 10 normal human adults excreted 7 ng MHPG mg-1 creatinine (range 2-18) as a sulfate conjugate. Ten rats excreted 0.8 μg day-1 (range 0.5-1.1) of MHPG also in the conjugated form. Urinary m -hydroxymandelic acid (MHMA) was also measured quantitatively. The ratio MHMA:MHPG was 1:1 in the rat and 6:1 in the human. This indicates that the overall reductive pathway of m-octopamine and m-synephrine metabolism is more important in the rat than in the human. o-Hydroxyphenylglycol (OHPG) and the three isomeric monomethoxy phenylglycols could not be detected in human or rat urine by these techniques.

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Trying to arrange a difficult marriage: A report on the workshop on ‘liquid chromatography mass spectrometry’, held in montreux, switzerland, 22-23 October 1981 (1982)

Arpino, Patrick J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 176-180

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: This report reviews the data presented at the first meeting ever held on the new analytical technique of combined liquid chromatography mass spectrometry. It briefly discusses the 14 oral communications and five discussion sessions heard during the two day workshop. Trends in future liquid chromatography mass spectrometry work are delineated.

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Studies of ergot alkaloids using high-performance liquid chromatography-mass spectrometry and B/E linked scansA preliminary report of this work was presented at the American Society for Mass Spectrometry, 29th Annual Conference on Mass Spectrometry and Allied Topics, Minneapolis, Minnesota (1981), Abstract No. RAMOA10 and the Joint Pharmaceutical Analysis Group in London May 1981.1 (1982)

Eckers, Christine ; Games, David E. ; Mallen, David N. B. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 162-173

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A crude extract from an ergot fermentation broth has been examined by high-performance liquid chromatography mass spectrometry (LC/MS). The [M + 1]+ ions formed from the mixture under chemical ionization conditions have also been studied using B/E linked scans with and without collision induced dissociation. Data obtained from high-performance liquid chromatography mass spectrometry have been used to identify 11 alkaloids in a mixture of at least 18 unknown molecules. B/E Linked scan spectra obtained with and without collision activated dissociation from pure samples proved useful in differentiating isomeric alkaloids and in providing stereochemical information. Problems were encountered in application of these latter techniques to studies of the crude extract; in particular in the identification of isomers and in the presence of peaks arising from fragment ions formed from higher mass alkaloids present in the mixture.

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Mass spectroscopy of natural products. XVI - Mass spectroscopic studies of thiazinylergolines (1982)

Schmidt, J. ; Seifert, K. ; Härtling, S. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 174-175

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Notes: The fragmentation behaviour of D-6(6-alkyl-4H-1,3-thiazin-4-on-2-yl)-8-methoxycarbonylergolines-I is described. Using collision induced dissociation (CID) mass spectrometry it could be established that the structure of the heterocyclic substituent at N-6 of the ergoline is retained during the fragmentation.

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Forthcoming mettings (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 180-180

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Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200090410

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Brain S. Middleditch, Stephen R. Missler, Harry B. Hines. Mass spectrometry of priority pollutants. Plenum press, New York, 1981. ISBN 0 306 405059. £29.50 (1982)

Piet, G. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 180-180

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URL: http://dx.doi.org/10.1002/bms.1200090411

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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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.1200090501

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Continuous 2HHO determination in H2O solution by a computer-controlled mass spectrometer (1982)

Pungor, E. ; Klibanov, A. M. ; Cooney, C. L. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 181-185

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Direct interfacing of a membrane based mass spectometer separator to an aqueous solution of water-saturted gas stream allows continuous monitoring of a vareity of dissolved volatile compunds. Even if the solution is saturated with atmoshpheric gases, we demonstrate that deuterated water concentration in aqueous solution can be measured over concentration ranges of interest to physiological studies, with an estimated, extrapolated detection limit less than the natural abundance.

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Simultaneous determination of phenobarbital and p-hydroxyphenobarbital and their stable isotope labeled analogs by gas chromatography mass spectrometry (1982)

Van Langenhove, A. ; Biller, J. E. ; Biemann, K. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 201-207

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Additional Material: 2 Ill.

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A gas chromatographic mass spectrometric assay for plasma trifluoperazine concentrations following single doses (1982)

Midha, K. K. ; Roscoe, R. M. H. ; Hall, K. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 186-190

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Notes: A gas chromatographic mass spectrometric assay using selected ion monitoring is described which permits the determination of trifluoperazine in plasma at concentrations ranging from 0.078 to 5.0 ng ml-1. It relies on the extraction of trifluoperazine and the internal standard, prochlorperazine or the tetradeuterated analogue of trifluoperazine, form basified plasma with a n-pentane/2-propanol solvent mixture. Following the evaporation of organic solvent, the residue is reconstituted in a small volume of methanol. Suitable aliquots were anlysed by the combined technique of gas chromatography/electron impact mass spectrometry with a data system. The described procedure is specific and enables the quantitation of 78 pg ml-1 of the drug with a coefficient of variation 〈7%. The method has demonstrated sufficient sensitivity to permit pharmacokinetic and bioavailability studies after a single 5 mg oral dose.

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Methodology for the identification of the urinary metabolites of the analgesic-narcotic antagonist, codorphone, by gas chromatography mass spectrometryA portion of this work was presented at the 29th Annual Conference on Mass Spectrometry and Allied Topics, Minneapolis, MN (1981) Abstract No. RPMOB3. (1982)

Evans, James V. ; Leeling, Jerry L. ; Helms, Richard J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 191-200

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Notes: Methodology is presented for the identification of codorphone and its metabolites in urine samples using gas chromatography mass spectrometry. The procedure focuses on the clean-up of biological samples and a derivatization technique suitable for these samples. Sep-Pak C-18 cartridges were employed in the clean-up procedure permitting the biological sample to be derivatized in a relatively small volume of reagents. The derivatizaion procedure incorporated a one-step trimethylsilyloxime reaction to prevent enol formation while simultaneously derivatizing free hydroxyl groups with the excess trimethylsilylimidazole present in the reaction mixture. This was followed by the addition of BSTFA directly to this reaction mixture to complete derivatization of any metabolities possessing dealkylation of the nitrogen. Using this derivatization scheme, synthetic metabolities were analyzed by gas chromatography mass spectrometry, and their mass spectra were characterized emphasizing the diagnostic fragment ions observed in the spectra. To illustrate the usefulness of this methodology, a urine sample obtained from a dog that had been dosed with codorphone was analyzed by gas chromatography mass spectrometry, and the metabolites were identified by comparison to the mass spectra of the synthetic derivatives.

