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  • 1
    Electronic Resource
    Electronic Resource
    High resolution recycle gas chromatography with off-line flame ionization detection (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 497-503 
    Details
    ISSN: 0935-6304
    Keywords: Recycle gas chromatography ; Capillary columns ; Off-line flame Ionization detector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preliminary results of a recycle system employing fused silica capillary columns are discussed. The unit, which can be operated with a pre-column for multidimensional GC, utilizes continuous stream splitting for off-line flame ionization detection. Commercially available rotary valves were used for recirculation of the chromatographic zone between column loops. Adsorptive activity, which is shown to be additive, is a serious limitation in the analysis of polar compounds. The successful application of recycle chromatography to increase resolution on non-polar mixtures is demonstrated.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100904
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  • 2
    Electronic Resource
    Electronic Resource
    Rapid and quantitative extraction and analysis of trace organics using directly coupled SFE-GC (1989)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 714-720 
    Details
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Capillary gas chromatography ; On-line coupling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Supercritical fluid extraction can be coupled with capillary gas chromatography (SFE-GC) using commercially-available on-column or split/splitless injection ports. While liquid solvent extractions require several hours or even days to perform, SFC-GC analyses can be completed in ≤ 1 hour including extraction, analyte concentration, and GC separation. SFE-GC yields chromatographic peak shapes that compare favorably with those obtained using conventional liquid solvent injections. Quantitative extraction and recovery of analytes is usually achieved in 10 minutes, and maximum sensitivity is obtained since the extracted analytes can be quantitatively transferred into the GC column for cryogenic focusing prior to GC analysis. SFE-GC analysis of a variety of organic pollutants from environmental solids and sorbent resins, and flavor and fragrance compounds from food products will be discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240121105
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  • 3
    Electronic Resource
    Electronic Resource
    Desorption chemical ionization and fast atom bombardment mass spectrometric studies of the glucuronide metabolites of doxylamine (1986)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 627-632 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three glucuronide metabolites of doxylamine succinate were collected in a single fraction using high-performance liquid chromatography (HPLC) from the urine of dosed male Fischer 344 rats. The metabolites were then separated using an additional HPLC step into fractions containing predominantly a single glucuronide metabolite. Analysis of the metabolites by methane and ammonia desorption chemical ionization, with and without derivatization, revealed fragment ions suggestive of a hydroxylated doxylamine moiety. Identification of the metabolites as glucuronides of doxylamine, desmethyldoxylamine and didesmethyldoxylamine was accomplished, based on determination of the molecular weight and exact mass of each metabolite using fast atom bombardment (FAB) ionization. This assignment was confirmed by the fragmentation observed in FAB mass spectrometric and tandem mass spectrometric experiments. Para-substitution of the glucuronide on the phenyl moiety was observed by 500-MHz nuclear magnetic resonance (NMR) spectrometry. A fraction containing all three glucuronide metabolites, after a single stage of HPLC separation, was also analysed by FAB mass spectrometry, and the proton- and potassium-containing quasimolecular ions for all three metabolites were observed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200131108
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  • 4
    Electronic Resource
    Electronic Resource
    Quantitative estimation of quaternary ammonium neuromuscular blocking agents in serum by direct insertion probe chemical ionization mass spectrometry (1986)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 327-332 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new method based on selected ion monitoring chemical ionization mass spectrometry was developed to measure the quaternary ammonium neuromuscular blocking agents, pancuronium and vecuronium, in serum. An ion-pair extraction procedure is utilized to separate the compounds of interest from biological fluids. The intensities of the ion currents produced by the bisamines formed from the drugs and the corresponding deuterated internal standards through thermolytic dequaternization are monitored. The assay shows good linearity over the range of 1-500 ng/ml. This assay has been utilized in a variety of clinical pharmacokinetic studies involving surgical pediatric, geriatric and obstetric patients requiring anesthesia.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200130703
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  • 5
    Electronic Resource
    Electronic Resource
    Fast atom bombardment mass spectrometry of alkali metal fluorides and chlorides; a comparison of the solid salt and glycerol matrix spectra (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 20 (1985), S. 600-605 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Fast Atom Bombardment (FAB) mass spectra of the alkali metal chlorides (Na, K, Cs) and fluorides (Na, K, Rb, Cs) were obtained from solids and a glycerol matrix, using a fast atom bombardment source. From solids the fluorides exhibited an ion abundance enhancement of the well-known [M(MF)4]+ cluster, which decreased with increasing cation size. A gradual decrease in the n=4 enhancement was observed as the salt was diluted with glycerol. In the chlorides only sodium chloride showed the n=4 relative enhancement. The mass spectra of the salts from a glycerol matrix at molar ratios of 1:1 to 1:10 showed that the spectra of the 1:1 solutions were similar to those from the solids, while glycerol adducts were found to increase with increasing glycerol concentration. A [M(MX)n(gly)]+ species that featured successive losses of HX was observed. It has not been established whether HX losses take place in solution, in the surface/vacuum interface and/or whether gas phase reactions might be responsible for the observation of the [M(MX)n(gly)-y HX]- species in the mass spectra of the MX/glycerol system.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210201003
