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  • 1985-1989  (1,994)
  • 1987  (1,994)
  • Analytical Chemistry and Spectroscopy  (1,177)
  • Chemical Engineering  (726)
  • Physical Chemistry
Source
Material
Years
  • 1985-1989  (1,994)
Year
Keywords
  • 101
    Electronic Resource
    Electronic Resource
    Thermospray LC/MS/MS analysis of wastewater for disperse azo dyes (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 343-354 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Primary effluent from a municipal wastewater treatment plant was used as the feed in bench scale activated sludge systems. These systems were spiked with disperse azo dyes at 1 mg l-1 and 5 mg l-1 levels and were sampled at various points in the process. Samples were analysed by high performance liquid chromatography with UV = visible detection and by thermospray ionization MS and tandem mass spectrometry (MS/MS) using direct injection or via column chromatography. The tandem mass spectrometry techniques were used both for method development purposes and for the specificity and extra information these techniques can provide. The investigation of the fate of disperse azo dyes in the activated sludge process was a major feature of this study. Major degradation products have been identified by tandem mass spectrometry analyses of these wastewaters. Precision and accuracy data generated by the thermospray tandem mass spectrometry technique are compared to those derived from the high performance liquid chromatography /UV-visible method.
    Additional Material: 14 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140709
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  • 102
    Electronic Resource
    Electronic Resource
    Collisional spectroscopy for unequivocal and rapid determination of morphine at ppb level in the hair of heroin addicts (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 63-68 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new analytical procedure for the identification of morphine in the hair of heroin addicts has been developed using collisional spectroscopy, on a commercially available, reverse geometry, double focusing instrument. Either collision-induced dissociation (B/E = const) linked scans or mass analysed ion kinetic energy spectra lead to an unequivocal and rapid determination of morphine in hydrolysed hair extract which may be compared with the data obtained by different and more traditional analytical methods.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140203
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  • 103
    Electronic Resource
    Electronic Resource
    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200140301
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  • 104
    Electronic Resource
    Electronic Resource
    Sequence analysis of unprotected tri-deoxyribonucleoside diphosphates by 252Cf-plasma desorption mass spectrometryThis paper is part III of a series ‘252Cf-Plasma Desorption Mass Spectrometry of oligonucleotides’. Part II corresponds to Ref. 12. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 83-90 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The negative Plasma Desorption Mass Spectra of ten unprotected tri-deoxyribonucleoside diphosphatesHereafter termed tri-deoxyribonucleotides. have been observed and analysed in detail. They all exhibit molecular ions as well as a characteristic fragmentation pattern. The ten trinucleotides selected were chosen in order to understand, in terms of sequence, the main features of the experimental spectra. It is shown that the structure and the sequence of the oligomers can be rapidly and easily derived from their PD Mass Spectrum.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140206
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  • 105
    Electronic Resource
    Electronic Resource
    Redox reactions occurring during secondary ion mass spectrometry of some heteroanthracycline antitumor antibiotic precursors (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 91-96 
    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 secondary ion mass spectra of the title compounds were produced by bombardment of solid deposits by 13 and 23 KeV cesium ions, respectively, and analyzed with a time-of-flight mass spectrometer. In addition to familiar protonation and alkali (mainly sodium) ion addition processes observed in the positive ion spectra and proton abstractions in the negative ion spectra (which enable determination of molecular weight) there is evidence from both spectral modes for oxidation-reduction processes in which species such as [M - H]+, [M - H + Na]+. and [M + 1]- are formed. It is argued that these may be formed rapidly from pre-associated molecules during bombardment/ionization rather than as a result of radiation damage. Sodium ion addition is apparently facilitated by the presence of electron pair donor groups, especially if chelation is possible.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140207
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  • 106
    Electronic Resource
    Electronic Resource
    Derivatives of dicyclopentadiene in ground water (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 97-102 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dicyclopentadiene, a waste product of manufacturing at the Rocky Mountain Arsenal near Denver Colorado, has been detected in ground water at this facility. Ground water extracts were analysed by gas chromatography-mass spectrometry (GC/MS) to determine if derivatives of dicyclopentadiene were present in addition to dicyclopentadiene and other chemical wastes. The derivatives thus identified were characterized by GC high resolution MS, deuterium exchange for active hydrogen in the chemical ionization source of the mass spectrometer, and GC/MS following on-column base catalyzed deuteration of enolizable hydrogen. Two ketone derivatives of dicyclopentadiene were identified by comparison with synthetic standards.Ground water derivatives of dicyclopentadiene were compared with mammalian enzymatic metabolites produced in vitro by incubation with immobilized rabbit liver cytochromes P-450. The metabolites were analysed by GC/MS and by GC/MS following derivatization and deuterium labelling. Although not found in ground water samples, the two metabolites were identified as monoepoxides of dicyclopentadiene by comparison with compounds synthesized in the laboratory.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140302
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  • 107
    Electronic Resource
    Electronic Resource
    Analysis of α-hydroxy metabolites of metoprolol in human urine after phosgene/trimethylsilyl derivatizationPresented at a Symposium on Analytical Techniques in Studies on Metabolism, April 1985, Stockhoim, Sweden. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 543-548 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three metoprolol metabolites containing an α-hydroxy group were identified in human urine by capillary column gas chromatography/mass spectrometry. After aqueous phase cyclization with phosgene the neutral or acidic derivatives formed were isolated by solvent extraction at pH 10 or 3, respectively. Following silylation the electron impact mass spectra of the metabolites exhibited a characteristic ion at m/z 336 of high abundance which originated from cleavage of the bond adjacent to the a-OTMS group. Most probably the identified compounds were formed by further biotransformations of α-hydroxy metoprolol, which is a primary metabolite. The analytical method is applicable to detect the metoprolol metabolites reported so far. A quantitative assay for one of the metabolites (H 119/72) with nitrogen selective detection is described. The total amount of this metabolite excreted by one subject within 24 h after dosing was about 0.25% of the given dose.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141003
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  • 108
    Electronic Resource
    Electronic Resource
    Identification of a new type of fragment ion in the collisional activation spectra of peptides allows leucine/isoleucine differentiation (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 583-586 
    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.1200141009
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  • 109
    Electronic Resource
    Electronic Resource
    Analysis of phospholipid molecular species in rat lung as dinitrobenzoate diglycerides by electron capture negative chemical ionization mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 573-578 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of electron capture negative ion desorption chemical ionization mass spectrometry was demonstrated in the analysis of phospholipid molecular species at the 1,3-dinitrobenzoate (DNB) diglyceride derivative. Modification of phosphatidylcholine (PC) or phosphatidylethanolamine (PE) by phospholipase C treatment and acylation of the resultant diglyceride with 3,5-dinitrobenzoylchloride afforded separation of the alkylacyl, alkenylacyl, and diacyl dinitrobenzoate subclasses by thin-layer chromatography (TLC). Separation of alkylacyl DNB into individual molecular species by reverse-phase high-performance liquid chromatography (RPHPLC) was demonstraed. Electron capture desorption chemical ionization of individual molecular species (10-25 ng) from a direct probe yielded a mass spectrum characterized by an intense molecular anion. This molecular anion was the base peak of the spectrum accounting for greater than 80% of the total ionization. From this molecular anion the total carbon number and degree of unsaturation of the fatty chains could be determined. Analysis of fatty acid content of the molecular species allowed unequivocal assignment of structure for the alkyl ether phospholipids. Using selected ion monitoring as little as 0.5 pmol of these species could be detected with a signal-to-noise ratio ≥3. This technique was useful in the analysis of low picomolar amounts of molecular species of ether phospholipids in the rat lung. Given an appropriate internal standard, analysis of dynamic changes in turnover, metabolism and precursor product relationships could be undertaken.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141007
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  • 110
    Electronic Resource
