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  • Analytical Chemistry and Spectroscopy  (5,640)
  • Biochemistry and Biotechnology  (2,788)
  • Engineering General  (2,473)
  • 1985-1989  (10,901)
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Keywords
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Years
Year
  • 101
    Electronic Resource
    Electronic Resource
    Announcement (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. i 
    Details
    ISSN: 0887-6134
    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.1200180702
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  • 102
    Electronic Resource
    Electronic Resource
    Analysis of chlorinated organic compounds in estuarine biota and sediments by chemical ionization tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 464-470 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complex sample matrices of estuarine biota tissue and bed sediment extracts were analyzed for selected chlorinated compounds. By using gas chromatography/positive chemical ionization/tandem mass spectrometry, the coeluting interferences present in gas chromatography/electron ionization mass spectrometry were eliminated in the biota tissue and bed sediment extracts. The selected chlorinated compounds included chlorobenzene; 1,2-, 1,3- and 1,4-dichlorobenzene; 1,2,3-, 1,2,4- and 1,3,5-trichlorobenzene; 1,2,3,4-, 1,2,3,5- and 1,2,4,5-tetrachlorobenzene; pentachlorobenzene; hexachlorobenzene; hexachloro-1,3-butadiene; octachlorostyrene; and octachloronaphthalene. Daughter ion spectra for these compounds are included. The detection limit for most of the compounds was 20 pg, and the instrument response was linear over five orders of magnitude, by using 13C-labelled hexachlorobenzene as the internal standard.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180704
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  • 103
    Electronic Resource
    Electronic Resource
    Stable isotope dilution analysis of n-hexanoylglycine, 3-phenylpropionylglycine and suberylglycine in human urine using chemical ionization gas chromatography/mass spectrometry selected ion monitoring (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 471-477 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We describe a gas chromatographic/mass spectrometric method for the accurate determination of n-hexanoylglycine, 3-phenylpropionylglycine and suberylglycine in urine for the diagnosis of hereditary medium-chain acyl-CoA dehydrogenase (MCAD) deficiency. These acylglycines had previously been detected in urine from patients with MCAD deficiency, but their diagnostic values were unknown because of a lack of appropriate analytical methods. n-Hexanoyl(1,2-13C)glycine, 3-phenylpropionyl(2-13C, 15N)glycine and suberyl(2-13C, 15N)glycine were synthesized and used as internal standards. Ammonia chemical ionization was utilized to generate intense [M + H]+ ions for selected-ion monitoring quantification. The whole procedure is fast and can be performed by a low-resolution gas chromatographic/mass spectrometric system, giving accurate results over a range of three orders of magnitude (0.0167-16.7 μg/ml). The results from the analyses of 54 urine samples from 21 MCAD-deficient patients and various control samples using this method established that n-hexanoyglycine and 3-phenylpropionylglycine were highly diagnostic for this disease, while suberylglycine was found less specific.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180705
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  • 104
    Electronic Resource
    Electronic Resource
    Physical properties of matrices used for fast atom bombardment (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 492-497 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Physical and chemical properties of common matrices are tabulated, with aims of facilitating rational matrix selection and providing input for fundamental studies of matrix-assisted ionization. The rationale for selecting tabulated properties is discussed.
    Additional Material: 10 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180708
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  • 105
    Electronic Resource
    Electronic Resource
    Deuterated Ritanserin analysis by gas chromatography/mass spectrometry: A sensitive technique to study human Ritanserin pharmacokinetics (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 498-502 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ritanserin, a new selective serotonin-S2 antagonist, was labelled in one 4-fluorophenyl moiety to obtain a (2H4)-labelled analogue having the following isotopic distribution: 2H0: 0.0%, 2H1: 0.1%, 2H2: 1.9%, 2H3: 5.8%, 2H4: 92.2%. (2H0/2H4) Ritanserin and the internal standard were isolated from the plasma by liquid/liquid extraction and analysed by selected-ion monitoring gas chromatography/mass spectrometry in the 70 eV electron impact mode. A detection limit of 0.1 ng ml-1 could be obtained for both (2H0) and (2H4)ritanserin. The precision (per cent coefficient of variation) and accuracy (per cent relative error) of the method were 4.1% and 4.1%, respectively. The method was used to determine the plasma levels of ritanserin and tetradeuterated ritanserin in three healthy male subjects receiving an equimolar mixture of 5:5 mg (2H0/2H4)ritanserin. The pharmacokinetics of both isotopomers proved to be identical, indicating the absence of an isotope effect, so that this technique might be very promising for use in bioequivalence studies.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180709
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  • 106
    Electronic Resource
    Electronic Resource
    Forthcoming events (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 511-511 
    Details
    ISSN: 0887-6134
    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.1200180712
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  • 107
    Electronic Resource
    Electronic Resource
    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200180801
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  • 108
    Electronic Resource
    Electronic Resource
    Analysis of 18O enrichment in biological fluids by continuous flow-isotope ratio mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 543-546 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel method is described for the analysis of 18O in urine by continuous flow-isotope ratio mass spectrometry (CF-IRMS), after sample equilibration with CO2. The method is shown to be fast, precise and accurate and therefore facilitates studies of total body water and water turnover in the clinical field. The method uses existing CF-IRMS instrumentation with minor hardware modification which does not compromise routine analysis of 13C and 15N. This method emphasizes the versatility of CF-IRMS and thus its economy for the biomedical research group using stable isotope tracers.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180805
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  • 109
    Electronic Resource
    Electronic Resource
    Differentiation of isomeric 2′-, 3′- and 5′-deoxynucleosides by electron ionization and chemical ionization-linked scanning mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 533-542 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A comparative mass spectral examination of the trimethylsilyl (TMS) derivatives of 2′-, 3′- and 5′-deoxyadenosine, 2′-, 3′- and 5′-deoxyguanosine, 2′-, 3′- and 5′-deoxyxanothosine and 2′- and 5′-deoxy-2-fluoroadenosine is presented. A general compilation of the major fragment ions found in the low-resolution electron ionization (EI) spectra of the eleven deoxynucleosides is given. Chemical ionization (CI)-collisional activation (CA) daughter ion spectra are reported using the deoxyadenosines as model compounds. Ion structures and fragmentation pathways are proposed for those ions characteristic of each of the isomers. Significant differences in fragmentation exist between the isomeric 2′-, 3′- and 5′-purine deoxynucleosides. The formation and structures of ten ions important in this differentiation are discussed. The CI-CA linked scan spectra provide complementary structural information relative to the EI mass spectra.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180804
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  • 110
    Electronic Resource
    Electronic Resource
    The antibiotic complex of retamycins: A fast atom bombardment mass spectrometric study (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 553-557 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometry is, for the first time, successfully applied to the underivatized anthracycline antibiotics retamycins E1 and E2, using bis-(2-hydroxyethyl)sulphide as the matrix compound. The spectra are characterized by abundant protonated molecular ions and also by a number of sequence ions, which can be easily rationalized in terms of the carbohydrate sequence in the molecules. The relative abundance of these ions seems to depend on the functionalities close to the glycosidic oxygen, and also on their stereochemical relationship. Structural results are also confirmed by the analysis of the FAB mass spectra of the acetyl derivatives.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180807
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  • 111
    Electronic Resource
    Electronic Resource
    Structural analysis of protein variants by mass spectrometry: Characterization of haemoglobin providence using a grand-scale mass spectrometer (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 563-565 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A grand-scale mass spectrometer with high mass resolution and high transmission was employed for the analysis of haemoglobin variant. Two variants were isolated from a haemolysate by chromatography. Secondary ion mass spectrometry of complex peptide mixtures derived from these variants precisely determined the molecular weight of abnormal peptides. The molecular weight, 2857.4 and 2858.4, indicated the amino acid substitutions of asparagine and aspartic acid, respectively, for lysine at position 82 of β globin chain. The mutations had been reported in haemoglobin Providence.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180809
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  • 112
    Electronic Resource
    Electronic Resource
    Mass spectral behaviour of some semisynthetic derivatives of vinblastine-type alkaloids (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 576-580 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectral fragmentation of the biomedically important vinblastine (1a) and its eight semisynthetic derivatives obtained by selective oxidation have been studied using in-beam electron impact ionization, low and high resolution, as well as linked scanning techniques. The mass spectra were obtained without any thermal decomposition and exhibited abundant molecular ions and several fragment ions of structural importance. It was found that decomposition of these indole-indoline dimers having a velbanamine, or a ψ-aspidosperma, or a ψ-eburnane type indole moiety connected with the aspidosperma skeleton of vindoline (sets 1-3, respectively) led to several fragments of common types due mainly to the presence of the vindoline skeleton. However, sets 1-3 possessing various indole parts give rise to significant and characteristic fragments of these subunits, too. Varying the N(1) substituent of the vindoline part (CH3 → H → CHO), a strong influence was observed in the relative importance of the main reaction routes. It can be rationalized in terms of the effect of substituent on the localization of the positive charge.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180812
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  • 113
    Electronic Resource
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    Qualitative and quantitative determination of Prevan® in cosmetic emulsions by direct analysis via fast atom bombardment/collisional spectroscopy (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 855-859 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The qualitative and quantitative determination of the Na salt of dehydroacetic acid, Prevan®, a widely employed antimould agent in cosmetic emulsions, has been obtained by the direct analysis of the emulsion itself by fast atom bombardment and collisional spectroscopy.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181003
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  • 114
    Electronic Resource
    Electronic Resource
    Fast atom bombardment mass spectrometry and selective acid hydrolysis for the analysis of partially modified retro-inverso peptide analogues (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 867-871 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometry has been successfully applied to the analysis of partially modified retro-inverso peptide isomers. The spectra are characterized by abundant protonated molecular ions and also by sequence ions due to fragmentation of the inverted bonds. Unambiguous information, as to the nature and the position in the backbone of the amino acids involved in the partial modification of the structure, are given by using a combination of FAB mass spectrometry and partial, selective acid hydrolysis, without separation of the resulting peptide mixtures.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181005
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  • 115
    Electronic Resource
    Electronic Resource
    Announcement (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. i 
    Details
    ISSN: 0887-6134
    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.1200180402
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  • 116
    Electronic Resource
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    Fast atom bombardment mass spectrometry of some aminoglucoses and glucosamine phosphates and sulphates (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 241-246 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment mass spectrometry in combination with collisional activation has been used to investigate a number os amino- and phosphate-substituted glucoses and of phosphate- and sulphate-substituted glucosamines. The collisional activation spectra of the [M - H]- ions readily reveal the presence of sulphate or phosphate substituents, whereas specific fragmentation reactions can be used to distinguish among the various positional isomers. The fragmentation of the pseudomolecular cations depends on the number of Na atoms incorporated. By selecting the appropriate pseudomolecular ion it is possible to get information on the nature and/or position of the substituents.