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Fast atom bombardment mass spectrometry of the angiotensin peptides (1982)

Barber, Michael ; Bordoli, Robert S. ; Sedgwick, R. Donald ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 208-214

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectra obtained from angiotensins I and II (a decapeptide and an octapeptide, respectively) are presented. Both positive and negative ion spectra are obtained using fast atom bombardment. The sequence information obtained is confirmed by metastable scanning and by the analysis of acetyl derivatives of these peptides.

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C. Merritt Jr and C. N. McEwen(EDS). Mass spectrometry, part B. Marcel Dekker, New York, 1980. $49.75 (1982)

Rose, M. E.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iii

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URL: http://dx.doi.org/10.1002/bms.1200090508

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Product news (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iv

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Source: Wiley InterScience Backfile Collection 1832-2000

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URL: http://dx.doi.org/10.1002/bms.1200090509

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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URL: http://dx.doi.org/10.1002/bms.1200090601

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Microbore high-performance liquid chromatography mass spectrometryA preliminary report of some of these studies was presented at the American Society for Mass Spectrometry, 29th Annual Conference on Mass Spectrometry and Allied Topics, Minneapolis, Minnesota (1981), Abstract No. RAMOA 6 and to the Joint Pharmaceutical Analysis Group in London, May 1981. (1982)

Games, David E. ; Lant, Michael S. ; Westwood, Steven A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 215-224

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Notes: The use of microbore liquid chromatography columns for high-performance liquid chromatography/mass spectrometry provides improved sensitivity for interfaces of the direct liquid introduction and moving belt types. In the latter case the use of the technique also assists in the handling of mobile phases containing a high percentage of water. Methods for improving the efficiency of microbore columns made from PTFE are described together with the use of a manual column switching technique to assist in some of the problems encountered due to column overload with microbore liquid chromatography columns. The utility of microbore liquid chromatography/mass spectrometry is illustrated by the analysis of an aqueous solution of phenolic compounds.

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Mass spectrometry of some modified nucleosides of the pyrimidine and purine series (1982)

Mikhailopulo, I. A. ; Kalinichenko, E. N. ; Zaitseva, G. V. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 225-232

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: The mass spectral fragmentation patterns of some pyrimidine and adenine nucleosides modified in a carbohydrate moiety have been investigated. The position of the chlorine atom in a carbohydrate moiety is characterized in the mass spectrum by the following peaks. In the case of pyrimidine nucleosides the location of the chlorine atom at C-3′ leads as a general fragmentation pathway to a loss of a Cl radical to yield ion a, which further decomposes into ions h, n and j having the composition base plus 30,68 and 56 mass units, respectively. The location of the chlorine atom at C-2′ involves initial elimination of HCI to form the ion(s) p which are transformed into the characteristic O2,2′-cyclo ion r. The latter is one of the most abundant ions in the mass spectra of O2,2′-cyclonuleosides. In the case of adenine chlorodeoxynucleosides the principal fragmentation routes from the molecular ion involve (i) a loss of a Cl radical and, further, the elements of H2O and formaldehyde 5′-CH2O result in the formation of the characteristic Ion n (b+68mass units); (ii) a reverse sequence of transformations of the molecular ion leading to ion n. An intense ion d containing a C-1′-C-2′ fragment of the carbohydrate ring with a substituent at C-2′is of considerable interest in elucidating the isomeric structure of the adenine chlorodeoxynucleosides. The same ion d is informative in establishing the isomeric structure of adenine 2′,3′- and 3′,5′-anhydronucleosides.

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Metabolism of 4-substituted-N-ethyl-N-methylanilines: Chromatographic and mass spectrometric identification of N-oxidation metabolic products formed in vitro (1982)

Cowan, David A. ; Patterson, Laurence H. ; Damani, Lyaquatali A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 233-240

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Notes: The electron impact and isobutane and ammonia chemical ionization mass spectral characteristics of the N-oxidation products of a series of 4-substituted-N-ethyl-N-methylanilines are described. The thermolability and the relative non-volatility of N-oxides of this type of tertiary aromatic amine makes their unequivocal identification by gas chromatography and electron impact mass spectrometry difficult. Mass spectral identification is facilitated by employing CI mass spectrometry where, under appropriate conditions, the N-oxides give intense protonated molecular ions. Chromatographic, electron impact and chemical ionization mass spectrometric evidence is presented which shows that these 4-substituted tertiary anilines undergo metabolic N-demethylation, N-de-ethylation and N-oxidation in vitro. The suitability of these tertiary aromatic amines as model substrates for mechanistic studies on C- and N-oxidation is discussed.

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Fragmentation patterns of trimethylsilyl derivatives of dihydrodiol glucuronides produced by metabolism of naphthalene and 1-methyl-N-naphthylcarbamateMention of a trademark or proprietary product does not constitute a guarantee or warranty of the product by the US Department of Agriculture and does not imply its approval to the exclusion of other products that may also be suitable. (1982)

Bakke, J. E. ; Feil, V. J. ; Struble, Craig

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 246-251

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Mass spectra from trimethylsilyl derivatives of three dihydrodiol glucuronides are reported. The aglycone moieties were characterized to be 1,2-dihydro-1,2-dihydroxynapthalene, 5,6-dihydro-5,6-dihydroxy-1-napthole (glycosidic linkage through 5 or 6 position) and a dihydrodihydroxymethylsulfonylnaphthalene.

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Mass spectrometric measurement of end-tidal xenon concentration for clinical stable xenon/computerized tomography cerebral blood flow studies (1982)

Dhawan, V. ; Goldiner, P. ; Ray, C. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 241-245

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: We have demonstrated the feasibility of using a compact dedicated mass spectrometer to monitor end-tidal xenon concentration in human subjects during stable xenon computerized tomography measurements of regional cerebral blood flow. End-tidal carbon dioxide concentration is monitored simultaneously and noninvasively without degrading the dynamic response to xenon. For clinical regional cerebral blood flow studies we employed a Nuclide 3-60-G Sectorr mass spectrometer with a 3 in radius, 60° magnetic sector and a variable (0-5000 V) ion accelerating potential. The required high vacuum (10-7 Torr) was achieved and maintained by means of a turbomolecular pump. A needlemetering valve was incorporated into an anesthesia mask connector, and exhaled gases were transported to the mass spectrometer via a 6 ft length of Teflon tubing (1/16 in i.d.). Molecular flow conditions between the sample and analysis chambers were provided by use of a gold foil leak (0.0005 in. hole). At an inlet pressure of 400 m Torr (achieved by means of the needle valve), the inlet system was characterized by a gas transport lag-time of 1.3 s and a rise-time constant of 85 ms. Xenon (doubly charged ion: m/z 68) and carbon dioxide (doubly charged ion: m/z 22) were monitored alternately at 75 ms intervals. Our experience with mass spectrometry has demonstrated the feasibility of using a compact dedicated instrument for accurately and non-invasively monitoring end-tidal xenon concentration in a clinical setting.