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    Guest editorial (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 589-589 
    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.1200141102
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  • 111
    Electronic Resource
    Electronic Resource
    Simultaneous determination of pool sizes and fractional turnover rates, of deoxycholic acid, cholic acid and chenodeoxycholic acid in man by isotope dilution with 2H and 13C labels and serum sampling (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 609-611 
    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 a method for simultaneous determination of the kinetics of the three major bile acids in man using (2,2,4,4-2H4) deoxycholic acid, (24-13C) cholic acid and (24-13C) chenodeoxycholic acid. The gas chromatographic/mass spectrometric-selected ion monitoring technique used provided complete separation of deoxycholic acid, cholic acid and chenodeoxycholic acid, which permitted simultaneous measurement of isotope ratios for all three bile acids. Since measurement of all three pool sizes and fractional turnover rates in a single experiment requires different isotopic labels for deoxycholic acid and cholic acid, we investigated the in vivo stability and applicability of (2,2,4,4-2H4) deoxycholic acid as a stable isotope marker for isotope dilution studies in man. No consistent differences were observed between deoxycholic acid pool sizes and fractional turnover rates determined in serum samples after administration of (2,2,4,4-2H4) deoxycholic acid and (24-13C) deoxycholic acid. Simultaneous administration of (2,2,4,4-2H4) deoxycholic acid (24-13C) cholic acid and (24-13C) chenodeoxycholic acid and isotope ratio measurements in serum permitted determination of pool sizes and fractional turnover rates of the three major bile acid and the 7α-dehydroxylation fraction. Pool sizes, fractional turnover rates and synthesis rates (input rates) agreed well with data obtained previously with (24-13C) labels in independent studies.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141106
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  • 112
    Electronic Resource
    Electronic Resource
    Identification of new steroids in patients with 17α-hydroxylase deficiency by capillary gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 633-637 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Urines of two children with 17α-hydroxylase deficiency contained a number of 5-pregnane- and pregnenediols, -triols and -tetrols with a hydroxy or oxo group in position 11 of the steroid ring. They are formed mainly from progesterone via 11-hydroxyprogesterone, pregnanolone and corticosterone, respectively, or from pregnenolone. Three metabolites not previously described, 16-hydroxypregnenolone, 6,21-dihydroxypregnanediol and 6-hydroxytetrahydrocorticosterone, were identified.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141111
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  • 113
    Electronic Resource
    Electronic Resource
    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200140601
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  • 114
    Electronic Resource
    Electronic Resource
    Observation of solvent effects on abundance of polyhydrogen adducts (M + nH)+ in fast atom bombardment mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 247-248 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The formation of polyhydrogen adducts of peptide molecules during fast atom bombardment (FAB) mass spectrometry (MS) is shown to be matrix dependent. FAB/MS analyses completed in glycerol solvent produced higher than expected peak intensities at m/z corresponding to (M + 2)+, (M + 3)+, and (M + 4)+ when the contributions of all stable isotopes present in the sample are included. Analysis of the same peptides in thioglycerol by positive or negative ion FAB yielded peak intensity distributions for the protonated molecule which matched those predicted from the natural abundance of stable isotopes. These findings suggest that thioglycerol should be the FAB matrix in analyses of peptides when determination of elemental or isotopic composition is desired.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140509
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  • 115
    Electronic Resource
    Electronic Resource
    Determination of the empirical formula of peptides by fast atom bombardment mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 249-256 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for calculating the empirical formulae of peptides from mass spectrometric data is described. Exact mass measurement data and isotopic peak ratios are used to generate a list of potential empirical formulae that fit a given compound within experimental error. The formulae are then analysed by a mathematical algorithm and only those corresponding to chain peptides formed from the basic amino acids are retained. Calculations conducted for typical peptides indicate that the approach may be useful for peptide identification if the experimental values are determined within an acceptable range of errors. Experimental measurements of the exact mass and isotopic peak ratios made using typical peptides demonstrate the feasibility of the approach.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140602
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  • 116
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    Editorial (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 303-303 
    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.1200140702
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  • 117
    Electronic Resource
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    Identification in man of urinary metabolites of a new bronchodilator, MDL 257, using triple stage quadrupole mass spectrometry-mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 325-330 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structure elucidation of drug metabolites directly from urine by tandem mass spectrometry (MS/MS) for a new bronchodilator is described. When urine samples from human subjects dosed with 400 mg of MDL 257 were examined by MS/MS, three major urinary metabolites previously characterized in animal studies were confirmed and two previously unsuspected metabolites were identified.Using the operational modes of a triple stage quadrupole mass spectrometer, it is possible both to detect and to identify possible metabolites. Since the pure drug and its metabolites often contain common structural daughter ions, the parent spectra of these common daughter ions should contain some or all of the molecular ions of possible metabolites. Daughter spectra of these suspected molecular ions were obtained and the resulting daughter spectra were interpreted for structural information of suspected metabolites.This study confirms the utility of MS/MS to do rapid metabolic profiling and identification directly from complex samples such as urine, with minimal time for sample preparation and analysis. This technique can provide unique and complimentary data when combined with the more classical approaches such as HPLC profiling, isolation, and off-line spectroscopy.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140705
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  • 118
    Electronic Resource
    Electronic Resource
    Direct measurement of dietary fractional absorption using calcium isotopic tracers (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 603-607 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fractional dietary Ca absorption, ‘a’, is measured by determining the ratio of two stable isotopic tracers, one of them orally (44Ca @ 0.2-0.5 mg/kg) and the other intravenously (42Ca @ 0.02-0.1 mg/kg). Thermal ionization mass spectrometry (TIMS) is used to measure the perturbation of natural abundance isotope ratios (delta % excess). Typical sensitivity of the TIMS permits detection of a 2.5 delta % excess change from the natural Ca isotope ratio with relative standard deviations of about 0.5%. At sufficiently long times absorption becomes constant so that ‘a’ is determined by a product of constants and a measured ratio.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141105
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  • 119
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    Measurement of prostaglandins, thromboxanes and hydroxy fatty acids by stable isotope dilution gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 617-621 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for measurement of PGF2α, PGE1, PGE2, 6-keto-PGF1α, TXB2, 2,3-dinor-TXB2 as well as 5-, 8-, 9-, 11-, 12-, 15-HETE and HHT, utilizing negative ion chemical ionization GC/MS is presented. A highly efficient separation and purification procedure prior to the derivatization sequence allows quantification of the arachidonic acid metabolites described in two GC/MS runs. The detection limit was in the femtomole range. Application of the method to the quantitative profiling of arachidonic acid metabolites in various tissues and incubation media is demonstrated.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141108
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  • 120
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    Monitoring the behaviour of 4-ketocyclophosphamide versus cyclophosphamide during capillary gas chromatography by mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 643-647 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary Gas Chromatography (CGC) is capable of determining underivatized cyclophosphamide (CPA) using SCOT OV 275 columns. Then CPA is subjected to in situ degradation resulting in formation of a cyclization product which can be determined selectively in biological fluids. In routine bioanalysis however cyclization products of CPA metabolites might interfere, e.g. 4-keto CPA. In the present study possible formation of cyclization products of 4-keto CPA similar to CPA was monitored by Mass Spectrometry. Cyclization of 4-keto CPA in situ was demonstrated to occur, resulting in a product similar to that of CPA. Both cyclization products could be determined selectively and it appeared that in situ cyclization of 4-keto CPA was negligible (〈5%), probably owing to extra stabilization of the CPA metabolite by keto-enol tautomerism as has been demonstrated by NMR.