    Additional Material: 8 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180406
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  • 117
    Electronic Resource
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    Capillary zone electrophoresis/tandem mass spectrometry for the determination of sulfonated azo dyes (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 253-257 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Full-scan capillary zone electrophoresis/mass spectrometry and capillary zone electrophoresis/tandem mass spectrometry (CZE/MS/MS) are demonstrated for the determination of monosulfonated and polysulfonated azo dyes at the low picomole levels. Under selected ion monitoring conditions femtomole levels of the dyes are detectable. Ion evaporation via the ion spray liquid chromatography/mass spectrometry interface is a mild form of ionization exhibiting only deprotonated singly charged or poly-deprotonated multiply charged negative molecular ions for sulfonated azo dyes. CZE/MS/MS daughter ion scanning after collision-induced dissociation of the molecular species for all sulfonated azo dyes contained the sulfonate ion (m/z 80). The presence of three sulfonated azo dyes in a wastewater extract was confirmed by parent ion scanning for the sulfonate daughter ion (m/z 80).
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180408
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  • 118
    Electronic Resource
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    Analysis of platelet activating factor in human saliva by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 258-264 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Platelet activating factor (PAF) bioactivity has been demonstrated in saliva from normal volunteers. We sought structural confirmation and evidence of heterogeneity in the 1-O-alkyl chain of the acetyl glyceryl ether phosphoryl choline (AGEPC) extracted from saliva by employing stable isotope dilution techniques in conjunction with gas chromatography/mass spectrometry. The method described involves removal of the polar phosphocholine moiety, accounts for acetyl group migration, and allows for acylation of the resultant free hydroxyl with pentafluorobenzoyl chloride. Thin-layer chromatography (TLC) purification is undertaken after phospholipase C cleavage and again after pentafluorobenzoyl chloride derivatization. The majority of the ion current is represented in the molecular anion, allowing measurement of 50 pg in biological fluid with a signal-to-noise ratio of ≥9. In one subject with markedly increased salivary PAF levels, we found evidence for molecular heterogeneity of AGEPC with production of not only C16:0 but also C18:0 and C18:1 in the alkyl chain. This technique, by using TLC in lieu of high-performance liquid chromatography, avoids potentially confounding trace contamination effects, produces spectra with few interfering signals and increases sample throughput.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180409
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  • 119
    Electronic Resource
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200180501
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  • 120
    Electronic Resource
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    Mass spectral investigations on trichothecene mycotoxins. VIII - thermospray ionization and collisionally activated dissociation of macrocyclic trichothecenes (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 287-300 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several structurally similar, biologically active macrocyclic trichothecenes were ionized under thermospray conditions followed by collisionally activated dissociation of the ammonium adducts. Most of the observed daughter ions were formed by bond cleavage at the exocyclic ester bridges. Compounds with similar ester bridges formed several common daughter ions and underwent similar neutral losses. Fragmentation pathways proposed for the dissociation of the adducts were confirmed from the corresponding neutral loss spectra. Simple experiments designed for the sequential monitoring of the characteristic daughter ions were used for the rapid, direct and accurate analysis of macrocyclic trichothecenes in real samples. The primary drawback of the method is its inability to distinguish between isomers.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180503
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  • 121
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    The identification of a dihydrodiol metabolite of propranolol excreted in horse urine (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1030-1033 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181113
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  • 122
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    Routine gas chromatographic/mass spectrometric analysis of fatty acid methyl esters using the ion trap detector (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1016-1022 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: About 60 long-chain fatty acids occur naturally in lipids of biological tissues and fluids, oils, fats and waxes. The ion trap detector (ITD) offers a convenient but powerful means for the routine analysis by gas chromatography/mass spectrometry of such fatty acids as their methyl esters (FAMES). Enhanced [M + 1]+ ions may be formed at higher sample levels of 50 ng or more. However, spectra still retain a predominantly electron impact (EI) character. Using the classical mass spectral performance test compound methyl stearate as an example, good library comparisons were obtained for spectra run over a dynamic range of 2 pg to 225 ng, when a mid-range ITD spectrum run on 7.5 ng was used as a reference. Almost equally good spectral comparisons were found with literature reference spectra run on both quadrupole and sector conventional mass spectrometers. Using human plasma phospholipid FAMES as an example, along with an ITD-generated EI spectral library of FAMES standards, it was seen that for most of the components present the mass spectral library comparison was good enough to permit identification based on mass spectrometry alone. For all components, a combination of gas chromatographic retention index and mass spectral information permitted an unequivocal identification.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181111
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  • 123
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    Positional isotopic analysis of 13C-labelled glucose by mass spectrometry: Applications to the study of gluconeogenesis in liver cells (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1010-1015 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The aim of the present investigation was to ascertain whether mass spectrometric analysis of glucose allows determination in small samples (0.01 nmol) of the sites and the extent of labelling of glucose produced by isolated liver cells from various gluconeogenic labelled precursors. The electron impact spectrum of the methyloxime pentatrimethylsilyl derivative of natural glucose affords fragment ions retaining specific carbon atoms, i.e. 1-2 (m/z 160), 1-2-3 (m/z 262), 3-4-5-6 (m/z 319), 4-5-6 (m/z 217), 5-6 (m/z 205), 6 (m/z 103). The mass fragmentography analysis of the same derivative of commercially available labelled glucose molecules (1-13C, 6-13C, 2-2H, 3-2H, 6,6-2H2) permitted evaluation of the degree of specificity of these fragment ions, and development of a calculation method for isotope incorporation. Using this methodology we found that incubation of hepatocytes with (2-13C)glycerol, (1,3-13C)glycerol or NaH13CO3 plus pyruvate or lactate produced (2,5-13C)glucose, (1,3,4,6-13C) glucose or (3,4-13C)glucose, respectively. The extent of labelling was measurable on individual carbon of the glucose molecule except for carbon 1. The lowest enrichment detectable on carbon 1-3 or 3 was found to be 0.5%. In conclusion, gas chromatography mass spectrometry is a reliable method for positional isotopic anlysis of 13C-labelled glucose, and appears useful in the study of the gluconeogenic pathway.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181110
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  • 124
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200180701
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  • 125
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    Analysis of glycolipids by fast atom bombardment mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1046-1050 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The positive and negative ion fast atom bombardment (FAB) mass spectra of four glycolipids obtained from microbial cultures are reported. The spectra of the glycolipids in the positive ion mode are characterized by abundant [M + Na]+, [M + Na + matrix]+ and [M + 2Na - H]+ species. In negative FAB conditions the molecules yield [M - H]-. Our understanding of the FAB behaviour of glycolipids in both positive and negative modes has been considerably aided in the structure elucidation, without any derivatization or degradation reaction of the compounds studied. The technique allows unambiguous molecular weight determination of low-microgram amounts of these glycolipids purified from biological sources and provides useful fragmentation information.
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    Identification of mustard related compounds in aqueous samples by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 484-491 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary column gas chromatography/mass spectrometry, under electron impact and chemical ionization conditions, was used for the detection and identification of mustard and other sulfur vesicant-related decomposition products in a number of aqueous sample extracts. Interpretation of the mass spectral, infrared, chromatographic and trimethylsilyl derivatization data acquired during this study enabled the identification of nineteen sulfur vesicant-related hydrolysis products. Many of the compounds characterized during these analyses, including a number of ether/thioether macrocycles and vinyl alcohols, have either not been previously reported or have not been previously associated with the decomposition of munitions-grade mustard.