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Mass spectral characterization of iopamidol (1982)

Clerici, Angelo ; Traldi, Pietro ; Grandi, Maurizio ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 257-264

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The mass spectrometric characterization of Iopamidoi (1) a new nonionic hydrosoluble contrast medium widely used in myelography and angiography, has been obtained by the analysis of the mass spectra of some derivative compounds using different ionization methods. The data obtained from the different techniques were complementary. Conclusive structural information has been gained with the fast atom bombardment technique.

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Differentiation of α- from γ-glutamyl dipeptides by chemical ionization mass spectrometry (1982)

Nagasawa, Herbert T. ; Magnan, Sanne D. J. ; Foltz, Rodger L.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 252-256

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Chemical ionization mass spectrometry has been shown to be a useful method for the differentiation of α- and γ-glutamyl dipeptides where the C-terminal amino acids are simple α-amino or α-imino acids without additional functional groups. The α-glutamyl dipeptides lost one and two molecules of H2O from the protonated molecular ion to give fragment ions at [MH—H2O]+ and [MH—2H2O]+. With the γ-glutamyl dipeptides, the characteristic fragment ions of highest intensities were the protonated pyroglutamic acid (pyrrolidone-5-carboxylic acid) ion at m/z 130, and a fragment ion corresponding to the protonated C-terminal amino acid. The procedure does not require derivatization of the dipeptide, and because only small sample sizes are needed it could prove useful for the characterization of synthetic samples and glutamyl dipeptides isolated and purified from biological sources.

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A. M. Lawson, C. K. Lim, W. Richmond (EDS). Current developments in the clinical applications of HPLC, GC and MS. Academic Press, London, 1980 (1982)

Chan, D. W.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iii

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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.1200090609

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Fast atom bombardment mass spectrometry of the large oligopeptides melittin, glucagon and the B chain of bovine insulinPresented in part at the Workshop in Biomolecular Mass Spectrometry, Cosenza, Italy, 6-10 September 1981. (1982)

Barber, Michael ; Bordoli, Robert S. ; Sedgwick, R. Donald ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 265-268

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Application of developments in the fast atom bombardment ion source and high field magnet technology are presented, which together have resulted in the ability to obtain mass spectra from involatile compounds with molecular weights in excess of 3000 daltons. Examples include resolved molecular species from melittin, glucagon and the oxidized form of the B chain of bovine insulin. It is concluded that there now exists a genuine requirement for extended mass range facilities to be available on a routine basis.

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Forthcoming meeting (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iv

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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.1200090612

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Fred W. McLafferty. Interpretation of mass spectra, third edition. University science books, Mill valley, California, 1980. pp. xvii + 303 (1982)

White V, Edward

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iii

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URL: http://dx.doi.org/10.1002/bms.1200090610

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Letter to the editors (1982)

Beynon, J. H. ; Cameron, D. ; Todd, J. F. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. iv

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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.1200090611

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

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URL: http://dx.doi.org/10.1002/bms.1200090701

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The application of stable isotopes in biomedical research (1982)

Haskins, N. J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 269-277

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Many of the ways in which stable isotopes are used in biomedical research are reviewed. The use of stable isotopes in stable isotope dilution assay, for metabolite identification and in pharmacokinetic studies, is discussed and relevant examples are given to illustrate the various points made. Isotope effects and their implications for future drug design are considered. Some of the toxicity problems associated with the use of stable isotopes are also considered. Finally, a brief subjective view of possible future advances is made.

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Thermal desorption mass spectrometry of organic salts (1982)

Yergey, Alfred L. ; Cotter, Robert J.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 286-292

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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 alkyl, alkyl/aryl and biologically important quaternary ammonium and phosphonium compounds have been obtained by a direct thermal process. No means of ionization other than the heating of a salt coated filament is used. The spectra consist primarily of even electron ions for which decomposition schemes involving four-center reactions are proposed. These spectra are similar to those obtained in fission fragment induced desorption, laser induced desorption and field desorption/collisional activation, but they are produced by a far simpler means.

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Effects of 20,25-diazacholesterol on cholesterol synthesis in cultured chick muscle cells: A radiogas chromatographic and mass spectrometric study of the post-squalene sector (1982)

Emmons, G. T. ; Rosenblum, E. R. ; Peace, J. N. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 278-285

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Radiogas chromatography, used in conjunction with mass spectrometry, has been used to analyze the sterol content of cultured chick muscle cells. Seven sterols, plus lanosterol, were detected. These sterols conformed to a linear biosynthetic pathway linking lanosterol and cholesterol. The reaction sequence is: C-14 demethylation, C-4 demethylation, Δ8 → Δ5 double bond rearrangement, Δ24 double bond reduction. When chick cells were treated with increasing concentrations of 20,25-diazacholesterol, components of this pathway and aberrant products accumulated. These accumulations suggest that diazacholesterol affects reductases, double bond isomerases and the C-14 demethylation enzymes of sterol biosynthesis.

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Analysis of molecular species of phospholipids by field desorption mass spectrometry (1982)

Sugatani, Junko ; Kino, Minoru ; Saito, Kunihiko ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 293-301

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Source: Wiley InterScience Backfile Collection 1832-2000

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Notes: Various glycerophospholipids including their trimethylsilyl and t-butyldimethylsilyl derivatives and cerebroside were analysed by field desorption mass spectrometry with a silicon emitter. Choline glycerophospholipids with diacyl residues and also alk-1′-enyl and acyl residues gave the readily interpretable field desorption mass spectra in which a sodium cluster ion [M + Na]+ was a base peak. As to phosphatidylethanolamine and cerebroside, a protonated molecular ion [M + H]+ was a base peak. The TMS and TBDMS derivatives gave a molecular ion [M]+. The field desorption analysis of natural phospholipids from myelin was carried out in comparison with the gas chromatographic mass spectrometric analysis.