    Additional Material: 14 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141113
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  • 121
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    Plasma desorption mass spectrometry coupled with conventional peptide sequencing techniques (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 669-673 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass of intact and enzymatically derived fragments of cecropin B, an antibacterial protein from the Chinese oak silk moth, Antherea pernyi, have been determined by 252Cf plasma desorption time-of-flight mass spectrometry. As a result, the carboxy terminal amino acid sequence of the protein was established.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141118
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  • 122
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    Selected ion monitoring analysis of monoamine metabolites in cerebrospinal fluid. Application to the study of in vivo effects of α2-antagonists (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 675-682 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The technique of isotope dilution mass spectrometry has been used for the measurement of biogenic amine metabolites in cerebrospinal fluid (CSF). CSF samples were collected from rabbits treated with α2-antagonists. The aim of our study was to determine the specificity of these drugs on the central nervous noradrenergic, dopaminergic and serotonergic activity as measured by the release of corresponding monoamine metabolites. 3-Methoxy-4-hydroxyphenylethylene glycol (MHPG) and vanilmandelic acid (VMA) were used as parameters for the noradrenergic activity, whereas homovanillic acid (HVA) and 5-hydroxyindole-3-acetic acid (5-HIAA) were employed to follow the dopaminergic and serotonergic activity, respectively. For the measurement of the biogenic amine metabolites a published GCMS method has been adapted. Samples of 200 μl CSF were processed. Following addition of deuterated internal standards and acidification, extraction was carried out with ethyl acetate. Preliminary experiments with the analysis of MHPG using diethyl ether for extraction gave rise to emulsion formation and resulted in poor recoveries for MHPG and in irreproducibility problems due to a preferential extraction of non-labelled MHPG, effects which were not observed with ethyl acetate extraction. Derivatization was done with a mixture of pentafluoropropionic anhydride/pentafluoropropanol (or hexafluoroisopropanol) in order to derivatize both hydroxyl and carboxylic acid groups. The derivatization procedure was optimized for the analysis of 5-HIAA by carrying out a second reaction step with pentafluoropropionic anhydride alone in order to complete the derivatization for the indolic NH moiety. The molecular ions of the derivatized products were selected for detection. The methodology has been applied to evaluate the effects of two α2-antagonists, i.e. yohimbine and idazoxan. Yohimbine was found to increase the CSF levels of the noradrenergic metabolites MHPG and VMA and of the dopaminergic metabolite HVA and to have serotonergic effects, whereas idazoxan was shown to exhibit noradrenergic effect only.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141119
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  • 123
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    Measurement of thyroxine in human serum by isotope dilution mass spectrometry. Definitive methods in clinical chemistry, V (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 683-688 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The determination of thyroid hormones is widely used for the diagnosis and therapy control of thyroid disorders. In particular, thyroxine in serum is one of the most frequently determined endocrine parameters. Unfortunately, the results obtained by the use of different commercial test kits vary significantly, and until now there has been no means to decide whether a particular enzyme or radioimmunoassay kit yields accurate results or not. It seemed, therefore, necessary to develop definitive or reference methods for the measurement of thyroxine and to apply this technique for the assessment of target values in control sera for internal and external quality control. In the present investigation, an analytical protocol using the isotope dilution mass spectrometry technique is described which is herewith proposed as a definitive method for the measurement of thyroxine in human serum. The procedure consists of the following steps. (i) Equilibration of endogenous thyroxine in a serum sample with 100 ng [13C2]thyroxine. (ii) Isolation of the thyroid hormones by using a cation exchange resin. (iii) Formation of the methyl ester by reaction with methanolic hydrochloric acid. (iv) Purification of the methyl ester by column chromatography on Sephadex LH-20. (v) Formation of the N,O-bistrifluoroacetyl derivative with trifluoracetic anhydride. (vi) Selected ion monitoring of fragment ions of the thyroxine and the [13C2]thyroxine derivatives at m/z 870 and 872 using a magnetic sector field mass spectrometer with electron impact ionization combined with a capillary gas chromatography column. This method is now used to assign target values in a German quality control scheme. The precision of the method is of the order of 1-2% (coefficient of variation).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141120
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    Identification and confirmation of arsenobetaine and arsenocholine in fish, lobster and shrimp by a combination of fast atom bombardment and tandem mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 723-732 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using fast atom bombardment (FAB) ionization combined with tandem mass spectrometry (MS/MS), the identity of arsenobetaine (AB) in extracts of sole, haddock, lobster and shrimp was unequivocally confirmed. Evidence was also presented for the presence of arsenocholine (AC) in the shrimp extract. Confirmation was obtained by comparing the collision-induced dissociation (CID) daughter ion and parent ion spectra of major ions in the FAB spectra from these extracts with those from the authentic standards.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141206
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  • 125
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    4,5-Dihydroxy-2-hexanone: A new metabolite of N-hexane and of 2,5-hexanedione in rat urine (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 563-572 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Male Wistar rats were exposed to 2000 ppm n-hexane or were treated with a single dose of 2,5-hexanedione (200 mg kg-1). Analysis of the urine collected after both treatments revealed the formation of 4,5-dihydroxy-2-hexanone via 5-hydroxy-2-hexanone or 2,5-hexanedione, respectively. Identification of this new n-hexane metabolite included enzymatic hydrolysis of the excreted glucuronide, derivatization of the keto group with O-methylhydroxyl-amine, and subsequent GC-MS analysis. The chemical structure derived from the mass spectra obtained was confirmed by further analysis of the methoxime-TMS derivatives and of deuterated 4,5-dihydroxy-2-hexanone excreted after treating rats with 2,5-[2H10]-hexanedione. 4,5-Dihydroxy-2-hexanone is proposed to be identical with a urinary constituent that is excreted by rats after n-hexane exposure and is converted to 2,5-dimethylfuran or 2,5-hexanedione, respectively, depending on the conditions of urine treatment prior to GC-MS analysis.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141006
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  • 126
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    Fast atom bombardment mass spectrometry of butyloxycarbonyl protected (BOC) peptides (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 53-61 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fast atom bombardment positive ion mass spectra and the [M + H]+ collisional activation spectra of t-butyloxycarbonyl protected peptides and the unprotected analogues have been compared. It is concluded that sequence information, especially from the collisional activation spectra, can better be derived from the underivatized peptides than from the BOC-peptides.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140202
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  • 127
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    Analysis of peptides containing oxidized methionine and/or tryptophan by fast atom bombardment mass spectrometryMention of a commercial or proprietary product in this paper does not constitute endorsement by the U.S. Department of Agriculture. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 69-72 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of peptides containing methionine and/or tryptophan with dimethylsulfoxide/hydrochloric acid/acetic acid resulted in oxidation of these amino acids respectively to methionine sulfoxide and oxyindolalanine. This reaction was monitored by fast atom bombardment mass spectrometry using a dithiothreitol/dithioerythritol liquid matrix. Under these conditions, only methionine and tryptophan were oxidized. Comparison of mass spectra of a sample before and after oxidation should provide a rapid screening procedure for determination of these residues in peptides.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140204
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  • 128
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    Mass spectrometry of the picolinyldimethylsilyl (PICSI) ethers: New derivatives for the structural determination of unsaturated fatty alcohols by gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 103-109 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Picolinyldimethylsilyl (PICSI) derivatives of long-chain fatty alcohols were prepared either in a two stage sequence involving reaction of the alcohol with an excess of bis(diethylamino)dimethylsilane followed by 3-pyridylcarbinol or by direct reaction with diethylaminodimethylsilyl-3-pyridylcarbinol. The mass spectra of the resulting PICSI derivatives were characterized by very abundant (base peak) molecular ions and a series of abundant radical-induced cleavage ions the masses and abundances of which gave information on the presence and position of double bonds from both mono- and poly-unsaturated alcohols.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140303
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  • 129
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    Identification and quantification of arsenocholine and acetylarsenocholine in trace amounts in biological material by use of pyrolysis gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 117-125 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical method, based on a selective extraction and pyrolysis gas chromatography/mass spectrometry assay of arsenocholine and acetylarsenocholine in aquatic organisms, is described. Characteristic fragmentation patterns were obtained from pyrolytically demethylated compounds. The molecules were rearranged in unique pathways which differed from those of corresponding nitrogen analogues. Qualitative determination of arsenocholine and acetylarsenocholine was achieved by gas chromatographic as well as mass spectrometric analysis of the thermal degradation products (trimethylarsine, dimethylvinylarsine and the demethylated arsenocholine or acetylarsenocholine). Arsenocholine and acetylarsenocholine in fish from industrially polluted water were isolated and identified. Massfragmentographic quantification of the arsenic compounds in fish was carried out by use of deuterium labelled analogues of arsenocholine and acetylarsenocholine as internal standards. The method showed a high sensitivity.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140305