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    Collisional activation mass spectrometry of doubly charged ions from hexachlorobiphenyl isomers (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 507-509 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180711
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    Facile connection of aluminium clad capillary GC columns to a magnetic sector mass spectrometer (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 503-506 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Guest editorial (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. ii 
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    ISSN: 0887-6134
    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.1200180802
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    Time-of-flight mass spectrometry: An increasing role in the life sciencesPlenary Lecture presented at the Seventh International Symposium on Mass Spectrometry in the Life Sciences. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 513-532 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Although available commercially since the mid-1950s, there has been a renewed and increasing interest in time-of-flight mass spectrometers during the last decade or more. Improvements have been made in mass resolution; and high-speed data acquisition systems have been developed which enable the recording of all ions in each time-of-flight cycle. Most importantly, these instruments have been coupled with several new ionization techniques, which are capable of desorbing the relatively large and intractable biopolymers whose structures are of interest to molecular biologists, biochemists and biophysicists. Primarily these are techniques which employ pulsed lasers, fission fragments and pulsed ion beams, for which a ‘non-scanning’ and/or high-transmission analyzer provides considerable analytical advantage. In this report we review some basic principles of the time-of-flight mass analyzer, highlighting efforts to improve dynamic focusing for instruments forming ions in the gas phase and static focusing for desorption instruments, and the progression from time-slice to time-array detection. We also review some of the accomplishments of instruments employing the time-of-flight analyzer, including: molecular weight determinations for peptides and small proteins; the analysis of tryptic digests, crude extracts and whole cells; the structural analysis of glycolipids, phospholipids and lipopolysaccharides; and the determination of covalent and metal-linked peptide dimers. We conclude with some recent developments in combining the time-of-flight analyzer with liquid chromatography using the continuous flow probe technique.
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    Plasma desorption mass spectrometric study of UV-induced lesions within DNA model compoundsThis is paper VI of a series ‘Plasma Desorption Mass Spectrometry of Oligonucleotides’. Paper V corresponds to Ref. 8. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 547-552 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive and negative plasma desorption (PD) mass spectra of the di-deoxyribonucleoside monophosphate d(TpT) and of its biologically relevant ultraviolet-induced intramolecular photodimers are examined and discussed. The photodimers which were analysed by PD mass spectrometry include the cis-syn and trans-syn cyclobutyl isomers d(T[p]T), the pyrimidine-pyrimidone photoadduct (6-4)d(TpT) and its Dewar valence isomer. Molecular ions, quasi-molecular ions and several fragment ions are observed in all cases. It is shown that, despite the absence of mass differences between these dinucleoside monophosphates, the fragmentation pattern differs significantly between the two main classes: cyclobutane dimers and (6-4) adducts. PD mass spectrometry can therefore be envisaged for characterizing their formation within short DNA fragments.
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    Characterization of acylcarnitines as their isobutyl ester derivatives using fast atom bombardment mass spectrometry and constant neutral loss scan (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 668-672 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple method is described for the characterization of acylcarnitines by fast atom bombardment mass spectrometry in combination with constant neutral loss (CNL) scan. Acylcarnitines in urine are extracted using cation-exchange chromatography and derivatized to their isobutyl esters. The fragmentation patterns of these compounds are studied by various linked-scan methods including B/E, B2/E and B/E√(1 - E) scans. Acylcarnitine isobutyl esters are found to lose two specific neutral fragments simultaneously so that a CNL scan of the combined mass produces a much enhanced spectrum without most of the background peaks. An example is given in which the CNL scan is used to diagnose a patient with medium-chain acyl CoA dehydrogenase deficiency. The use of linked-scan techniques to monitor a specific metastable ion transition can be exploited for characterizing structurally related compounds and therefore the technique reported in this paper may have much wider applications to mixture analysis.
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    Solvent-sample interactions in thermospray mass spectrometry of antineoplastic nitrogen mustards (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 219-223 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conditions are reported for the optimization of thermospray mass spectrometric analysis of antineoplastic nitrogen mustard alkylating agents. In aqueous ammonium acetate mobile phase, multiple sequential solvolytic reactions occur with these highly labile compounds, and protonated molecular ions of the reaction products are observed. However, when high proportions of acetonitrile or other organic modifier are added to the mobile phase, solvolytic reactions are much reduced and abundant protonated molecular ions are detected. One exception to these observations is phosphoramide mustard, which solvolyses under all conditions attempted. A lower limit for detection of melphalan using direct injection and summing the ion current between m/z 120 and 870 is about 150 ng. Successful thermospray liquid chromatographyl/mass spectrometry of these compounds should be possible using high percentages of methanol in the mobile phase or increasing the organic contant by post-column solvent modification.
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    The determination of sulfonated azo dyes in municipal wastewater by ion spray liquid chromatography tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 233-240 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A liquid-solid extraction method suitable for rapid screening of sulfonated azo dyes in municipal wastewater has been developed. The dyes (Color Index Acid Yellow 23, Red 14 and Yellow 49) were separated on a short, reversedphase liquid chromatographic column with a water-methanol gradient containing 2 mM sulfuric acid. The column effluent was directed via a split-valve to an ion spray liquid chromatography/mass spectrometry (LC/MS) interface to an atmospheric pressure ionization mass spectrometer. The ion spray LC/MS system produced abundant [M - Na]- and [M - 2Na]2- ions according to the number of sulfonic acid substituents. Collision-induced dissociation of the parent ions for the dyes studied gave the SO3-. fragment common to sulfonated compounds plus additional daughter ion fragments characteristic of each dye. The dyes were quantified by monitoring from four to six different daughter ions of each dye. The relative abundances and the sum of the daughter ion current counts were used for confirmation and quantification with external standards. Recoveries of the dyes were in the range of 70-122%, and the relative standard deviation of replicate determinations was 5.4-12%. The method detection limit was three times higher for Acid Yellow 23 compared with the other two dyes, which could be detected down to 50 ppb in municipal wastewater.
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    Forthcoming events (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 279-279 
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    ISSN: 0887-6134
    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.1200180411
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    Identification of in vitro metabolites of 3-ethyl-2,6-dimethyl-4H-pyrido(1,2a)pyrimidin-4-one (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 308-313 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (2-14C)3-Ethyl-2,6-dimethyl-4H-pyrido(1,2a)pyrimidin-4-one is metabolized in vitro by liver microsomes to at least 12 metabolites. The metabolites were isolated and purified by thin-layer chromatography and high-performance liquid chromatography and identified by mass spectrometry and nuclear magnetic resonance spectrosopy. The mostly mono- and dihydroxylated isomers were distinguished on the bases of their electron ionization mass spectra and the metastable daughter ion spectra of selected ions.
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    Characterization of epoxides of polyunsaturated fatty acids by mass spectrometry via 3-pyridinylmethyl esters (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 328-336 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The isomeric epoxides of linoleic, arachidonic and docosahexaenoic acids were prepared by reaction with m-chloroperoxybenzoic acid and, after separation by normal-phase high-performance liquid chromatography, were esterified with 3-pyridylcarbinol via the unstable imidazolide generated by the reaction with 1,1′-carbonyldiimidazole. The electron impact mass spectra of these derivatives showed a molecular ion and a sequence of peaks with two characteristic abundant ions that resulted from formal cleavage of the carbon-carbon bonds at the oxirane ring. Both these ions retained the ester group. This fragmentation pattern allowed the unequivocal identification of the separate epoxide isomers.
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    Thermospray mass spectroscopy/high performance liquid chromatographic identification of the metabolites formed from arteether using a rat liver microsome preparation (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 337-351 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermospray LC/MS methods with internal standardization were developed for the quantification of the antimalarial arteether and six of its metabolites at the 1-10 μg/ml level in liver microsome preparations without the use of solvent extraction. The thermospray mass spectra of arteether and most of its metabolites exhibited strong [M + NH4]+ and [M - OR]+ peaks arising from the molecular ion adduct and the loss of the alkoxy or hydroxy group of the side chain. In addition to the six metabolites for which authentic reference standards were available, three additional metabolites were detected. The major metabolites of arteether were found to be dihydroartemisinin, deoxydihydroartemisinin, 3-hydroxydeoxydihydroartemisinin, two isomers of hydroxyarteether, and 3-hydroxydeoxyarteether. Deoxyartheether was not found at significant concentrations in the microsome preparation.
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    Desorption chemical lonization mass spectrometry of cosmomycins A, B, C, D and ditrisarubicin B (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 352-354 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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    Peptide sequencing by partial methanolysis and fast atom bombardment mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 168-173 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possibility of obtaining sequence information on peptides by partial methanolysis with 5 N HCl in dry methanol and subsequent fast atom bombardment (FAB) of the resulting mixture was investigated. This procedure was tested using four peptides of different size and amino acid composition. The results obtained demonstrate that this approach is effective in producing FAB spectra containing more sequence information than the spectra of the untreated peptides. For the compounds investigated the spectra contain enough information to unequivocally reassemble the original sequence.