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Chemical ionization mass spectrometry of amygdalin with ammonia gas (1982)

Cairns, Thomas ; Siegmund, Emil G.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 307-309

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Under ammonia chemical ionization conditions using the liquid chromatographic moving belt interface for sample introduction, molecular weight information has been observed for the cyanogenic glyceside, amygdalia (D-mandelonitrile-β-D-glucosido-6-β-D-glucoside). Additionally, the use of deuterated ammonia has permitted a detailed fragmentation pathway to be outlined via determinations of total acidic hydrogens.

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URL: http://dx.doi.org/10.1002/bms.1200090707

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A selected ion monitoring assay for dopamine and its metabolites using negative chemical ionization (1982)

Wood, Paul L.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 302-306

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A 4 min gas chromatographic run on 3% SP-2250 allows for the simultaneous gas chromatographic selected ion monitoring assay of dopamine, homovanillic acid, dihydroxyphenylacetic acid and 3-methoxytyramine after a one-step derivatization with pentafluoropropionic anhydride and hexafluoroisopropanol. A comparison of electron impact, positive chemical ionization and negative chemical ionization conditions indicated dramatic increases in sensitivity with negative chemical ionization. This assay has wide applications for the measurement of monoamines and their metabolites in biological samples.

Additional Material: 6 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200090706

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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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.1200090801

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Pulse injection, 13C tracer studies of lactate metabolism in humans during rest and two levels of exercise (1982)

Mazzeo, Robert S. ; Brooks, George A. ; Budinger, Thomas F. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 310-314

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: In order to determine the role of lactic acid as a metabolic substrate during exercise, the extent of its oxidation was studied using (13C)lactate under three different metabolic conditions in two subjects. During rest, easy exercise (work below the lactate inflection point), and hard exercise (work above the lactate inflection point), 100 mg of Na+-D,L(+)-2,3-(13C)lactate was injected via an indwelling catheter inserted in an antecubital vein. Blood as well as expired gas samples were collected up to 2 h post-injection. Subjects worked at average intensities of 53% and 74% VO2max during easy and hard exercise, respectively. During rest and easy exercise, blood lactate concentrations remained stable at 1-2 mM. During hard exercise, blood lactate increased to 3-4 times those observed at rest. Excretion of 13CO2 peaked much sooner and enrichment of 13C in CO2 was greater during both exercise intensities than during rest. Cumulative recovery of injected 13C as 13CO2 averaged 13.2 and 86.2% through 120 min during rest and easy exercise. Through 45 min of hard exercise, recovery of tracer as CO2 was the same as during a similar time point of easy exercise, 51.8%. The results support the contention that oxidation is the major fate of lactate during exercise.

Additional Material: 3 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200090708

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Detection of fluoroborate anion in water at ppb levels using negative ion field desorption mass spectrometry (1982)

Van der Greef, J. ; de Brauw, M. C. Ten Noever ; Zwinselman, J. J. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 330-332

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A method is described for the determination of fluoroborate anion in water using field desorption mass spectrometry in the negative ion mode. The fluoroborate anion can be determined at concentrations as low as 4 ppb and both the sensitivity and specificity of this method are compared with those of field desorption and fast atom bombardment mass spectrometry in the positive ion mode.

Additional Material: 3 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200090804

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Electron impact and methane, isobutane and ammonia chemical ionization mass spectra of peptide amides related to melanostatin (Pro-Leu-Gly-NH2) (1982)

Björkman, Svea

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 315-322

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Eighteen peptide amides related to Melanostatin, Pro-Leu-Gly-NH2, were studied by electron impact and methane, isobutane and ammonia chemical ionization mass spectrometry. In general the methane and isobutane chemical ionization spectra, which were qualitatively similar, gave more pertinent structural information than the electron impact spectra. In ammonia chemical ionization, both the peptide amides and their fragment ions reacted with unionized reagent gas to give protonated peptide amides together with some other fragments not observed in methane or isobutane chemical ionization. Moreover, a Melanostatin analogue containing a dehydroproline residue underwent aromatization and double bond reduction in chemical ionization, and the two reactions may possibly have been linked.

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Metabolism of isosafrole and dihydrosafrole in the rat (1982)

Klungsøyr, Jarie ; Scheline, Ronald R.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 323-329

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The urinary metabolites of isosafrole(1,2-methylenedioxy-4-propenylbenzene) and dihydrosafrole (1,2-methylenedioxy-4-propylbenzene) in the rat were identified using gas chromatographic mass spectrometric methods. Additionally, the amounts of the individual metabolites excreted were determined gas chromatographically. Metabolite excretion was 89% (isosafrole) and 97% (dihydrosafrole) of the dose in 72 h. Although isosafrole was metabolized by allylic hydroxylation and via the epoxide-diol pathway, demethylenation leading mainly to 1,2-dihydroxy-4-propenylbenzene was by far the most prominent reaction. This was similarly true with dihydrosafrole which was metabolized mainly to 1,2-dihydroxy-4-(1-propyl) benzene. The total amount of demethylenated metabolites formed were 92% (isosafrole) and 95% (dihydrosafrole) of the identified material.

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Gas chromatographic mass spectrometric determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma using the nitrogen-15 labelled compound as internal standard (1982)

Gerardin, A. ; Gaudry, D. ; Wantiez, D.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 333-335

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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 quantitative determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma by gas chromatography mass spectrometry has been developed. After addition of 1,2,3-propanetriol(15N)trinitrate as internal standard, plasma (1 ml) is extracted by a mixture of pentane and methyl acetate (90:10). The extracts are purified by partition between, first, the extraction solvent and a mixture of acetonitrile and water (60:40) and, secondly, the resultant aqueous phase and benzene. The solvent is evaporated to a small volume before injection. The fragment ions at m/z 46 and 47 are monitored for the measurement of the [NO2]+ and [15NO2]+ ions using electron impact ionization. The mean recovery (%) ±SD in blind plasma samples spiked with amounts in the concentration range 0.35-3.52 nmol I-1, was 97.4 ± 9.0 (n = 58). Within a day, recovery experiments gave rise to coefficients of variation of 9.6, 6.4 and 2.7% at the levels 0.44,0.88 and 11 nmol I-1, respectively. Concentrations in plasma down to about 0.2 nmol I-1 (50 pg mI-1) could be estimated. Percent recovery of duplicate determinations in the range 0.5-1.96 nmol I-1± SD was 99.4 ± 6.0 (n = 80).