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    A comparison of chromatographic and chromatographic/mass spectrometric techniques for the determination of polycyclic aromatic hydrocarbons in marine sedimentsNRCC No. 26728. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 375-381 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The establishment of reliable values for concentrations of 16 priority pollutant polycyclic aromatic hydrocarbons (PAH) in a suite of marine sediment reference materials included an examination of the methods used to determine such compounds. Results from the five techniques used indicate large method biases. The biases arise from chemical interferences in methods which use non-selective measuring systems with separation techniques which do not first completely resolve the analytes; e.g., single-parameter optical detectors with high performance liquid chromatographic (HPLC) techniques or a flame ionisation detector (FID) with capillary column gas chromatographic (GC) methods. Measurement by a mass spectrometer with HPLC and GC removes much of the method bias. Results for a representative sediment are discussed to illustrate these conclusions.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140805
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  • 131
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    Ionization dynamics within the high pressure electron capture mass spectrometer; the unusual spectra of derivatized polycyclic aromatic amines and perchlorinated unsaturated hydrocarbons (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 401-415 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A kinetic model for chemical events occurring within the high pressure electron capture mass spectrometer (HPECMS) ion source is developed which includes four different pathways by which unconventional negative ions can be produced. These routes to unusual ions include reactions of gas phase free radicals, surface-assisted reactions, ion-electron and ion-ion recombination reactions, and ion-wall neutralization. The model developed here provides a diagnostic tool useful for the elucidation of unusual HPEC spectra. Such spectra for two environmentally important classes of compounds are explained by use of the model. These compound classes include the trifluoroacetic derivatives of polycyclic aromatic amines, which have been shown to be present in materials derived from liquified coal, and the derivatives of hexachlorocyclopentadiene, which are used as pesticides. It is shown in this study that several processes, in addition to electron capture, can be operative in the typical HPECMS ion source, and that these processes can be used advantageously for the generation of informative and sensitive mass spectral signals.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140808
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  • 132
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    Gas chromatographic/mass spectrometric characteristics of purified synthetic isomers of tetrachlorodibenzofuranNRCC No. 27656. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 457-464 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thirty seven of the thirty eight isomers of tetrachlorodibenzofuran (TCDF) have been synthesized by unambiguous routes, and purified. The 1,2,8,9-TCDF isomer could not be thus prepared, and attempts to make it by pyrolysis of appropriate precursors also failed. Retention characteristics of TCDFs under gas chromatographic conditions were determined, and found to agree well with those predicted by an existing mathematical model derived from data obtained for TCDF isomers prepared by more ambiguous procedures. Mass spectral characteristics were also obtained, particularly relative response factors for the molecular ions of the TCDF isomers under electron ionization (EI) conditions. A discussion of the likely transferability of these relative response factors between mass spectrometers of different types is included. Chemical ionization (CI) mass spectra were also obtained, for both positive and negative ions. These CI spectra yielded little structural information not available from the EI data, and problems of lack of sensitivity and of reproducibility render them less suitable for trace analysis of TCDFs. Some unusual ion chemistry was observed under CI conditions, which can be rationalized in terms of pre-ionization attack on the TCDF molecule by free radicals in the source.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200140813
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200140901
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    FD and FAB mass spectra of some oligopeptides of the tryptophyllin familyThis paper has been presented in part as a poster at the 10th International Mass Spectrometry Conference, Swansea (UK), 13 September 1985. Abstract no. 534. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 487-493 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass spectra of some natural thryptophyllins and synthetic analogues have been obtained by using field desorption and fast atom bombardment as soft ionization techniques to overcome the low volatility of these oligopeptides. Field desorption spectra generally show the molecular ion as base peak; some fragments of thermal origin are present at higher emitter heating current, thus providing additional structural information.Fast atom bombardment mass spectra show a more regular fragmentation of the peptide backbone, which allow the complete amino acid sequence to be checked. The presence of two consecutive proline residues in some of the examined molecules affects their fragmentation pattern in both field desorption and fast atom bombardment mass spectrometry giving rise to spectral features which are useful from the diagnostic point of view.The two ionization methods are compared and the advantage of the combined use of both techniques is pointed out.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140903
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  • 135
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    Bioavailability determination of lidocaine by capillary gas chromatography ammonia chemical ionization mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 513-516 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method was developed to measure bioavailability of lidocaine by simultaneous peroral and intravenous dosing. Lidocaine hydrochloride corresponding to 125 mg base was given perorally. Simultaneously, 30 mg of deuterated lidocaine-d3 were injected intravenously. Blood samples were taken at intervals for 270 min. Plasma samples were spiked with mepivacaine hydrochloride as internal standard, alkalinized to pH 11.7 and extracted with diethyl ether. The extracts were analysed by capillary GC ammonia CI MS using a 15 m × 0.32 mm i.d. glass capillary column coated with SE-54. The ion source pressure was 0.4 Torr of ammonia as reagent gas. Quasimolecular ions were monitored at m/z 235, 238 and 247 for lidocaine, lidocaine-d3 and mepivacaine, respectively.Calibration curves were linear from 0.2 to 5.0 nmol lidocaine ml-1 plasma. Interday reproducibility of this method was 6.9% for lidocaine-d3 (n = 16; 1.90 ± 0.13 nmol ml-1). Bioavailability of lidocaine in 5 normal volunteers ranged from 26 to 36% (mean 31 ± SD 5%) and in a cirrhotic with an end-to-side portacaval shunt it approached 100%, as anticipated. The method is well suited for determination of bioavailability of lidocaine after simultaneous administration of rather small and safe doses both intravenously and perorally.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140906
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  • 136
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200141001
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  • 137
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    Study of deuterium isotope effects on protein binding by gas chromatography/mass spectrometry. Caffeine and deuterated isotopomers (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 653-657 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A study of the binding to human serum albumin (HSA) of caffeine and its deuterated isotopomers, 1-C2H3-, 3-C2H3-, 1,7-(C2H3)2-, 3,7-(C2H3)2- and 1,3,7-(C2H3)3-caffeine, was performed by equilibrium dialysis. Free and bound fractions were measured by gas chromatography/mass spectrometry. Important and significant (Fischer and Student tests) isotope effects were observed on binding parameters: sites total concentration (N = 1732) μM for 1,3,7-(C2H3)3-caffeine versus 822 μM for caffeine; number of sites (n = 3 for 1,3,7-(C2H3)3-caffeine v. 1 for caffeine); and extent of binding (46% for 1,3,7-(C2H3)3-caffeine v. 27% for caffeine).A study of competition for HSA binding between caffeine and its 1,3,7-(C2H3)3- and 3,7-(C2H3)2-isotopomers confirmed the results obtained in direct binding studies. These isotope effects are discussed in terms of (a) tools for molecular pharmacology, (b) precautions to be taken when such labelled drugs are used in clinical pharmacology.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200141115
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    A mass spectrometric approach to the identification of conjugated drug metabolites (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 689-697 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For the identification of intact underivatized drug conjugates, the mass spectrometric technique of choice is fast atom bombardment (FAB); the combined use of both positive and negative ion FAB usually provides information on the molecular mass and nature of conjugates under study, while the number of exchangeable hydrogen atoms can be determined using trideuterated glycerol as the FAB-matrix. Electron impact and desorption chemical ionization spectra can be used to study the aglycone part of the conjugated metabolites. With this approach metabolites conjugated with glucuronic acid, sulphuric acid and amino acids have been identified. The identification was supported by analysis of reference compounds, prepared by chemical synthesis. The examples given are selected from current metabolism studies on drug candidates in development within Organon's research.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141121
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  • 139
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    Structural determination of lipid a from gram negative bacteria using laser desorption mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 591-598 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Laser desorption mass spectrometry has been employed for the structural determination of lipid A components derived from the lipopolysaccharides (LPS) of gram-negative bacteria. Mass spectra were obtained for methylated monophosphoryl lipid A from Neisseria gonorrhoeae and Rhodopseudomonas sphaeroides, for diphosphoryl lipid A from Escherichia coli and for the intact LPS from the Re Mutant of E. coli consisting of triphosphoryl lipid A and two KDO (2-keto-3-deoxyoctonate) units. Fragmentation of the phosphate (or pyrophosphate) on the reducing glucosamine is followed by fragmentation of acyl-linked fatty acids. Also observed are fragmentions which correspond to the distal portion of the molecule.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141103
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  • 140
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    Metabolic kinetics and quantitative analysis by isotope dilution thermospray LC/MS (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 623-625 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of thermospray LC/MS for quantitative analysis using isotope dilution is reviewed. Assays for acetylcholine, glucose, sorbitol, cortisol, testosterone and 1,25-(OH)2-vitamin D in biological fluids are discussed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141109
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  • 141