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    Mass spectrometric analysis of cardiac glycosides by the desorption/ionization technique potassium ion ionization of desorbed species (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 177-184 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of cardiac glycosides by the desorption/ionization (D/I) mass spectrometric technique potassium ion ionization of desorbed species (K+ IDS) is presented. K+ IDS mass spectra of digitonin, digoxin, digoxigenin, digitoxin and ouabain are discussed to demonstrate the capabilities of this D/I method. The K+ IDS analysis consists of two steps: thermal desorption of neutral molecules representative of the analyte, followed by gas-phase addition of K+ ions to these species. Structural and molecular weight information of the cardiac glycosides is obtained with the K+ IDS technique. The most intense peak in the K+ IDS mass spectrum of an analyte, M, is frequently the [M]K+ ion. Interpretation of the K+ IDS mass spectra is simple, since one thermal degradation mechanism dominates. This mechanism is a 1,2-elimination process. A variation of the original K+ IDS technique, performed by changing the ionizing metal from K+ to Na+ (i.e. Na+ IDS), is presented for the analysis of digoxin. The Na+ IDS mass spectrum of digoxin contains more structural information than the K+ IDS mass spectrum of that compound. This may lead to a means of controlling the types of information obtainable with this D/I technique by varying the cation that is thermionically generated. K+ IDS analyses can be performed rapidly, no sample derivatization is necessary, no matrix is required and little instrument modification is necessary.
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    Quantitative metabolic profiling of valproic acid in humans using automated gas chromatographic/mass spectrometric techniques (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 192-199 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated gas chromatographic/mass spectrometric assay is described for the antiepileptic drug valproic acid (VPA) and 14 of its metabolites in plasma or urine. Quantitative analysis of the parent drug and its biotransformation products was carried out with the aid of trimethylsilyl derivatives, and was performed by selected ion monitoring gas chromatography/mass spectrometry (normally of [M - CH3]+ species) using an HP 5790 mass selective detector (MSD) quadrupole mass spectrometer. The analysis was fully automated, in that simple injection, data acquisition, integration, quantification and report functions were carried out during unattended operation by an HP 59970C ChemStation™ computer system. The method exhibits good accuracy and high precision, with correlation coefficients greater than 0.990 for all standard curves. Replicate analyses of pooled plasma samples over a 4 month period exhibited an inter-day variation of less than 15% for the parent drug and ten of its metabolites. Moreover, the high dynamic range of the MSD instrument permitted quantification of VPA and minor metabolites thereof (e.g. the hepatotoxic terminal olefin, Δ4-VPA) at levels as disparate as 260 μg ml-1 (VPA) and 14 ng ml-1 (Δ4-VPA) in a single analysis. The high stability and sensitivity of the assay, combined with the fully automated features of the instrumentation, make the method ideally suited to expanded clinical studies and for the routine monitoring of potentially high-risk patients on VPA therapy.
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    Electrochemically assisted fast atom bombardment negative ion mass spectrometry of quinonesThis paper is dedicated to Professor Kenneth L. Rinehart Jr, in honor of his 60th birthday. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 878-883 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several 1,4-quinones, including vitamin K1, have been examined by electrochemically assisted fast atom bombardment (EFAB) negative ion mass spectrometry. The resulting mass spectra of these substances show a significant increase in signal/chemical noise when compared to normal fast atom bombardment (FAB) mass spectra. Additionally, the use of EFAB results in some control over the reduction processes normally associated with FAB mass spectrometry.
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    Semi-quantitative method for high molecular weight neuropeptides by high-performance liquid chromatography/thermospray mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 897-903 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-performance liquid chromatography/thermospray mass spectrometry (HPLC/MS) was evaluated and optimized for the determination of β- and γ-endorphin. Thermospray spectra for the endorphins could be acquired under ion evaporation conditions, when a low vaporizor temperature (94°C) and high source temperature are used. The spectra showed [M + H]+, [M + Hx-1 + Nax]+ (x = 1-3) together with double charged ions. Positive ion detection exhibited higher ion currents than negative ion detection. Thermospray HPLC/MS was used to generate a linear calibration curve from 10 to 300 pmol. Thermospray displayed good run-to-run reproducibility (2-7%) and accurately measured spiked quantities of β- and γ-endorphin within 15% of the spiked values.
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    Negative ion chemical ionization gas chromatography/mass spectrometry of valproic acid metabolites (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 918-926 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A negative ion chemical ionization (NICI) gas chromatographic/mass spectrometric method is described for the identification of 15 valproic acid (VPA) metabolites as their pentafluorobenzyl derivatives. Samples analyzed were serum, urine and saliva taken from a volunteer on VPA at steady state and also given selected doses of (2H6)VPA. Metabolite peaks were identified by comparison to synthetic standards. All the metabolites, like the parent drug, produced abundant [M - 181]- ions, except 3-keto VPA, which gave an [M - 181 - CO2]- ion. Using the NICI method, two new VPA metabolites were identified. One of these metabolites was characterized as 4′-keto-2-ene VPA by synthesis, while the second one appeared to be a positional isomer of 4′-keto-2-ene VPA. The sensitivity of the method was also sufficient to detect metabolites of VPA in saliva. The ratio of the levels of (Z)-2-ene VPA to (E)-2-ene VPA was much greater in saliva than in serum, suggesting stereoselective plasma protein binding or transport of these two metabolites. The lower limit of detection for the quantification of VPA in serum or saliva was 2 ng ml-1.
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    The use of GC-MS-MS for the characterization of naturally occurring methyl alkanes (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 939-941 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181016
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    Fragmentation of deuteromethanol from 3,3′,4,4′-[2H4]-prostanoid pentafluorobenzylester/methoxime/trimethylsilylether derivatives by collisionally activated decomposition (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 937-938 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In negative ion chemical ionization mass spectra of prostanoid pentafluorobenzylester(PFB)/methoxime(MO)/ trimethylsilylether(TMS) derivatives [M-PFB]- is the most abundant fragment ion. Collisionally activated decomposition (CAD) spectra of this ions show nearly only fragmentation of trimethylsilanol (TMSOH), (CH3)2Si=CH2, carbon dioxide and methanol. CAD spectra of [M-PFB]- ions of 3,3′,4,4′-deuterated PGE2 and 6-oxo-PGF1α PFB/MO/TMS derivatives fragmentation of methanol and deuteromethanol (CH3OD) is observed. The ratio of CH3OH/CH3OD is about 3:1 (PGE2) and 9:1 (6-oxo-PGF1α) respectively. This loss of deuterium in the internal standard needs to be considered when employing the isotope dilution technique in quantitative prostanoid analysis and tandem mass spectrometry.
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
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    ISSN: 0887-6134
    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.1200181101
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    Quantitative determination of naltiazem in human plasma by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 978-982 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic/mass spectrometric procedure has been developed for the quantification of a diltiazem analog, naltiazem, in human plasma. The assay utilizes an extraction at neutral pH with hexane:ethylene dichloride:methyl-t-butyl ether (70:20:10), selective ion monitoring, methane or ammonia positive chemical ionization mass spectrometry and stable isotope dilution. The method has been used to analyze plasma concentrations of naltiazem in clinical samples over a range of 2-200 ng ml-1, using 1 ml of plasma.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181105
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    Preparation and mass spectral characterization of pentafluorobenzyl derivatives of alkyl and hydroxyalkyl-nucleobase DNA adducts (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 958-972 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentafluorobenzyl (PFBz) derivatives of the following nucleobases were prepared: cytosine, 5-methylcytosine, O2-methylcytosine, O2-ethylthymine, O4-ethylthymine, 5-hydroxymethyluracil, N6-methyladenine, O6-methylguanine, O6-hydroxyethylguanine and O6-hydroxyethylpurine. 13C nuclear magnetic resonance was diagnostic for O- versus N-attachment of the PFBz moiety: the resonance of the methylene carbon appeared in the range 29.15-42.13 ppm for NCH2C6F5, and 58.45-69.01 for OCH2C6F5. Considerable structural information was provided by mass spectrometry with ionization by electron impact. All of the derivatives were detected with high sensitivity and specificity by gas chromatography with detection by electron capture negative ion mass spectrometry, reflecting not only their chemical and physical stability, but also their strong tendency to form a structurally diagnostic anion, [M - PFBz]-, in high yield under these ionization conditions. PFBz derivatives are therefore attractive forms of alkyl-substituted nucleobases for analysis by mass spectrometry.
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    URL: http://dx.doi.org/10.1002/bms.1200181103
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    Electron impact mass spectrometry of substituted 1,3,8-triazaspiro[4,5]decan-4-ones (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1000-1004 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The neuroleptic butyrophenone drug spiroperidol (8-[4-fluorophenyl)-(4-oxobutyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one) and related compounds are valuable tools for mapping the dopamine receptors in the brain. During the development of the radiochemical synthesis of these compounds with very short-lived isotopes suitable for positron emission tomography studies, positive electron impact mass spectrometric information was obtained. Ion series are present in the spectra of all 12 compounds studied, which unambiguously allow recognition of type and site of substitution on the spiro system.
    Additional Material: 2 Tab.