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Determination of formaldehyde in biological tissues by gas chromatography/mass spectrometry (1982)

d'A. Heck, Henry ; White, Earl L. ; Casanova-Schmitz, Mercedes

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 347-353

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A quantitative method is described for the determination of formaldehyde in biological tissues by stable isotope dilution using gas chromatography/mass spectrometry. (13C2H2)Formaldehyde is used as the isotopic diluet. After tissue homogenization, derivatization is carried out in situ with pentafluorophenylhydrazine, followed by extraction and analysis using selected ion monitoring. The sensitivity of the technique is higher than that of conventional methods of formaldehyde analysis, enabling endogenous formaldehyde to be quantitatively analyzed in tissues, even in samples as small as 20 mg wet weight. The effects of exposure to airborne formaldehyde or to airborne methyl chloride on the formaldehyde concentrations of several tissues of Fischer-344 rats are reported.

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URL: http://dx.doi.org/10.1002/bms.1200090808

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Quantitative analysis of 5-fluorouracil and 5,6-dihydrofluorouracil in plasma by gas chromatography mass spectrometry (1982)

Aubert, C. ; Sommadossi, J. P. ; Coassolo, Ph. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 336-339

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: 5-Fluorouracil and 5,6-dihydro-5-fluorouracil were analysed in the plasma of patients by combined gas chromatography mass spectrometry. 5-Bromouracil was the internal standard. After extraction from plasma with an isopropanol-diethyl ether mixture (20/80) the components were pentylated and the derivatives produced extracted into diethyl ether. Electron impact mass spectrometry was used for the simultaneous quantitative determinations of 5-fluorouracil and 5,6-dihydro-5-fluorouracil (detection limit 10 ng mI-1 5-fluorouracil, 80 ng mI-1 5,6-dihydro-5-fluorouracil). Chemical ionization was utilized to measure 5,6-dihydro-5-fluorouracil concentrations 〈80 ng mI-1 (sensitivity 10 ng mI-1). The biological applicability of these two techniques was demonstrated by analysing plasma samples from patients after administration of 5-fluorouracil or 5′-deoxyfluorouridine by intravenous injections and infusions.

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Stable isotope methodology in a pharmacokinetic study of the interaction of theophylline and cimetidine (1982)

Vestal, Robert E. ; Thummel, Kenneth E. ; Musser, Beth ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 340-346

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Theophylline administered orally and (1, 3-15N,2-13C)theophylline administered intravenously in tracer quantities were used to investigate under steady-state conditions the interaction of theophylline with cimetidine in a patient with chronic obstructive pulmonary disease. Both compounds were quantified simultaneously by mass spectral-analysis after solvent extraction and high pressure liquid chromatographic purification of plasma samples. The assay is reliable and accurate to a plasma level of 50 ng mI-1 for the stable isotope tracer with a practical lower limit of detection of 10 ng mI-1.

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URL: http://dx.doi.org/10.1002/bms.1200090807

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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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.1200090901

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Field desorption mass spectrometry of cobalamine derivatives mixture analysis thermolytic reactions and comparison with fast atom bombardmentField Desorption Mass Spectrometry of Corrins Part V; for Part IV, see H. M. Schiebel and H.-R. Schulten, Naturwissenschaften 67, 256 ( 1980). (1982)

Schiebel, H. M. ; Schulten, H.-R.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 354-362

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: For cobyrinic acid heptamethylester derivatives, field desorption mass spectrometry can be used as a fast and sensitive analytical method for synthesis control in corrin chemistry. Since molecular ions are formed with high relative abundance, their identification in mixtures using accurate mass measurements and direct isotopic determination is feasible. Detailed structural information can be obtained by thermally-induced fragmentation of the organometallic compounds on the emitter surface. Consecutive loss of the axial ligands and the substituent in position 10 of the corrin ring is observed with increasing sample temperature. Furthermore, at higher emitter heating currents, the product of the elimination of the acetic acid side-chain from C-7 is found analogously as in preparative thermolysis. The field desorption study presented here allows not only the detection of thermally generated end-products but also of reactive intermediates and thus gives a specific insight into the mechanisms of thermolysis. A preliminary comparison of the field desorption and fast atom bombardment mass spectra of some corrins is presented.

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URL: http://dx.doi.org/10.1002/bms.1200090809

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Single ion monitoring assay for the serotonin re-uptake blocker Org 6582 in plasma (1982)

Vink, Jan ; van Hal, Henk J. M. ; van de Laar, Gerrit L. M.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 370-375

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: An assay method has been developed to determine the serotonin re-uptake blocker Org 6582 as its free base in plasma. As internal standard an isomer of Org 6582 is used. The assay procedure includes protein precipitation by addition of trichloroacetic acid, n-hexane extraction from basic medium and derivatization with trifluoroacetic acid anhydride. Quantification is performed using gas chromatography mass spectrometry by monitoring the molecular ions of the N-trifluroacetyl derivatives of Org 6582 and internal standard at m/z 315. The assay method was applied to plasma samples from toxicological and from Phase I clinical studies. The assay characteristics are discussed in relation to comparable assay methods routinely employed in the authors' laboratory to monitor drug levels.

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Studies on molecular species of choline and ethanolamine glycerophospholipids obtained from rat brain myelin and synaptosomes by gas-liquid chromatography mass spectrometry (1982)

Kino, Minoru ; Matsumura, Tadaki ; Gamo, Masami ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 363-369