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    Identification of urinary metabolites in rats exposed to the nephrotoxic agent 2,3,4-trimethylpentane (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 639-641 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Branched-chain hydrocarbon-induced nephropathy in male rats was examined using 2,3,4-trimethylpentane. Lesions are elected only in male rats, not in females or in controls. Mechanisms of nephropathy may be the interaction of metabolites with the male rat-specific protein alpha 2u globulin. The identified urinary metabolites of 2,3,4-trimethylpentane in male rats given the hydrocarbon by gavage are 2,3,4-trimethyl-1-pentanol, 2,3,4-trimethyl-2-pentanol and 2,3,4-trimethyl-1-pentanoic acid. Of the C8-isomers, 2,3,4-trimethylpentane dosing leads to the highest incidence of kidney damage in male rats.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141112
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  • 142
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    Quantitative determination of erythromycin 2′-ethylsuccinate in human plasma by fast atom bombardment mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 659-662 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for simultaneous quantitative determination of erythromycin 2′-ethylsuccinate and erythromycin in human plasma is described. After extracting the deuterium-labelled internal standards and analytes from alkalinized plasma to diethyl ether the extracts were analysed by fast atom bombardment mass spectrometry. The quantification limit for 2′-ethylsuccinate ester was 50 ng ml-1 and for erythromycin 100 ng ml-1. The calibration curves were linear up to 5 μg ml-1 for both. The precision of the method at higher concentration was less than 2% and at the quantification limit ∼6% for both analytes.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141116
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  • 143
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200141201
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  • 144
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    Picogram level determination of fluphenazine in human plasma by automated gas chromatography/mass selective detection (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 699-704 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated capillary column gas chromatography electron-impact mass selective detection method has been developed for the determination of a major tranquilizing agent, fluphenazine. Using a new purification method and incorporating a deuterated internal reference, a limit of quantitation of 50 pg per ml of plasma was obtained.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200141202
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  • 145
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    Analysis of native neutral glycosphingolipids by combined high performance liquid chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 149-153 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conditions for normal phase high performance liquid chromatrography-chemical ionization mass spectrometry of underivatized glycosphingolipids with the use of a moving belt transport interface were investigated. Chromatography was performed on a 2 mm ID × 3 cm column packed with 5 μm spherical silica. A gradient of increasing methanol and water in methylene chloride was used to resolve mono-, di-, tri-, and tetraglycosylceramides and sulfatides in less than 15 min. A polyimide belt was used to transport the sample residues to the mass spectrometer where ammonia chemical ionization mass spectrometry was used to obtain spectra. One to 5 μg of each component was sufficient to obtain full spectral scans. Mono- and dihexosylceramide spectra showed [M + H]+ ions of good abundance, while the higher glycosphingolipids have molecular weights that exceed the range of the mass spectrometer utilized. All glycosphingolipids gave ions characteristic of their ceramide, fatty acid, long chain base and carbohydrate components. Sequence information which reflected the relative position of hexose and N-acetylhexosamine residues was also obtained.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140403
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  • 146
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    Identification and quantitation of alcophosphamide, a metabolite of cyclophosphamide, in the rat using chemical ionization mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 167-172 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alcophosphamide was identified in urine obtained from Sprague-Dawley rats treated with a 1:1 mixture of cyclophosphamide and β-(2H4)cyclophosphamide using chemical ionization mass spectrometry and the ion cluster technique. This compound was also quantified in rat plasma using gas chromatographic-mass spectrometry under ammonia chemical ionization following administration of cyclophosphamide. Apparent terminal half life of 76.2+/-13.7 min and area-under-the concentration-time curve value of 24.8+/-8.6 μg min/ml were obtained for derived alcophosphamide following iv bolus administration of cyclophosphamide. Following co-administrations of unlabeled and β-(2H4)cyclophosphamide via iv/po and iv/ip routes, apparent terminal half-lives of 68.4+/-16.4 and 71.8+/-10.1 min were found for the iv portions and 106.7+/-25.2 and 73.9+/-5.2 min for the non-iv portions, respectively, for the derived alcophosphamide. Phosphoramide mustard was found to be a major circulating and urinary metabolite in the rat following iv administration of preformed alcophosphamide which gave a plasma half-life of 1.9 h.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140406
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  • 147
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    Confirmative assay and quantitative determination of Hedera Helix L. saponins (α-hederin, hederacosides B and C) in raw plant extracts and in cosmetic formulations by EI and CAD MIKE spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 187-194 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The current methods for the qualitative and quantitative control of cosmetologically active triterpenic saponins in raw plant extracts and in cosmetic formulations are far from satisfactory in terms of specificity and sensitivity. Here we describe a method for the simultaneous detection and quantification of Hedera helix L. saponins directly using crude extracts from plant and cosmetic matrices. The first is achieved by conventional EI-mass spectral analysis (direct DEI conditions); the second by CAD MIKE spectrometry (collisionally activated decomposition mass-analysed ion kinetic energy spectrometry) of the EI-induced fragmentation product at m/z 248, which is common to the three saponins of Hedera helix L. (α-hederin, hederacosides B and C). The method is sensitive (sub ppb level), specific and since it is rapid it might be conveniently employed for the routine quality control of these active constituents in plant extracts and in cosmetic formulations.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140409
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  • 148
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    A comparison of the gas chromatographic and mass spectrometric properties of the pentafluoropropionyl and heptafluorobutyryl derivatives of the methyl, trifluoroethyl, pentafluoropropyl and hexafluoroisopropyl esters of twelve acidic metabolites of biogenic amines (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 197-206 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The gas chromatographic and mass spectrometric properties of the methyl, trifluorethyl, pentafluoropropyl and hexafluoroisopropyl esters of the pentafluoropropionyl and heptafluorobutyryl derivatives of twelve important acidic metabolites of biogenic amines have been investigated. The optimum derivatization conditions for the different classes of metabolites have been established and the byproducts formed in some of the derivatizations have been identified. Under certain derivatizing conditions, back-exchange of deuterium in the labelled internal standards was observed. No single derivative appears to be ideally suitable for the simultaneous quantitative analysis by GC/MS of all twelve metabolites, so extracts of plasma and urine were split and a combination of the methyl or trifluoroethyl esters of the pentafluoropropionyl derivatives were used.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140502
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  • 149
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    Profiling and quantification of biogenic amines in wine by constant B2E linked scan mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 229-233 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The constant B2E linked scan is shown to be an excellent tool for the profiling of biogenic amines in wine samples. The fragment ion at m/z 169 of the dansylated amines is used for the precursor ion search in combination with direct sample evaporation. Besides the profile a semi-quantification may be achieved when using suitable amines as internal standards with standard deviations of 12-17%. More accurate results with standard deviations of 3-5% are obtained when using deuterated analogues as internal standards. Both methods are applied to the analysis of biogenic amines in synthetic mixtures and actual wine samples.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140506
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  • 150
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    252-Californium plasma desorption mass spectrometry of glycerophospholipids (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), 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: 252-Californium plasma desorption mass spectrometry was applied to the study of five different classes of phospholipids namely phosphatidylcholine, phosphatidylethanolamine, phosphatidylglycerol, phosphatidylserine and phosphatidylinositol. Positive and negative ion spectra were compared to spectra obtained using other ionization techniques. Plasma desorption mass spectra provide useful information on the molecular weight of compounds from all classes, particularly in the case of phosphatidylserine - a class that has failed to show satisfactory quasimolecular ions with either Fast atom bombardment, FAB or Field desorption, FD. The observed fragmentation is also indicative of the structure of the studied compounds.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140508
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  • 151
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    Use of immobilized exopeptidases and volatile buffers for analysis of peptides by fast atom bombardment mass spectrometryMention of a commercial or properietary product in this paper does not constitute endorsement by the U.S. Department of Agriculture. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 235-239 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: β-Lipotrophin (62-77) or Ac-gastrin releasing peptide was incubated with immobilized carboxypeptidase Y or aminopeptidase M. Subsequent aliquots of each incubation mixture were analysed by fast atom bombardment mass spectrometry using a dithiothreitol/dithioerythritol liquid matrix. The use of immobilized enzymes and volatile buffers for exopeptidase digestions enabled rapid and facile separation of enzyme from digestion products. This approach to mass spectral peptide analysis reduced spectral background arising from a glycerol matrix, buffer salts, or enzyme proteins and contaminants, enabling analysis of as little as 200 picomoles of a suitable peptide.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140507
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  • 152