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    Analysis by fast atom bombardment mass spectrometry of 4,4-dicarboxy-5-(pyridoxyl-5′-phosphate)-proline, of 4-carboxy-5-(pyridoxyl-5′-phosphate)-proline and 4,4-dicarboxy-5-pyridoxylproline (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 995-999 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: γ-Carboxyglutamic acid (Gla) reacts easily and quantitatively with piridoxal-5′-phosphate in H2O at room temperature, to give the 4,4-dicarboxy-5-(pyridoxyl-5′-phosphate)-proline (1). This product has been characterized by fast atom bombardment (FAB) mass spectrometry, including the B/E linked scan technique, ultraviolet and 1H nuclear magnetic resonance (NMR) analysis. In order to support further on the structure of 1, the 4-monodecarboxyderivative (2), obtained by heating compound 1 at 100°C for 30 min and the 5′-dephosphoderivative (3), obtained by enzymatic hydrolysis of 1 with alkaline phosphatase, were also analysed by FAB and 1H NMR techniques. FAB was shown to be the only adequate ionization technique to deal with such thermolabile and non-volatile compounds and could provide an elegant and fast method to detect Gla in biological matrices.
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    Quantitative determination of arecoline in plasma by gas chromatography chemical ionization mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1005-1009 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary gas chromatography/mass spectrometry (GC/MS) method for the quantitative analysis of arecoline in plasma has been developed for concentrations in the range 1-50 ng ml-1. Hexadeuterated arecoline was utilized as the internal standard. The removal of drug from plasma was accomplished by a two-step liquid/liquid extraction procedure involving a wash step followed by extraction with 5% triethyl amine in ethyl acetate. The GC/MS determinations were carried out with temperature-programmed capillary GC and ammonia chemical ionization mass spectrometry. The [M + H]+ ions of both analyte and internal standard were monitored at m/z 156 and 162, respectively. The method is linear and has sufficient sensitivity, precision, accuracy and selectivity for analysis of drug levels in human plasma.
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    Identification of point of specific enzymic cleavage of P1,P4-bis(5′-adenosy) tetraphosphate by negative ion FAB mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 450-452 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180615
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    Determination of the new aromatic retinoic acid Ro 13-7410 in plasma by two-dimensional gas chromatography negative ion chemical ionization mass spectrometry with selected-ion monitoringDedicated to Professor Dr. Gerhard Spiteller on the occasion of his 60th birthday. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 453-463 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific method for the determination of the aromatic retinoic acid Ro 13-7410 in plasma at the picogram per millilitre level is described. The method involves extraction of plasma using Extrelut-1 columns, purification of the extract with Bond Elut-NH2 cartridges, derivatization with pentafluorobenzyl bromide, and subsequent analysis by two-dimensional capillary gas chromatography using the zone-cutting technique, stable isotope dilution and selective negative ion monitoring chemical ionization mass spectrometry. A tetradeuterated analogue is used as internal standard. Quantification is possible down to 25 pg/ml using 1 ml of plasma. The coefficients of variation of the method as calculated from quality control samples are 8.5 and 4.2% at the 100 and 400 pg/ml levels. The method has been applied to the analysis of plasma of volunteers following an oral dose of 40 μg Ro 13-7410 and plasma of dogs following an intravenous and oral dose of 25 and 50 μg, respectively.
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    URL: http://dx.doi.org/10.1002/bms.1200180703
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    Identification and determination of tert-alkylphenols in carp from the trenton channel of the Detroit River, Michigan, USA (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 478-483 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Whole carp from the Detroit River were analyzed by gas chromatographic mass spectrometry. Seven tertiary alkyl phenols (tert-pentylphenols, tert-butyl-tert-pentylphenols, a di-tert-pentylphenol and a tri-tert-pentylphenol) and eight chlorinated derivatives of these compounds were identified from their mass spectra and confirmed with synthesized authentic standards. 2,4-Di-tert-pentylphenol was the most abundant of these compounds; in one fish sample, its concentration was about 140 ppm. The same alkyl phenols were also found in technical-grade 2,4-di-tert-pentylphenol, which is manufactured at a chemical plant located near the Detroit River. Comparison of the alkyl phenol levels in carp with those in nearby sediments showed that many of these compounds are taken up by carp and that carp can be used to roughly track local sediment contamination.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180706
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    Molecular species analysis of phospholipids by negative ion fast atom bombardment mass spectrometry: Application of surface precipitation technique (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1051-1056 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Eight phospholipidic classes from bovine brain cortex and soybean were prepared and purified by preparative high-performance and liquid chromatography, and their molecular species were identified by negative ion fast atom bombardment mass spectrometry using the ‘surface precipitation’ method. Its main advantages are: (i) clear-cut and abundant diagnostic ions for structural elucidation of the species; (ii) fragments characteristic of the main fatty acids, the polar head-group and the molecule frame in phospholipids; (iii) less background caused by the liquid matrix.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181204
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    Metabolism of a thromboxane A2 antagonist in isolated rat hepatocytes (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1057-1062 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metabolism of a thromboxane A2 antagonist (±)-5-(Z)-7-(3-endo-phenylsulphonylaminobicyclo[2.2.1]hept-2-exoyl)-heptenoic acid (S-145) in isolated rat hepatocytes was examined by high-performance liquid chromatography and gas chromatography/mass spectrometry. As the hydrophobic metabolites, bis-nor S-145, tetra-nor S-145 and bis-nordihydro S-145 were identified, and two other products were estimated to be monohydroxylated S-145 and dehydrogenated S-145. On the basis of kinetics of S-145 metabolism, a metabolic pathway of S-145 in isolated hepatocytes is tentatively proposed.
    Additional Material: 7 Ill.
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    Direct detection of organic compounds in water at parts-per-billion levels using a simple membrane probe and a quadrupole ion trap (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 1063-1070 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organic compounds present in aqueous solutions can be analyzed directly using a quadrupole ion trap detector (ITD) when the solution is introduced via a hollow fiber membrane probe. The flow-through configuration used for sample introduction allows the aqueous solution to flow through the capillary membrane tubing while the organic compounds which selectively permeate the membrane are ionized in the ion source. In this mode of operation, the instrument shows high sensitivity. Chemical ionization mass spectra for a set of ten organic compounds of environmental interest were recorded and the ITD/membrane system was found to consistently allow detection of part-per-billion (ppb) levels of these compounds directly from water without any preconcentration. Analysis of well water samples containing ppb to part-per-million levels of organics was demonstrated using the ITD/membrane system. The combination of the membrane probe and ion trap produces a compact, inexpensive, rapid and sensitive system for environmental analysis. The flow-through membrane configuration was also used with a direct insertion probe in a triple quadrupole. Detection limits in the ppb range for organic compounds in water were measured. Detection of particular compounds in complex matrices was demonstrated by detection of 10 ppb 2-methoxypyridine in a fermentation medium using a triple-quadrupole mass spectrometer.
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    URL: http://dx.doi.org/10.1002/bms.1200181206
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    Ultrastructural localization of aluminium in liver of aluminium maltol-treated rabbits by laser microprobe mass analysis (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 598-602 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By means of laser microprobe mass analysis (LAMMA), we have studied the ultrastructural localization of aluminium in livers of aluminium maltol-treated rabbits. This animal model was developed to study long-term aluminium toxicity using systemic (intravenous) administration of aluminium. We could only detect aluminium in electron-dense inclusion bodies found in large, sometimes multinucleated cells. These results prove that the actual observation of aluminium deposits in liver with LAMMA gives more information than bulk analysis and can be very useful to explore mechanisms of toxicity.
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    URL: http://dx.doi.org/10.1002/bms.1200180815
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    Porous-layer open-tubular gas chromatography in combination with an ion trap detector to assess volatile metabolites in human breath (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 613-616 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the quantification of major volatile substances in human breath without preconcentration. Methanol, ethanol, acetaldehyde and acetone are well separated by porous-layer open-tubular column gas chromatography. Low-level detection was possible by means of an ion trap detector. Halothane has been used as internal standard.
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    URL: http://dx.doi.org/10.1002/bms.1200180817
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    Cholesterol and bile acid synthesis: Utilization of D2O for metabolic studies (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 624-628 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Human fibroblasts and hepatoma (Hep G2) cells were grown in media containing 25% D2O. Cholesterol extracted from the cells and bile acids obtained from the media were analyzed by gas chromatography/mass spectrometry (GC/MS). Fibroblasts that were transferred serially in media containing D2O continued to grow and to synthesize cholesterol enriched in deuterium. The observed distribution of deuterium-enriched species of cholesterol corresponded to a distribution that was calculated based on C = 27, 13C = 1.107%, D2O/H2O = 0.25, hydrogen derived from water = 20, and is in agreement with the concept that deuterium incorporation occurs randomly and represents mostly the NADPD/NADPH ratio in the medium. The deuterium enrichment of cholesterol from hepatoma cells indicated a shift of the most abundant species from m/z 373 to m/z 375, which corresponds more closely to the derivation of 25 hydrogens from water and implies the formation of deuterated acetate in the medium. Analysis of chenodeoxycholic acid, the predominant bile acid synthesized by Hep G2 cells in vitro, indicates its derivation from both pre-formed and newly synthesized cholesterol and that A ring transformation from cholesterol utilizes deuterium derived from water. Analysis of the bile acids derived from hamster bile following the administration of D2O confirms that similar events occur in vivo.