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: By converting to t-butyldimethylsilyl derivatives, molecular species of ethanolamine glycerophospholipid including both 1,2-diacyl and 1-alk-1′-enyl-2-acyl (plasmalogen) types were able to be analysed by a gas chromatography mass spectrometry selected ion monitoring technique. The samples analysed were ethanolamine glycerophospholipid and also choline glycerophospholipid obtained from myelin and synaptosomes of rat brain, both of which are characteristic subcellular organella of the nervous system. Main molecular species of ethanolamine glycerophospholipid were as follows: in myelin as 1,2-diacyl type, 36:1 (mainly 18:0/18:1), and as 1-alk-1′-enyl-2-acyl type, 34:2 (mainly vinyl 16:0/18:1), 36:2 (mainly vinyl 18:0/18:1) and 36:3 (mainly vinyl 18:1/18:1), whereas in synaptosomes as 1,2-diacyl type 36:1 (mainly 18:0/18:1), 38:4 (mainly 18:0/20:4) and 40:6 (18:0/22:6), and as 1-alk-1′-enyl-2-acyl type 34:2 (mainly vinyl 16:0/18:1), 36:2 (mainly vinyl 18:0/18:1), and 36:3 (mainly vinyl 18:1/18:1). The molecular species of choline glycerophospholipid consisted almost entirely of 1,2-diacyl type and they were in myelin 34:1 (mainly 16:0/18:1), 36:1 (mainly 18:0/18:1) and 36:2 (mainly 18:1/18:1), whereas in synaptosomes 32:0 (mainly 16:0/16:0), 34:0 (16:0/18:0), 34:1 (mainly 16:0/18:1) and 36:1 (mainly 18:0/18:1). In myelin as 1-alkyl-2-acyl type, 34:1 (1-hexadectl-2-octadecenoyl) was present at about 7%.

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Mass spectrometry of 2-substituted-4-arylthiazoles: II-identification of microsomal nitroreduction product by mass spectrometry (1982)

Mattammal, Michael B. ; Zenser, Terry V. ; Davis, Bernard B.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 376-380

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Electron impact fragmentation of 2-methyl-4-(4-nitropenyl)-thiazole and 2-amino-4-(4-nitrophenyl)-thiazoles were studied. Prominent fragment ions result from: (1) elimination of an NO2 radical and of a neutral NO molecule; (2) 1,2 cleavage of the thiazole ring in both compounds to give a phenoxythiirene ion; and (3) subsequent cleavage of this phenoxythiirene ion to give the common ions [C7H5] and [C5H3]. An anaerobic microsomal nitroreduction product of 2-methyl-4-(4-nitrophenyl) thiazole was isolated and its structure was determined by electron impact, chemical ionization and high resolution mass spectrometry to be 2-methyl-4-(4-aminophenyl)-thiazole.

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Mass spectra of metabolites of 1-(tetrahydro-2-furanyl)-5-fluorouracil and related compounds (1982)

Marunaka, Teruyoshi

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 381-389

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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 metabolites of the antitumour agent 1-(tetrahydro-2-furanyl)-5-fluorouracil and their related compounds were measured by field desorption, chemical ionization and electron impact methods. The molecular ions of these compounds were observed in all methods. In the electron impact mass spectra of hydroxylated 1-(tetrahydro-2-furanyl)-5-fluorouracil and 5-fluorouracil-nucleosides, which differ in the position of the hydroxyl group on the tetrahydrofuran ring or sugar ring, the patterns of fragment ions formed by transition of labile hydrogens were extremely effective for determination of the structures of these compounds. Furthermore, the characteristic fragment ions produced by the retro Diels-Alder decomposition of the 5-fluorouracil skeleton provided useful information for determining the position of the substituent on the 5-fluorouracil skeleton.

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URL: http://dx.doi.org/10.1002/bms.1200090905

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Geographical variations in the carbon isotope composition of the diet and hair in contemporary man (1982)

Nakamura, K. ; Schoeller, D. A. ; Winkler, F. J. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 390-394

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Geographic variations in the carbon isotope composition of the human diet and human hair were investigated. The carbon isotopic composition of common foodstufls purchased in Chicago, USA, Tokyo, Japan and Munich, FRG, were determined by combustion and differential isotope ratio mass spectrometry. The dietary protein carbon for the United States (-18.1‰) was calculated to be enriched in 13C relative to the Japanese (-21.2‰) and the German (-23.6‰) diets. To a large degree, the differences reflected the consumption of corn-fed animal products in the United States and Japan, as well as seafood in Japan. The carbon isotopic composition of hair (-16.4, -18.0 and -20.4%) for the three respective populations correlated with the calculated values of the dietary protein, but were 2-3% enriched in 13C. Changes in the isotopic composition of beard hair were shown to record the changes in dietary composition in travelers visiting the respective regions.

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URL: http://dx.doi.org/10.1002/bms.1200090906

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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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.1200091001

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The accurate determination of serum glucose by isotope dilution mass spectrometry - two methods (1982)

White V, E. ; Welch, M. J. ; Sun, T. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 395-405

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Two isotope dilution mass spectrometric methods have been developed for the determination of D-glucose in human serum. Each uses a uniformly labeled (13C)glucose as the internal standard. The first method involves conversion of glucose into 1,2: 5,6-di-O-isopropylidene-α-D-glucofuranose and an extensive clean-up, followed by quantitation using packed column gas chromatography mass spectrometry. In the second method, glucose is converted into α-D-glucofuranose cyclic 1,2: 3,5-bis(butylboronate)-6-acetate. The wet chemistry work-up is simpler, but analysis by capillary gas chromatography mass spectrometry is required. Both methods exhibit excellent precision (coefficients of variation 〈0.3%) and provided mean values that agree within 1% for all serum pools tested.

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Halogen anion formation by polybrominated compounds in negative chemical ionization mass spectrometry (1982)

Greaves, John ; Bekesi, J. George ; Roboz, John

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 406-410

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Bromine anions from polybrominated biphenyls and bromobenzenes form in great abundance by dissociative electron capture. Nitrogen reagent gas moderates bromine expulsion more than does methane. The relationship between bromine anion to molecular anion ratio and the number of bromine atoms in the molecule is logarithmic. Asymmetric arrangement of bromine atoms favors decreased bromine anion formation. Increased source temperature favors dissociative electron capture, but also decreases sensitivity. The apparent composition of polybrominated biphenyl mixtures is strongly influenced by the range of masses scanned if bromine anions are excluded.

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URL: http://dx.doi.org/10.1002/bms.1200090908

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Mass spectra of the trimethylsilyl ethers of some 3β-hydroxy-Δ5-C21 steroids (1982)

Harvey, D. J. ; Middleditch, B. S. ; Brooks, C. J. W.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 411-418

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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 trimethylsilyl derivatives of 22 3β-hydroxy-Δ5-pregnenes have been examined with the aid of deuterlum labelling and high resolution mass measurements. The influence of additional hydroxy and keto substituents on the characteristic fragment ions is discussed and fragmentation mechanisms for several ions characteristic of hydroxylation at specific sites (11 and 16) are proposed.