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    Fast atom bombardment/tandem mass spectrometry of physalaemin-like peptides (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 281-287 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fragment ion spectra obtained from collision-induced decomposition of protonated molecular ions have been used to determine amino acid sequences of several physalaemin-like peptides which were recently purified from rabbit stomach. This technique was chosen because the peptides were available in microgram quantities and were anticipated to contain pyroglutamate as the blocked N-terminal residue. Such spectra of several synthetic analogs of the naturally occurring peptides were obtained and analyzed to confirm the veracity of this peptide sequencing strategy. In addition, methyl ester derivatives of these synthetic peptides provided a crucial test for the spectral interpretation via the mass shifts thus induced.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140607
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  • 153
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    Forthcoming events (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 301-302 
    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.1200140610
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  • 154
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    Formation of [M + 14] anions from fluorene: Negative ion CI studies using GC/MS, MS/MS and FTMS (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 395-399 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Under negative ion chemical ionization conditions, fluorene yields an anion at [M + 14] mass units. This species has been determined to correspond to [M + O - 2H]-, with the loss of two hydrogen atoms at the C-9 position and addition of oxygen to form a structure similar to 9-fluorenone.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140807
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  • 155
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    The electron capture negative ion mass spectra of 2,6-dinitroaniline and 2,4-dinitrophenol herbicides and related nitrobenzene derivatives (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 417-434 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron capture, negative ion mass spectra of a group of 2,6-dinitroaniline and 2,4-dinitrophenol herbicides are presented. In addition, the spectra of a series of mono- and dinitrobenzene derivatives are reported. These compounds exhibit a wide range of fragmentation behaviors. Simple spectra, dominated by intense molecular ions, are observed for certain groups of compounds, while others give spectra dominated by ions which result from ortho interactions and other complex rearrangements. The fragmentation behavior of these compounds is investigated using isotopically labelled compounds and accurate mass measurements. The question of nitro group reduction reactions, under electron capture conditions, is examined using 15N labelled compounds. Electron capture negative ion (ECNI) mass spectrometry is found to be a sensitive and reproducible technique for the identification of nitro compounds.
    Additional Material: 19 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140809
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  • 156
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200140201
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  • 157
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    Determination of the urinary cortisol production rate using (1,2,3,4-13C)cortisol. Isotope dilution analyses at very small enrichments (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 73-82 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An isotope dilution mass spectrometric method to determine the urinary cortisol production rate (CPR) in babies and children is described. The method uses stable isotopically labelled (1,2,3,4-13C)cortisol. The tracer is intravenously administered to the patient and urine is collected for the following three days. Following extraction, enzymic hydrolysis, purification and isolation by high-performance liquid chromatography (HPLC) the urinary cortisol metabolites tetrahydrocortisone, tetrahydrocortisol, α- and β-cortolone are separately oxidized to the common product, 11-oxo-aetiocholanolone. The methyl oxime tert-butyldimethylsilyl ether derivative (MO TBDMS) was analysed by gas chromatography mass spectrometry. Quantification of the isotope enrichment was carried out by selected ion monitoring of the base fragment ion at m/z 344[M-103]+ for unlabelled, and at m/z 348 for labelled 11-oxo-aetiocholanolone. HPLC isolation of the metabolites together with the oxidation step allowed very small isotope enrichments, sometimes down to 0.1% (1:1000), to be reliably measured against a linear calibration graph containing 0 to 1% (13C4) enrichments. The standards for the calibration graph were synthesized from mixtures of labelled (13C4) cortisol and natural cortisol, and the calibration graph was prepared each time samples were measured. The long term instrumental precision of the isotope dilution analyses was 0.91% for a derivatized sample containing a (13C4) enrichment of 0.5% (measured on six different days over seven months). The coefficient of variation of the complete procedure for the four cortisol metabolites was between 1.17 and 2.14%. The clinical applicability of the method is demonstrated by presenting the results of a CPR determination in a patient.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140205
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  • 158
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    Routine gas chromatographic/mass spectrometric analysis of urinary organic acids. Results over a three-year period (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 663-668 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organic acidaemias are an important part of inborn errors of metabolism. The biochemical diagnosis is based on gas chromatographic/mass spectrometric identification of urinary organic acids. Since 1973 we have used gas chromatographic analysis of the methyl esters of urinary organic acids. Mass spectral identification was performed only when an abnormal gas chromatographic profile was suspected. In 1983 we introduced routine gas chromatographic/mass spectrometric analysis organic acids. More than 1500 urine samples from 1000 children have been analysed and we encountered more than 40 abnormal profiles: 18 classical organic acidaemias (propionic, methyl-malonic, isovaleric, glutaric type I and 3-hydroxy-3-methyl glutaric acidaemias); 6 aminoacidopathies with excretion of branched chain keto acids (leucinosis) or succinylacetone (tyrosinosis type I); 14 massive dicarboxylic acidurias with excretion of suberyl and hexanoyl glycine and deficiency of the medium chain acyl CoA dehydrogenase in four patients. The use of gas chromatography/mass spectrometry routinely allows the identification of abnormal metabolites excreted in small amounts: β-methyl-crotonyl glycine indicative of biotin deficiency: γ-hydroxybutyric acid; and 3-methyl-glutaconic + 3-methy-glutaric acid is in a 3-methyl-glutaconic aciduria type II. Abnormal profiles due to metabolites of drugs as valproate, salicylate and barbiturate can be recognized immediately. This simple gas chromatographic/mass spectrometric system can lead to diagnosis, in one day, of rare but severe diseases needing a specific and early treatment.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141117
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  • 159
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    Determination of serum cortisol by thermospray liquid chromatography/mass spectrometry: Comparison with gas chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 717-722 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The determination of serum cortisol by thermospray liquid chromatography/mass spectrometry (LC/MS) has been assessed. The method incorporates stable isotope dilution and innumoadsorption extraction. [M + H]+ ions are monitored during LC/MS. The within-assay reproducibility is satisfactory (coefficient of variation 7% at a concentration of 190 ng ml-1), though inferior to that achieved with the (more lengthy) procedure of gas chromatography/mass spectrometry (GC/MS). Satisfactory agreement between LC/MS (y) and GC/MS (x) data was observed (y = 0.934x + 12.4 ng ml-1; r = 0.968; n = 14). It is concluded that the generation of precise reference data for the assessment of routine cortisol assays is at present better achieved by GC/MS. LC/MS, however, provides satisfactory quantitative data via a more simple and rapid method.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141205
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    The alkylthio-isoindole derivatives of biogenic amines: A mass spectrometric study (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 737-738 
    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.1200141208
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  • 161
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    Determination of deuterium level in biological fluids by isotope ratio mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 339-342 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water is produced by vacuum sublimation of biological fluids directly into reaction vessels in preparation for reduction using zinc. Following heating to 450°C the hydrogen produced is admitted directly to the mass spectrometer. The standard derivation, σ10 of analysis of water samples was 1.08-1.23% while for blood plasma σ6 = 2.02-2.62%. The method allows the determination of very low levels of deuterium in biological fluids, thus allowing very small doses of deuterium oxide to be used in studies of body water in animals and possibly humans.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140708
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200140801
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  • 163
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    Analysis of cyclopentafused isomers of benz(a)anthracene in wood smoke (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 369-374 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A previously-unidentified peak occurring in chromatograms of the polycyclic aromatic hydrocarbon fraction from wood smoke particulate extracts analysed by capillary gas chromatography on a DB-5 column was found to correspond in retention index and molecular mass either to benzo(a)fluoranthene or to benzo(1)aceanthrylene, one of a series of four novel and highly mutagenic cyclopentafused isomers of benz(a)anthracene. Detailed sub-fractionation, and re-analysis on a liquid crystal capillary column, indicated that the identity of this peak was most likely to be benzo(a)fluoranthene, a compound not previously reported in woodsmoke.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140804
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  • 164
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    Determination of polycyclic aromatic hydrocarbons and alkylated-polycyclic aromatic hydrocarbons in particulate extracts using negative ion chemical ionization mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 383-394 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatography/mass spectrometry using a combination of electron impact (EI) and Negative Ion Chemical Ionization (NICI) was used for the determination of polycyclic aromatic hydrocarbons (PAH) and alkylated-PAH in extracts of two particulate materials which are Standard Reference Materials: SRM 1650 Diesel Particulate Matter, and SRM 1649 Urban Particulate Matter. The selectivity of NICI mass spectrometry for certain PAH enabled identification and selective determination of isomeric PAH and alkylated-PAH in the particulate SRMs. Quantitative determinations for methylfluoranthenes, methylpyrenes, methylbenzofluoranthenes and methylbenzo(a)pyrenes in the two particulates showed that the methyl-substituted species were present at levels as high as 30 percent of the parent-PAH concentrations. Similarities in the alkylated-PAH content of the air and diesel particulate materials are discussed in relation to the sources of the two materials.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140806