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200180901
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    Confirmation of organophosphorus pesticide residues in food applying gas chromatography/mass spectrometry with chemical ionization and pulsed positive negative detectionPart of this paper was presented at the 6th International Congress on Pesticide Chemistry, 15 August 1986, Ottawa, Canada. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 645-651 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A confirmatory technique for residue analysis of organophosphorus pesticides in food samples applying gas chromatography/mass spectrometry is described. The use of capillary columns is essential to achieve the separation of the great number of pesticides in use. Chemical ionization with the simultaneous recording of positive and negative ions results in the highest detection sensitivity for all 72 compounds. A selection of three ions was made for each pesticide and the parameters were optimized to gain highest detection sensitivity. The method was proved with food samples from the daily routine control.
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    URL: http://dx.doi.org/10.1002/bms.1200180902
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    Application of megabore capillary gas chromatography/mass spectrometry in the analysis of samples generated by the volatile organic sampling train (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 138-144 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method of analyzing volatile organic sampling train (VOST) samples by megabore capillary gas chromatography/mass spectrometry has been developed to enhance compound resolution and to improve the characterization of products of incomplete combustion in stack emissions. Several analytical systems were evaluated. The combination of components which gave the best overall performance consisted of a clamshell oven used to desorb the Tenax® and/or Tenax®/charcoal VOST cartridges onto an analytical trap in a commercial purge and trap unit. The purge and trap unit thermally desorbed the contents of the analytical trap onto a megabore capillary column installed in a gas chromatograph where the VOST target compounds were characterized and quantified by a computerized mass spectrometer. All VOST target compounds showed response factors with coefficients of variation of less than 25% for triplicate analyses at four concentrations. The time of analysis using the capillary column was 30% faster than the present VOST protocol that requires packed-column gas chromatography.
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    Metabolic studies of explosives 6. Electron impact and chemical ionization mass spectrometry of metabolites of 2,4-dinitrotoluene (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 149-156 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of metabolites of 2,4-dinitrotoluene have been synthesized and analysed by electron impact and chemical ionization mass spectrometry. Identification characteristics of these metabolites by their mass spectra have been determined. Differentiation of isomers is made possible by electron impact ions which are characteristic to the position of the methyl group with regard to the nitro group and to the position of the carboxylic acid group with regard to the nitro group. Metabolites containing an acetyl amino group are characterized by an [M - COCH2]+. electron impact ion.
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    URL: http://dx.doi.org/10.1002/bms.1200180302
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    Characterization of seven antihistamines, their N-oxides and related metabolites by fast atom bombardment mass spectrometry and fast atom bombardment tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 157-167 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We have examined the synthetic N-oxides of five ethylenediamine-type antihistamines using fast atom bombardment (FAB) mass spectrometry and FAB tandem mass spectrometry (MS/MS). Fragmentation of the protonated molecule in the normal and collisionally activated spectra appeared to be characteristic for this class of antihistamine N-oxide. Spectra were also acquired from an ethanolamine and a propylamine antihistamine N-oxide for comparison. These results were very similar to those obtained from biologically produced antihistamine N-oxides, as well as isomeric metabolites, which were readily distinguished from the N-oxides by characteristic fragmentation. In addition, a prominent ion 16 daltons lower in mass, which has been attributed to loss of elemental oxygen from the protonated N-oxide in chemical ionization mass spectral studies, was shown to be a matrix-dependent product of the solution-phase reduction of the antihistamine N-oxide to the parent antihistamine during FAB ionization. These results demonstrate that with a non-reducing matrix such as glycerol, FAB mass spectrometry and FAB MS/MS are excellent methods for the characterization of the non-conjugated antihistamine metabolites such as the N-oxides.
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    URL: http://dx.doi.org/10.1002/bms.1200180303
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    High-performance liquid chromatographic/mass spectrometric and high-performance liquid chromatographic/tandem mass spectrometric analysis of carbamate pesticides (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 200-206 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermospray ionization mass spectra of selected carbamate pesticides were obtained using both single-stage and triple-stage quadrupole mass spectrometry in conjunction with high-performance liquid chromatography. With the use of the single-quadrupole mass spectrometer and ammonium acetate as the mobile phase, enhanced sensitivity for the analytes of interest was obtained by monitoring the relatively intact [M + 1]+ or [M + 18]+ adduct ions. Further structural characterization of the carbamates was not readily obtainable owing to the lack of diagnostic bond cleavages. The single-stage quadrupole analyses were therefore complemented by triple-stage quadrupole analyses. Here, collisionally activated daughter ion spectra exhibited structure-specific fragmentations. In addition, the enhanced selectivity and specificity provided by tandem mass spectrometry allowed use of the technique as a rapid screening tool for carbamates without the need for the chromatographic separation step.
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
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    ISSN: 0887-6134
    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.1200180401
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    Mass spectral analysis of phenprocoumon and O-alkyl phenprocoumons (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 224-232 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electron impact mass spectra of the oral coumarin anticoagulant phenprocoumon and its 4-O-alkyl and 2-O-alkyl (methyl and ethyl) derivatives (including deuterium and 13C-labelled compounds) have been analysed using accurate mass measurements and B/E and B2/E constant linked-scan techniques; fragmentation routes have been proposed which are different from those for simple coumarins and other oral coumarin anticoagulants. All compounds showed an ethyl group migration from the phenylpropyl side chain to the coumarin ring; the O-alkyl derivatives presented additionally a rearrangement with bond formation between a C atom of the O-alkyl group and the phenyl ring of the side chain. Previous literature reports about fragment ion structures for methylated phenprocoumon have been revised.
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    Indole derivatization procedures for electron capture negative chemical ionization mass spectrometry: Identification of 1-methyl-1,2,3,4-tetrahydro-β-carboline in rat brain and lung (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 247-252 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Procedures have been developed for the isolation of pharmacologically active indole compounds from biological samples and for the introduction of electron-capturing groups, pentafluorobenzyl and trifluoroacetyl, onto the indole nitrogen atom. The resulting derivatives have good gas chromatographic properties and strong electron affinities which make them highly suitable for detection capture negative chemical ionization mass spectrometry. These procedures were used to identify 1-methyl-1,2,3,4-tetrahydro-β-carboline as a component of rat brain and lung.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180407
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    Mass spectrometric approaches to the confirmation of maduramicin α in chicken fat (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 57-63 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Because of the structural information it provides, mass spectrometry has gained widespread acceptance as the preferred analytical technique for drug residue confirmatory procedures. For the confirmation of the polyether ionophore antibiotic, maduramicin α, in chicken fat, the techniques of desorption chemical ionization (DCI), thermospray liquid chromatography/mass spectrometry (TSP LC/MS), and thermospray liquid chromatography/tandem mass spectrometry (TSP LC/MS/MS) were investigated as potential approaches. Sample clean-up was found to be totally inadequate for DCI and only marginally acceptable for TSP LC/MS. Only TSP LC/MS/MS adequately resolved the analyte from the tissue coextractives and generated satisfactorily reproducible mass spectrometric data for a confirmatory method. The techniques developed here should be applicable to other commonly used polyether ionophores.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180108
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    Enhanced silver cationization of polycyclic aromatic hydrocarbons containing bay regions in molecular secondary ion mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 83-85 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The relative abundances of silver cationized molecules [Ag + M]+ relative to molecular ions (M+.) in the secondary ion mass spectra of polycyclic aromatic hydrocarbons (PAHs) are directly related to the structures of the PAHs. Compounds containing a ‘bay region’, a concave area at the periphery of the molecule, give [Ag + M]+: M+. abundance ratios which exceed 0.62, whereas this ratio is less than 0.18 for the molecules that lack this structural feature. This allows the recognition of PAHs containing bay regions and the distinction of certain isomeric PAHs, such as phenanthrene and anthracene. Other metals, including copper and nickel, show similar behavior.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180112
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200180201
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    Fast atom bombardment (tandem) mass spectrometric analysis of intact polar ether lipids extractable from the extremely halophilic archaebacterium Halobacterium cutirubrum (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 96-105 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) mass spectrometric analyses of the three major polar ether lipids extracted from Halobacterium cutirubrum produced simple positive and negative ion mass spectra which contained ions with masses which corresponded to cationized or deprotonated lipid molecules. Structural information was obtained on individual components of polar lipid mixtures by discrete selection of ion masses when the instrument was operated in the tandem mass spectrometric mode. Tandem mass spectra contained abundant ions at masses which indicated collision-induced cleavage of phosphate (di)ester, sulphate ester or glycosidic linkages. This study showed that FAB (tandem) mass spectrometry can be used to analyse intact polar ether lipids present at microgram concentrations in crude lipid mixtures and these analyses can indicate the presence of structural features (i.e. O-methylation and the presence of cyclic isoprenoidyl chains) which are difficult to determine with other analytical methods.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180203