Additional Material: 2 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200091002

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Identification of 4,6-dioxoheptanoic acid (succinylacetone), 3,5-dioxooctanedioic acid (succinylacetoacetate) and 4-oxo-6- hydroxyheptanoic acid in the urine from patients with hereditary tyrosinemia (1982)

Lindblad, Bengt ; Steen, Göran

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 419-424

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: In the urine from patients with hereditary tyrosinemia, three characteristic compounds have been found. They have been identified as 4,6-dioxoheptanoic acid (succinylacetone), 3,5-dioxooctanedioic acid (succinyl-acetoacetate) and 4-oxo-6-hydroxyheptanoic acid. The identities have been established by mass spectrometry of several derivatives, and by comparison with a synthetic sample of 4,6-dioxoheptanoic acid.

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URL: http://dx.doi.org/10.1002/bms.1200091003

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Simultaneous determination of antipyrine, 4- hydroxyantipyrine, 3-hydroxymethylantipyrine and norantipyrine in urine by gas chromatography chemical ionization mass spectrometry (1982)

Tang, B. K. ; Uchino, H. ; Inaba, T. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 425-428

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: A simple, accurate and precise procedure was developed to quantify, in a single run, antipyrine, 4-hydroxyantipyrine, 3-hydroxymethylantipyrine and norantipyrine in urine. The stable isotope-labelled internal standards for the assay were obtained from a subject who ingested deuterium labelled antipyrine and produced urine containing the labelled drug and metabolites.

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URL: http://dx.doi.org/10.1002/bms.1200091004

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Mass spectrometric identification of indole compounds produced by Rhizobium strains (1982)

Badenoch-Jones, J. ; Summons, R. E. ; Entsch, B. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 429-437

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The following indole compounds have been unequivocally identified and semi-quantitated in culture supernatants of Rhizobium strains by gas chromatography mass spectrometry: indole-3-aldehyde, trytophol, indole-3-carboxylic acid, indole-3-glycollc acid, indole-3-actic acid, indole-3-glyoxylic acid, N-acethyl-L-tryptophan and indole-3-pyruvic acid, as well as indole-3-acetic acid. The strains included a number of chosen Rhizobium mutants defective in various stages of nodule formation, and the biological implications of the findings are discussed. Two alternative approaches to sample purification were taken, one based primarily on solvent partitioning and the other on high-performance liquid chromatography. The advantages of each method are discussed. Gas chromatographic retention times and mass spectra are given for the TMS derivatives of 17 authentic indole standards.

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URL: http://dx.doi.org/10.1002/bms.1200091005

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Field desorption mass spectrometry of betaine hydrohalides (1982)

Sano, Mitsuji ; Ohya, Kazumi ; Kitaoka, Hiroaki ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 438-442

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Field desorption mass spectra of betaine hydrohalides are generally characterized by field desorption ions such as [Betaines+H]+ and cluster ions [nBetaines+H]+. In compounds where the conformation between [N]+ and COOH in the molecule is unable to form a betaine structure, the field desorption mass spectra consist only of compiex field desorption ions due to thennal decomposition products. Quaternary ammonium cations [C]+ and cluster ions [nC+(n - 1)A]+, which arise from ordinary quaternary ammonium compounds, are hardly produced. The effect of counter-ions on the field desorption mass spectra and the mechanism of field desorption ion formation are also discussed.

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URL: http://dx.doi.org/10.1002/bms.1200091006

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Masthead (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982)

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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.1200091101

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Presence of four Fusarium mycotoxins and synthetic material in ‘yellow rain’: Evidence for the use of chemical weapons in laos (1982)

Rosen, Robert T. ; Rosen, Joseph D.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 443-450

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Analysis of a ‘yellow rain’ sample by selected ion monitoring revealed the presence of three trichothecenes: T-2 toxin, diacetoxyscirpenol and 4-deoxynivalenol in concentrations of at least 48,42 and 58 ppm, respectively. The concentration of zearalenone, another Fusarium mycotoxin, was estimated to be at least 265 ppm. Evidence for a formulation which contained polyethylene glycol was also obtained.

Additional Material: 12 Ill.

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URL: http://dx.doi.org/10.1002/bms.1200091007

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Negative ion chemical ionization mass spectrometry of trichothecenes: Novel fragmentation under OH- conditions (1982)

Brumley, William C. ; Andrzejewski, Denis ; Trucksess, Eric W. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 451-458

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Hydroxide ion chemical ionization mass spectra of two classes of trichothecenes are described. The spectra provide molecular weight information as well as fragment ions indicative of structure. The discussion of fragmentation is aided by the use of high resolution mass measurements, mass analyzed ion kinetic energy spectra and chloride attachment spectra. Certain novel fragmentation processes under hydroxide ion conditions are noted. The chloride attachment spectra are also useful for verification of molecular weight.

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URL: http://dx.doi.org/10.1002/bms.1200091008

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High resolution mass spectra of mono-, di-and trihydroxy stereoisomers of bile acids (1982)

Iida, Takashi ; Chang, Frederic C. ; Matsumoto, Taro ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 473-476

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: High resolution mass spectra were measured for six monohydroxy, 12 dihydroxy and eight trihydroxy isomers of methyl 5β-cholanates, which differ from one another in the position and configuration of hydroxyl groups at C-3, C-7 and/or C-12. Characteristic fragment ions serving to distinguish between the isomers are discussed.

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URL: http://dx.doi.org/10.1002/bms.1200091104

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The use of capillary column gas chromatography and negative ion chemical ionization mass spectrometry to confirm the administration of synthetic corticosteroids to horsesThese results were presented, in part, as a poster presentation at the 12th BMSS Meeting, Cambridge, 1981. (1982)

Houghton, E. ; Teale, P. ; Dumasia, M. C. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 459-465

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The negative ion chemical ionization mass spectra of the MO-TMS derivatives of the corticosteroids prednisolone, betamethasone and dexamethasone have been obtained using capillary column gas chromatography mass spectrometry. The spectra showed abundant diagnostic ions at m/z〉300 allowing for clear discrimination between the three steroid derivatives. A capillary column gas chromatographic mass spectrometric method using negative ion chemical ionization mass spectrometry has been developed to confirm the presence of the parent steroids in horse urine following the administration of proprietary preparations of prednisolone and betamethasone.