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  • 165
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    Environmental contamination by polychlorinated dibenzo-p-dioxins and dibenzofurans associated with pulp and paper mill discharge (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 443-447 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sludge from seven pulp and paper mills was analysed for 2,3,7,8-TCDD. The level of contamination ranged from not detectable (1 pg/g) to over 400 pg/g. Analyses for other planar polychlorinated contaminants indicated high levels of contamination by other PCDDs and PCDFs. Polychlorinated xanthenes and xanthones were identified as potential interferences in these analyses.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140811
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  • 166
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    A hybrid HRGC/MS/MS method for the characterization of tetrachlorinated-p-dioxins in environmental samplesPresented in part at 13th Annual Meeting of the Federation of Analytical Chemistry and Spectrometry Societies, St. Louis, Missouri, September, 1986. (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 449-456 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new instrumental method for the characterization of the analyte 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) by selected reaction monitoring (SRM) analysis is investigated. The method uses high-resolution gas chromatography coupled to a hybrid tandem mass spectrometer. The technique was evaluated with regard to four performance parameters: sensitivity, linearity, repeatability and selectivity. The method compares favorably with the traditional selected ion monitoring HRGC/HRMS technique, and the selectivity of the new method is shown to surpass the established HRGC/HRMS method. This new method could allow the characterization of samples that have undergone less rigorous cleanup than is now possible by the traditional mass spectrometric methods. The presence of TCDDs in a real sample was confirmed by using the new HRGC/(hybrid)MS/MS SRM method, which was not possible by using HRGC/HRMS analysis.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200140812
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    Isotope effect in negative ion chemical ionization mass spectrometry of deuterium labelled lormetazepam (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 257-261 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This study identified the reason for the poor quantification of Iormetazepam-TMS (1) using negative ion chemical ionization with lormetazepam-1,1,1-2H3-TMS (2) as an internal standard. Mass spectra of lormetazepam and its deuterium labelled compounds determined at various ion source temperatures (100-250°C) gave almost the same behaviour for 1 and lormetazepam-3′,4′,5′,6′-2H4-TMS (3) but a different one for 2, suggesting that the poor quantification was due to an isotope effect. This was confirmed by the findings that the ratios of ion currents of the base peaks of 1 and 3 were independent of the ion source temperature but those of 1 and 2 varied markedly with it. This phenomenon was also observed in the mass fragmentography of the molecular ion, although to a lesser degree than that of the above fragment. In both positive ion chemical ionization and electron impact ionization modes, no isotope effect arose because there was no corresponding fragment to cause the isotope effect.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140603
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  • 168
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    GC/MS identification of organosulphur compounds in environmental samples (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 275-280 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Twenty-one organosulphur compounds were detected in a survey of water, industrial effluent, sediment and fish samples, using automated gas chromatography/mass spectrometry developed for the identification of forty target semi-volatile and volatile organosulphur compounds. The compound classes detected in the environmental samples are three allotropes of sulphur, three thioethers, five sulphones, six thiophenes, one thiol, two sulphonamides and one thiazole. The compounds were detected in the approximate concentration range 0.1 to 2000 parts per billion (ppb). α,α-Dichlorodimethyl sulphone was detected in environmental samples subjected to biodegradation and chemical treatment.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140606
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  • 169
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    A system for collecting high-resolution time-of-flight mass spectrometric data (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 295-299 
    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.1200140609
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  • 170
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    Field desorption tandem mass spectrometry of anthracycline antibiotics, cosmomycin A, B, A′, B′, C and D (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 305-312 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Field desorption mass spectrometry was applied to a series of underivatized anthracycline, cosmomycins, to obtain fragment ions which were mass analysed using the linked scan technique without using collision activated dissociation. The daughter spectra of the various protonated compounds contain sugar sequence information which is in the mass spectra. The mass spectrometric data make it clear that field desorption tandem mass spectrometry can become a valuable additional technique for the structural analysis of anthracyclines.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140703
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  • 171
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    Characterization of benzo(a)pyrene metabolites by high performance liquid chromatography-mass spectrometry with a direct liquid introduction interface and using negative chemical ionization (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 555-561 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polynuclear aromatic hydrocarbons are ubiquitous pollutants that may become highly carcinogenic during their metabolism by organisms. Benzo(a)pyrene is an example of such a compound. Benzo(a)pyrene metabolite standards, which are labile, polar compounds, have been used to evaluate high performance liquid chromatography-mass spectrometry as an analytical technique for polynuclear aromatic hydrocarbon metabolites. The chromatography used microbore (1 mm i.d.) C18 columns with acetonitrile/water as the elution solvent which became the reagent/moderator gas. A direct liquid introduction interface was used and characteristic spectra were obtained in the negative chemical ionization mode. Molecular or pseudomolecular ions were obtained for five phenols (m/z 268 and m/z 267) and three trans-dihydrodiols (m/z 286, m/z 285, m/z 284). Useful spectra were also obtained for a tetrahydrotriol, four tetrahydrotetrols and three conjugated metabolites. Fragmentation usually involved loss of water and anions at m/z 284 and m/z 268 were common to most of the spectra. Variations in the source/desolvation chamber temperature between 175°C and 275°C caused significant alterations in the relative abundance of molecular and fragment ions. Dissociative electron capture was the dominant ionization process.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141005
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  • 172
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    Use of the ‘ortho effect’ for chlorinated biphenyl and brominated biphenyl isomer identification (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 579-582 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The ‘ortho effect’, observed for chlorinated biphenyls (PCBs) and brominated biphenyls (PBBs) having the 2,2′, 2,2′,6 or 2,2′,6,6′ halogens, can be combined with GC retention index for isomer specific identifications by gas chromatography/mass spectrometry (GC/MS). This technique reliably allows accurate structure assignments for environmental monitoring without the use of multiple GC determinations that employ different chromatographic phases. Validation of the ortho effect for 129 PCBs and PBBs is reported, including a survey of all PCB mass spectra in the EPA/NIH mass spectral database. Presence or absence of ortho effect and reduction in magnitude for 2,2′, 6,6′ substitution may be related to the formation of a planar, bridged halonium ion intermediate upon electron ionization in the mass spectrometer.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141008
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  • 173
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    Masthead (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987) 
    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.1200141101
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  • 174
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    HPLC of anions on coated reversed phase columns using indirect UV-detection and eluents containing nitrophthalic acids (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 12-16 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; HPLC of anions ; Coated reversed phase columns ; Indirect UV-detection ; Nitrophthalic acids in HPLC eluents ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analysis of anions by HPLC has been optimized in the direction of reduced analysis times with standard reversed phase columns and UV detection. This was achieved by use of a new eluent containing 3-nitrophthalic acid and small proportions of acetonitrile. Resin-based and silica-based anion exchangers of varying ion-exchange capacities are prepared with cetyltrimethylammonium bromide by a rapid dynamic coating technique. Some new, strong eluents containing nitrophthalic acids are evaluated and compared with an eluent containing potassium hydrogen phthalate. Addition of acetonitrile was found to improve the retention behavior of mono- and divalent anions. An automatic system was developed for the analysis of chloride, nitrate, and sulfate in drinking water. It is shown that a water sample can be analyzed in less than two minutes on a column of 25 mm length.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100103
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  • 175
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    Microbore HPLC column performance and temperature programming capabilities (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 27-31 
    Details
    ISSN: 0935-6304
    Keywords: Microbore HPLC Column ; Performance and Temperature ; Programming Capabilities ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Microbore columns (1 mm i.d.) are compared to conventional 4.6 mm i.d. columns with respect to speed, efficiency and sensitivity. If column lengths, particule diameter, packing efficiency, mobile phase, and linear velocity are the same, most chromatographic properties such as speed (analysis time), efficiency, pressure drop, and sensitivity are the same. The major differences are the column volumes, the void volumes, and the volumetric flow rates for equal linear flow velocities. The low flow rates of microbore columns (30 to 200 μl/min), conserve solvent and make for easier interfacing to other instruments such as MS, NMR, or FTIR. Temperature programming of microbore HPLC columns produces faster analyses for large k′ values, increased sensitivity (due primarily to sharper peak shape), and increases the range of compounds which can be handled in an isocratic mode.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100106