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    On-line negative ion liquid chromatography/mass spectrometry for the analysis of bile acids using low- and high-resolution mass spetrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 702-706 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatographic/mass spectrometric analysis of a mixture of bile acids has been carried out using a double-focusing mass spectrometer. A solution of polyethylene glycol was added post-column using a second pump and a micro vortex mixer. The mass spectrometer was tuned to give a 10 000 resolution, and mass measurement accuracies of greater than 3 mmu were obtained on-line.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180909
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    Direct analysis of organics contained in aqueous solutions by membrane interface: A dedicated electron impact ion source (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 707-712 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Traces of p-cresol, 2-methyl-2-pentanol and trichloroethylene in aqueous solution have been detected using a silicone membrane source adapted for a VG ZAB-2F instrument. With these solutions, flowing through a silicone capillary placed few millimetres from the main electron beam, a qualitative and quantitative analysis in the ppm range has been achieved. The influence of the main instrumental factors (solution temperature, analyte concentration, flows and different substances) has been widely studied, leading to a clear parameterization of this source.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180910
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    Gas chromatographic/mass spectrometric determination of alicyclic primary hydroxylamines in metabolic studies in vitro (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 724-726 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The combination of gas chromatography and mass spectrometry (GC/MS) is effective for separation and identification of the hydroxylamine metabolites of alicyclic primary amines after acetylation. These products give mass spectra contianing diagnostic fragment ions which are of great value for identification of metabolites. The mass spectra of diacetyl alicyclic primary hydroxylamines gave prominent characteristic peaks at m/z (M - 42), (M - 42 - 42), (M - 101), 118 (AcNOAc) and 76 (AcNOH). GC/MS analysis of the incubation extracts has shown that the N-hydroxylamines are the major metabolites of alicyclic primary amines in rabbit liver microsomes.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180913
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    Automated probe mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 733-737 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method of fully automating the analysis of routine samples using probe introduction techniques has been designed and developed. Unattended 24 h operation has dramatically increased the ability to process large numbers of samples and has freed much of an operator's time to perform other tasks.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180915
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    Collisional activation spectra of bisbenzylisoquinoline alkaloidsCDRI Commuication No. 4408. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 738-740 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Collisional activation (CA) spectra of the molecular protonated ions generated under fast atom bombardment (FAB) and the molecular ions under electron ionization (EI) from 14 bisbenzylisoquinoline alkaloids have been compared. The FAB CA spectra show mainly elimination of MeOH from the MH+ ion and no characteristic fragmentation pattern. The EI spectra, on the other hand, show abundant structurally diagnostic ions free of doubly charged ions. The double benzylic cleavage results in bisisoquinoline ions giving rise to the most intense peak in the spectra of all the compounds. Loss of one of the isoquinoline moieties comprising rings C and D and elimination of both the benzyl groups (rings E and F) are characteristic of compounds containing no 1,4-dioxine bridge (1-5). These compounds are also characterized by more abundant (〉50%) [M - Me]+ ions, while the compounds with a 1,4-dioxine bridge give [M - Me]+ ions with 〈50% abundance.
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    Characterization of the spheroliths present in primary atypical bandkeratopathy using laser microprobe mass analysis (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 753-756 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Laser microprobe mass analysis was applied to study the chemical composition of spheroliths in the Bowman's membrane of patients suffering from primary atypical bandkeratopathy. The inclusions appear to consist mainly of calcium phosphate.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180918
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    Characterization of new bacterial transformation products of 1,1,1-trichloro-2,2-bis-(4-chlorophenyl) ethane (DDT) by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 741-752 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The microbial transformation of DDT, DDD and DDE was studied in Gram-negative strain B-206 and a number of phenolic metabolites were identified as the trimethylsilyl derivatives in the bacterial extracts by gas chromatography/mass spectrometry. The major metabolites of DDT were DDD, DDE, DDMU, 1,1,1-trichloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′-chlorophenyl) ethane, 1,1,1-trichloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′-hydroxy phenyl) ethane, and 1,1,1-trichloro-2,2-bis-(2-hydroxy-4-chlorophenyl) ethane. Conversely, DDD was mainly degraded into DDE, 1,1-dichloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′-cholorophenyl) ethane and 1,1-dichloro-2-(2-hydroxy-4-chloropheyl)-2-(4′-hydroxyphenyl) ethane. Finally, DDE was transformed into DDMU, 1,1-dichloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′-chlorophenyl) ethylene, 1,1-dichloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′hydroxyphenyl) ethylene and 1-chloro-2-(2-hydroxy-4-chlorophenyl)-2-(4′-chlorophenyl) ethylene. The phenolic metabolites exhibited [M - TMSCl]+., [M - HCl - TMSCl]+. and/or [M - HCl - TMSCl - Me]+ fragment ions which reflect the presence of an ortho hydroxyl group in these molecules. Other mass spectral features used to determine their struture are presented and a metabolic scheme accounting for their formation is proposed.
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    URL: http://dx.doi.org/10.1002/bms.1200180917
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    Thermospray mass spectrometry and tandem mass spectrometry of polar, urinary metabolites and metabolic conjugates (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 767-774 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the characterization of glucuronide and sulfuric acid conjugates and alkyl phosphates by thermospray tandem mass spectrometry (MS/MS). Primary thermospray mass spectra were generated using ammonium acetate buffer and filament-on ionization with both positive and negative ion detection. In positive ion mode molecular weight information was obtained for glucuronic, phosphoric and other weak acids. Under these conditions, however, spectra were not obtained for the sulfate adducts or phosphate salts. Negative ion thermospray mass spectrometry was more versatile, providing spectra of all metabolic structures examined. Positive and negative ion mass spectra provided complementary information for glucuronic acids. Collisionally activated dissociation (CAD) mass spectra of the glucuronide [M + NH4]+ or [M - H]- ions exhibited characteristic glucuronide ‘fingerprints’ as well as prominent aglycone ions. The aryl sulfates were hydrolyzed to the corresponding phenols under buffer/thermospray conditions and for these analytes CAD mass spectra were obtained from [phenate]- or [phenol + acetate]- parent ions. The M- of dimethyl thiophosphate underwent sequential loss of alkyl and alkoxy radicals and formaldehyde with collisional activation. MS/MS greatly enhances the power of the thermospray interface by providing fragmentation information useful both in the identification of unknowns and for improved mass spectrometry specificity.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180921
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    Analysis of worker Monomorium minimum ant's venom using gas chromatography/mass spectrometry and gas chromatography/tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 780-786 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analysis of the venom of Monomorium minimum worker ants by gas chromatography/mass spectrometry and gas chromatography/Tandem mass spectrometry has shown the structures of three 2,5-dialkylpyrrolidines and 2,5-dialkylpyrrolines in the venom.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180923
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    Strategy for the analysis of cuticular hydrocarbon waxes from insects using gas chromatography/mass spectrometry with electron impact and chemical ionization (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 787-800 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatographic/mass spectrometric methods have been developed for the analysis of cuticular hydrocarbon waxes from termites, ants and house flies. A combination of electron impact, chemical ionization with ethylene oxide, methane and ammonia together with methoxy mercuration followed by reductive demercuration, enabled alkane and alkene components of waxes from Reticulitermes termites, Hypoponera eduardi, Camponotus Vagus, and Cataglyphis cursor ants and Calliphora Vomitora house flies to be characterized.
    Additional Material: 11 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200180924
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    Probing the stereochemistry of D(-)-ribose and D(-)-arabinose isomers by triple-quadrupole mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 801-808 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Collision-induced dissociations and ion-molecule reactions in a triple-quadrupole mass spectrometer are used to distinguish qualitatively between permethylated D(-)-ribose and D(-)-arabinose isomers. Differences are observed in the [MH]+ daughter ion spectra of each isomer at relatively low ion kinetic energies from 0 eV to 7 eV (laboratory frame of reference) for collisions with inert nitrogen gas. Loss of neutral methanol is favored for the D(-)-ribose isomer. With permethylated D(-)-arabinose, methanol elimination is less likely to occur and the rearrangement ion [H3COCH2CHOCH3]+ exists in significantly greater abundance. At low precursor ion kinetic energies, the D(-)-arabinofuranoside participates in a selective exothermic proton transfer reaction with methyl-amine to yield the [CH3NH3]+ ion. In contrast, the proton transfer reaction with permethylated D(-)-ribose is an endothermic process with a definite translational energy onset. From this measured threshold ion kinetic energy, the proton affinity of methyl-2,3,5-tri-o-methyl-D(-)-ribofuranoside was estimated to be 940 ± 8 kJ mol-1. In additional experiments where both saccharide isomers function as collision gases, a reactive trimethylsilyl ion is used to distinguish successfully between methyl-2,3,5-tri-o-methyl-D(-)-ribofuranoside and methyl-2,3,5-tri-o-methyl-D(-)-arabinofuranoside isomers.
    Additional Material: 7 Ill.