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URL: http://dx.doi.org/10.1002/bms.1200091102

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The electron capture negative ion chemical ionization mass spectra of 2-(4′,6′-bistrifluoromethyl-2′-pyrimidinyl)-tetrahydroisoquinoline and 4-substituted analogues (1982)

Murray, S. ; Waddell, K. A.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 466-472

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Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Reaction of debrisoquine and 4-hydroxydebrisoquine with hexafluoroacetylacetone to form pyrimidinyltetrahydroisoquinolines is used as the basis for a gas chromatographic mass spectrometric assay for these two compounds. The electron impact, positive ion chemical ionization and electron capture negative ion chemical ionization mass spectra of these pyrimidinyltetrahydroisoquinolines are described and compared. The latter were found to give an intense response under electron capture negative ion chemical ionization conditions, thus allowing the development of a much more sensitive assay for debrisoquine and 4-hydroxydebrisoquine. Derivatives of the hydroxyl group in 2-(4′,6′-bistrifluoromethyl-2′-pyrimidinyl)-4-hydroxytetrahydroisoquinoline were synthesized with a view to further improving the electron capture negative ion chemical ionization response. The resulting mass spectra showed extensive fragmentation for perfluoroacyl esters and halogenated silyl ethers. Only dimethylsilyl and trimethylsilyl ethers gave similar spectral responses to the parent compound.

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Investigations on antipyrine metabolism: IIFor Part I see Ref. 27. - Analysis of conjugated metabolites of antipyrine in rat and human urine by off-line combination of liquid chromatography and field desorption mass spectrometry (1982)

Lehmann, W. D. ; Böttcher, J. ; Bässmann, H. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 477-482

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The complex pattern of conjugates in the metabolism of antipyrine in man and rat has been investigated using an off-line combination of liquid chromatography and field desorption mass spectrometry. Using this approach, field desorption mass spectrometry enables the direct identification of underivatized glucuronides and sulphates in antipyrine metabolism on the basis of the corresponding protonated or cationized molecules representing the base peaks in the field desorption mass spectra. All conjugated metabolites of antipyrine established so far - four glucuronides and three sulphates - were identified in extracts of urine after stepwise purification by column chromatography and subsequent mass spectrometric analysis.

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URL: http://dx.doi.org/10.1002/bms.1200091105

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Simultaneous determination of terbutaline and salbutamol in plasma by selected ion monitoring (1982)

Lindberg, Claes ; Jönsson, Sven

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 493-494

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Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: We describe a method for simultaneous determination of terbutaline and salbutamol in plasma, based on gas chromatography chemical ionization mass spectrometry. Deuterium labelled terbutaline was used as internal standard for both drugs. The method has been used for the analysis of plasma samples obtained from asthmatic patients. The coefficient of variation at 0.3 ng ml-1 was 4.6% for terbutaline and 5.3% for salbutamol with a sample volume of 4 ml. The recovery of both drugs was 〉80%.

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URL: http://dx.doi.org/10.1002/bms.1200091107

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Negative ion chemical ionization and collisional activation mass spectrometry of naturally occurring bornyl C4—C5 esters (1982)

Bambagiotti A., M. ; Giannellini, V. ; Coran, S. A. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 495-498

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The negative ion chemical ionization mass spectrometry of bornyl butyrate, isobutyrate, valerate and isovalerate has been studied in detail. Collisional activation experiments have shown their analytical usefulness in the determination of the structure of the carboxylate fragment anions.

Additional Material: 5 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200091108

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Negative chemical ionization mass spectrometry of organophosphorus pesticidesPreliminary results were given in a lecture at the 1. European Conference on Food Chemistry in Vienna, Austria, 17.-20.02.81 (1982)

Stan, H.-J. ; Kellner, G.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 483-492

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The negative ion mass spectra of 52 organophosphorus pesticides obtained by chemical ionization with methane under electron capture conditions are presented. The influence of different ionization parameters on the total ion current as well as the relative intensities of the various fragment ions was investigated. In general, the mass spectra show few fragment ions, but these are characteristic for the chemical class of the compound (phosphate, phosphorothionate, phosphorothiolate, phosphorodithioate). The occurrence of the molecular anion is strongly dependent on the structure of the molecule and its ability to stabilize by charge delocalization the radical formed in the primary electron capture reaction. This takes place particularly in the organophosphorus esters of the parathion group which have an aromatic moiety with an electron attracting substituent. The phosphorothionates of the parathion group form a stable thiophenolate fragment which competes in the stability with the molecular anion. The relative intensity of these two ions in the spectrum is dependent on the ion source temperature.Because of the few, but intense fragment ions formed, negative ion mass spectrometry with multiple ion detection is expected to be a valuable tool for residue analysis in food and environmental samples.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200091106

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Liquid chromatography/mass spectrometry using glass lined stainless steel microbore columns (1982)

Alcock, Nicholas J. ; Corbelli, Luigi ; Games, David E. ; [et al.]

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. 499-504

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ISSN: 0306-042X

Keywords: Chemistry ; Analytical Chemistry and Spectroscopy

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Combined liquid chromatography/mass spectrometry using a moving belt interface and commercially available glass lined stainless steel microbore reverse phase liquid chromatographic columns is described. The chromatographic performance is comparable with that obtained with conventional columns, and the lower mobile phase flow rates used enable improved liquid chromatographic/mass spectrometric sensitivities to be obtained since all the liquid chromatographic eluent can be handled by the interface and instrumental background due to solvent impurities is reduced. The utility of the approach is illustrated with studies of extracts from timbo powder, Imperatoria ostruthium and Calophyllum inophyllum. Using the carbamate pesticides IPC and CIPC the potential of microbore liquid chromatography/mass spectrometry for quantitative studies is demonstrated.

Additional Material: 6 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/bms.1200091109

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Stephen I. Goodman and Sanford P. Markey. Diagnosis of organic acidemias by gas chromatography-mass spectrometry. Alan R. Liss, Inc., New York, 1982 (1982)

Sweeley, Charles C.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. i

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ISSN: 0306-042X

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.1200091111

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I. Howe, D. H. Williams and R. D. Bowen. Mass spectrometry, principles and applications, 2nd edition. McGraw-Hill Inc., New York, 1981 (1982)

Bowen, D. V.

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. i

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ISSN: 0306-042X

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.1200091110

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Forthcoming meetings (1982)

Chichester : Wiley-Blackwell

Biological Mass Spectrometry 9 (1982), S. ii

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ISSN: 0306-042X

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.1200091112

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