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  • 6
    Electronic Resource
    Electronic Resource
    Ion-molecule reactions observed for nitroaromatic compounds in negative ion fast atom bombardment mass spectrometry (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1988), S. 685-691 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analyses of a series of nitroaromatic compounds using fast atom bombardment (FAB) mass spectrometry are discussed. An interesting ion-molecule reaction leading to [M + O - H]- ions is observed in the negative ion FAB spectra. Evidence from linked-scan and collision-induced dissociation spectra proved that [M + O - H]- ions are produced by the following reaction: M + NO2- → [M + NO2]- → [M + O - H]-. These experiments also showed that M-· ions are produced in part by the exchange of an electron between M and NO2- species. All samples showed M-·, [M - H]- or both ions in their negative ion FAB spectra. Not all analytes studied showed either [M + H]+ and/or M+· in the positive ion FAB spectra. No M+· ions were observed for ions having ionization energies above ∼9 eV.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210231002
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  • 7
    Electronic Resource
    Electronic Resource
    Positive ion-molecule reactions in OCS/hydrocarbon mixtures (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 20 (1985), S. 115-121 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The positive ion-molecule reactions of OCS have been investigated in an ion cyclotron resonance spectrometer. A variety of reactions in OCS/hydrocarbon mixtures have been investigated for various C1—C4 hydrocarbons - alkanes, alkenes and alkynes. The formation of organosulfur ions is found in reactions in OCS/hydrocarbon (Cn) mixtures with n 〈4. Formation of organosulfur ions is observed from hydrocarbon ions reacting with OCS and [OCS]+· and S+· reacting with the hydrocarbons. The proton affinity of OCS has been determined to be 688.7±8 kJ mol-1 while that of CS2 is measured to be 712.1±8 kJ mol-1. Comparison with the proton affinity of CO2 shows that the proton affinity increases as sulfur is substituted for oxygen.
    Additional Material: 7 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210200209
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  • 8
    Electronic Resource
    Electronic Resource
    Use of fast atom bombardment mass spectrometry for the characterization of nitroaromatic isomers (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1988), S. 267-273 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive and negative ion fast atom bombardment (FAB) mass spectra of some monosubstituted nitroaromatic isomers are reported. Generally ions carresponding to [M + H]+ and M+ are observed in the positive ion FAB spectra; ions such as [M - H] - and M-· are observed in the negative ion FAB spectra. The use of FAB mass spectra to distinguish the isomers is discussed. Comparisons of FAB, chemical ionization and electron impact mass spectra of the same isomers (wherever possible) are reported. The structural information obtained in the negative ion FAB spectra complement those obtained in the positive ion FAB spectra.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210230409
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  • 9
    Electronic Resource
    Electronic Resource
    Ion formation in fast atom bombardment mass spectrometry: a divided probe investigation of gas-phase reactions (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 24 (1989), S. 497-503 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Some ion-formation processes during fast atom bombardment (FAB) are discussed, especially the possibility of reactions in the gas phase. Divided (two halves) FAB probe tips were used for introducing two different samples into the source at the same time. Our results showed [M + A]+ ions (where M = crown ethers and A = alkali metal ions), can be produced, at least in part, in the gas phase when crown ethers and sources of alkali metal ion are placed on two halves of the FAB probe tip. The extent of this ion formation depends on the volatility of the crown ether and on steric factors. Cluster ions such as (M + LiCl)Li+, (2M + LiCl)Li+, [2M + K]+ and [2M + Na]+ are also observed to form in the gas phase. Unimolecular decompositions contribute to some ions detected in FAB. When the alkali ion salt and the crown ether are mixed together the probability of [M + A]+ ion formation increases significantly, regardless of the volatility of the crown ether.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210240710
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  • 10
    Electronic Resource
    Electronic Resource
    Comparison of the thiocarbonyl13C NMR resonances of N-phenylthioureas, N-phenyl thiocarbamates and N-phenyl dithiocarbamates (1986)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 24 (1986), S. 460-461 
    Details
    ISSN: 0749-1581
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 13C NMR spectra of N-phenylthioureas, N-phenyl thiocarbamates and N-phenyl dithiocarbamates of the ethyl and n-butyl type are compared. Significant differences are observed in the chemical shift of the thiocarbonyl carbon, which do not parallel the electronegativity of the bonded heteroatom.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260240513
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