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    Determination of herbicides and their degradation products in surface waters by gas chromatography/positive chemical ionization/tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 820-827 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A rapid, sensitive and specific method was developed for the analysis of selected herbicides and their degradation products in surface water samples using gas chromatography/positive chemical ionization/tandem mass spectrometry (GC/PCI/MS/MS). Compounds included atrazine and its degradation products (deethylatrazine and deisopropylatrazine), simazine, alachlor and its degradation products (2-chloro-2′,6′-diethylacetanilide, 2-hydroxy-2′,6′-diethylacetanilide and 2,6-diethylaniline) and metolachlor. Daughter ion spectra for the protonated molecule of these compounds were generated and are described. The coeluting interferences present using GC/electron impact mass spectrometry in the surface water samples were eliminated by using GC/PCI/MS/MS in the neutral loss mode to detect specific daughter ions. The detection limit for most of the compounds was 200 pg, and instrument response was linear over three orders of magnitude.
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    URL: http://dx.doi.org/10.1002/bms.1200180928
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    FAB and tandem mass spectrometry of synthetic neuropeptides and their 2H-labelled analoguesPresented in a preliminary form on the Third International Symposium on The Synthesis and Applications of Isotopically Labelled Compounds, Innsbruck, 1988. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 836-840 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast atom bombardment (FAB) combined with tandem mass spectrometry has been used to verify the amino acid sequence in Org 2766 [H-Met(O2)-Glu-His-Phe-D-Lys-(Phe-OH)] and its deuterated analogues. It is shown that FAB mass spectrometry in addition to the [M + H]+ ion yields dominantly N-terminal sequence ions and some C-terminal sequence ions. These results together permit determination of the amount of deuterium incorporated and the position of the denterated amino acids in the peptide.
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    URL: http://dx.doi.org/10.1002/bms.1200180930
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    Masthead (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989) 
    Details
    ISSN: 0887-6134
    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.1200181001
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    Mass spectrometric approaches in structural characterization of cephalosporins (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 851-854 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectrometric behaviour of five structurally different cephalosporins has been studied in detail by means of different ionization/desorption methods (electron impact, fast atom bombardment, desorption chemical ionization, laser-induced vaporization) and metastable ion studies (linked scans and mass-analysed ion kinetic energy spectrometry). The best results were obtained by fast atom bombardment mass spectrometry, leading to both molecular ions and fragment ions diagnostic for structural identification.
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    URL: http://dx.doi.org/10.1002/bms.1200181002
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    The analysis and characterization of isomeric metabolites of temelastine by the combined use of thermospray liquid chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 860-866 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the development and application of a combined thermospray liquid chromatographic/mass spectrometric and liquid chromatographic/tandem mass spectrometric method for distinguishing between five isomeric metabolites of Temelastine, comprising four hydroxylated metabolites and one N-oxide. The method allows the unambiguous characterization of all of the isomers either on their own or in the presence of each other. Clear results were obtained for the characterization of these metabolites in biological samples. Temelastine showed extensive phase I and phase II metabolism and the methodology was used to study the aglycone structures of the glucuronide conjugates derived from the hydroxylated metabolites. Photo-diode array ultraviolet spectroscopy was used as a complementary technique to help elucidate the site of glucuronidation in these species.
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    URL: http://dx.doi.org/10.1002/bms.1200181004
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    The structural identification of drug metabolites using thermospray liquid chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 872-877 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structural identification of drug metabolites has been carried out using thermospray liquid chromatography/mass spectrometry (LC/MS). It has allowed the direct analysis of biological samples, in this case in vitro hepatocyte incubations, with the minimum of sample preparation. The technique also provided molecular weight information on several conjugates including glucuronides, a glutathione conjugate and one unidentified conjugate. A number of minor metabolites were also successfully identified using this method. The examples discussed in this paper illustrate the value of LC/MS in identifying unknown drug metabolites covering a wide polarity range in a complex biological mixture. However, this would not have been possible, if the interface had been unable to handle gradient separations.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181006
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    Analysis of thermoplastic resins for brominated dibenzofurans (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 884-896 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Certain thermoplastic resins, brominated diphenyl ether flame retardants, a pyrolysate and fumes collected during resin extrusion were analyzed for brominated dibenzofurans (PBDF) to assess the potential for encountering PBDF in the environment. EPA methods (RCRA Method 8280 and CERCLA IFB WA84-A002) were modified as needed to allow determination of PBDF in these matrices. Except for the base resins, all samples were found to contain PBDF. The pyrolysate also contained compounds whose structures were assigned to be brominated dioxins (PBDD) and possibly brominated xanthenes (PBX) or methyl-PBDF.
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    URL: http://dx.doi.org/10.1002/bms.1200181008
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    Fast atom bombardment tandem mass spectrometry for amino acid sequence determination in tripeptides (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 910-917 
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    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass spectral information obtained from the spectra of 26 tripeptides was carefully studied. The data were obtained from their mass, metastable ion and collisional activation spectra. On the basis of the positive ion tandem mass spectra a simple and unambiguous method for the sequence determination of amino acids in tripeptides and Y3″ ions is proposed. The use of negative ion spectra for sequence determination in tripeptides is evaluated.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200181011
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  • 195
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    Determination of pravastatin sodium and its major metabolites in human serum/plasma by capillary gas chromatography/negative ion chemical ionization mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 904-909 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary gas chromatography/negative ion chemical ionization mass spectrometry method has been developed to measure pravastatin sodium, an anti-hypercholesterolemic agent, and two of its major metabolites in human serum. Injected on a capillary column, derivatized pravastatin sodium and the two, metabolites were detected at levels of 0.5 pg μl-1 injected with a signal-to-noise ratio of 3 to 1. The limit of detection was 0.3 ng ml-1 serum of each compound with 95% confidence using a weighted linear regression analysis. Prior to analysis, samples were purified on 200 mg C18 solid-phase extraction columns and derivatized with pentafluorobenzyl bromide and N,O-bis-(trimethylsilyl)-trifluoroacetamide. An excess of pentafluorobenzyl bromide was removed by reaction with propionic acid.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181010
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  • 196
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    A rapid screening procedure for the detection and quantification of clenbuterol in bovine urine using thermospray liquid chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 935-936 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181014
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  • 197
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    Characterization of isomeric dimethylfuranocoumarins by electron impact ionization and surface and gaseous collision activation mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 927-934 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Five dimethylfuranocoumarin isomers have been examined by conventional electron impact (EI) mass spectrometry and by collisional activation tandem mass spectrometry using collisions upon both gaseous and solid targets. Kiloelectron-volt collision-induced dissociation (CID) experiments were conducted upon the molecular cation (M+.), the molecular anion (M-.) and the protonated molecule ([M + H]+). Low-energy (electron-volt) CID and surface-induced dissociation (SID) experiments were performed on the molecular cation (M+.) as a function of collision energy in order to vary the internal energy deposited into the ion.Characteristic fragment ions were observed in the EI mass spectra of each isomer, which allowed for their clear distinction. High-energy CID performed on the molecular cation (M+.) yielded similar daughter ion spectra for each isomer, although small variations in the relative intensities of selected fragment ions allowed for their distinction. Nearly identical CID spectra were obtained for the molecular anions and protonated molecules. Low-energy CID performed upon the molecular cation under multiple-collision conditions at collision energies ranging from 10 to 29 eV yielded nearly identical daughter ion spectra for all but one isomer, suggesting that isomerization to a common ion structure may have occurred. By contrast, ion/surface (SID) collisions on M+. were highly effective in distinguishing the various isomers in that characteristic fragment ions were obtained for each compound. Remarkable features of the SID data are the extensive degree of fragmentation recorded for these aromatic molecules, and the reduced tendency of the activated ion to undergo rearrangement to a common ion structure.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181013
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  • 198
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    K. Busch, G. Glish and S. Mcluckey. Mass spectrometry/mass spectrometry: Techniques and applications of tandem mass spectrometry, VCH publishing, New York, 1988. Mass Spectrometry/Mass Spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 942-942 
    Details
    ISSN: 0887-6134
    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.1200181017
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  • 199
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    Forthcoming events (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 943-943 
    Details
    ISSN: 0887-6134
    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.1200181018
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  • 200
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    Computer program (SEQPEP) to aid in the interpretation of high-energy collision tandem mass spectra of peptidesDedicated to Dr Günther Ohloff on the occasion of his 65th birthday. (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 945-957 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An algorithm (SEQPEP) that aids in the interpretation of high-energy (〉 1 kV) collision-induced dissociation mass spectra of peptide ions generated by fast atom bombardment (FAB) ionization is described. The only required input is a list of product ion masses and relative abundances generated by the mass spectrometer data system, the mass of the precursor [M + H]+ ion, and the mass of any C-terminal modification, if present (e.g., amide). Possible N-terminal modifications and amino acid compositions are not required as input. In the output, sequences are ranked according to the fraction of total product ion current that can be accounted for as either sequence-specific or non-sequence-specific fragment ions. These are listed by ion type. One of the major advantages of this program over algorithms described earlier is the incorporation of ion types more recently discovered. Also, this program is much faster, requiring less than 5 min of central processing unit time for an input of as many as 100 product ions. The results obtained from 50 peptides, including some generated when sequencing a protein of previously unknown structure, are discussed.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200181102
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