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  • 176
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    Chromatography calendar (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 50-52 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100113
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  • 177
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    Selective removal of water in purge and cold-trap capmary gas chromatographic analysis of volatile organic traces in aqueous samples (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 60-66 
    Details
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Cold-trapping ; Drying ; Gas stripping ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The design and features of an on-line purge and cold-trap pre-concentration device for rapid analysis of volatile organic compounds in aqueous samples are discussed. Excessive water is removed from the purge gas by a condenser or a water permeable membrane in order to avoid blocking of the capillary cold-trap. Synthetic mixtures covering concentrations ranging from tenths to tens of ppb's and different chemical classes are used to study the effect of various process factors on the efficiency and selectivity of water removal as well as on the purging recovery. The importance of the concentration of the solutes, the flow rate in conjunction with the volume of the purge gas, and the temperature of the condenser, the cold-trap and the sample is emphasized. Theoretical models describing the purge process and the blocking of the cold-trap agree fairly well with the highly reproducible experimental results (σ = 2-4%). Both the condenser and the Nafion membrane successfully remove water, although some compounds, dependent on volatility and polarity, are partly or completely lost. It is shown that non-polar volatile organic compounds are efficiently enriched so that recoveries between 80-100% and a detection limit of 1 ppt can be obtained. The applicability of the system is illustrated on some examples.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100202
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  • 178
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    Product news (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 93-93 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100208
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  • 179
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    Chromatography calendar (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 94-94 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100209
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  • 180
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    Permethylated β-cyclodextrin as stationary phase in capillary gas chromatography (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 105-107 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography (GC) ; Capillary column ; Permethylated β-cyclodextrin stationary phase ; Positional isomers separation ; Enantiomer pair separation ; 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/jhrc.1240100214
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  • 181
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    Masthead (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987) 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100301
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  • 182
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    Separation and determination of purpurea glycosides in Digitalis purpurea leaves by micro-HPLC (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 137-140 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography, Micro-HPLC ; Purpurea glycosides ; Digitalis purpurea ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A micro high-performance liquid chromatographic (micro-HPLC) method was developed for the determination of purpurea glycoside A, purpurea glycoside B, and glucogitaloxin in Digitalis purpurea leaves. The extract of dry leaf powder was applied to a Sep-Pak silica cartridge followed by preparative thin-layer chromatography prior to micro-HPLC analysis. The analysis was performed on an ODS micro column, using acetonitrile-methanol-water (21:20:45) and ultraviolet detection (220 nm). The amounts of purpurea glycoside A, purpurea glycoside B, and glucogitaloxin per 100 mg of dry leaf powder were estimated to be 52.6, 50.7, and 108.6 μg, respectively.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100306
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  • 183
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    Determination of ethyl carbamate in alcoholic beverages by two-dimensional gas chromatography (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 151-152 
    Details
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Column switching ; Alcoholic beverages ; Ethyl carbamate ; 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/jhrc.1240100310
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  • 184
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    A contribution to high-temperature silylation (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 158-159 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Silylation ; Critical surface tension ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100313
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  • 185
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    Improved heat-shrinkable PTFE joints also for thin capillaries (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 156-157 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Polytetrafluoroethylene (PTFE) joints ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100312
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  • 186
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    Obituary (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 172-172 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100402
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  • 187
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    Long-acting androgens: Analytical and preparative HPLC of testosterone esters (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 186-190 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Analytical HPLC ; Preparative HPLC testosterone esters ; Long-acting androgens ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Procedures are described for the normal phase and reverse phase HPLC analysis of testosterone esters having diverse side chains: examples are given of the gram-scale purification of these compounds using two commercial preparative liquid chromatography and an economical and efficient laboratory-assembled preparative liquid chromatograph.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100406
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  • 188
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    Evaluation of dead time calculation in liquid chromatography using a linearization procedure for homologous series (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 191-200 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Dead time calculation ; Homologous series ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mathematical method for the calculation of the dead time (tm) in HPLC was evaluated using a computer simulation approach, in which artificial perturbations were introduced to Simulated homolog retention times. The calculation was based on a modified and extended Grobler and Bálisz (GB) method. Investigated wav how the precision of the calculated tM is affected by: statistical fluctuations in retention times and which, and how many homolog retention times are used. Based on these simulations a two-step procedure for the tM calculation is proposed: In the first step the linearity of log tR, n vs carbon number n is checked using as many homolog retention times as possible. The slope value bo of the first linear regression in the GB method is used for the selection of homolog retention times in the final tM calculation. In the second step the optimal selection of homologs is made and the final tM calculation is carried out. Guidelines for homolog selection are given.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100407
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  • 189
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    Collection of gas chromatographic fractions for NMR analysis (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 213-214 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cryogenic trapping ; NMR analysis ; Flavor and aroma analysis ; 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/jhrc.1240100414
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  • 190
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    Masthead (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987) 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100501
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  • 191
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    High precision trace analysis in capillary gas-liquid chromatography using an inlet based on the static solvent effect (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 235-239 
    Details
    ISSN: 0935-6304
    Keywords: Trace analysis ; Capillary chromatography ; Solvent effect inlet ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A sample inlet, based on the static solvent effect has been designed and constructed. The inlet can handle samples up to 20 μl which allows for the detection, using an F. I. D., of constituents in the parts per billion range. The reproducibility of the inlet in terms of peak percentage area is around 1% relative standard deviation over a range of chemical types.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100505
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  • 192
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    Supercritical ammonia as mobile phase in capillary chromatography (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 257-262 
    Details
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Capillary columns ; Ammonia ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Instrumentation was assembled that allows the use of supercritical ammonia as mobile phase in capillary supercritical fluid chromatography. Several modifications of the typical chromatographic system were necessary, especially with respect to injection and detection. In addition, the stabilities of various polysiloxane stationary phases were studied. The chromatography of polarizable and polar basic materials was demonstrated using a nonpolar polysiloxane stationary phase.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100509
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  • 193
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    Sample introduction in high speed capillary gas chromatography; input band width and detection limits (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 273-279 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; High speed capillary GC ; Sample introduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The speed of analysis in capillary gas chromatography can be substantially increased by reduction of the column inner diameter. However, special demands are then posed upon instrumental design. In particular, the sampling system is highly critical because it has to be capable of delivering extremely small injection band widths which must be compatible with the column inside diameter. This study focuses on the evaluation of two potentially suitable sample introduction systems with respect to input band width and detection limits and their compatibility with small bore (≦ 100 μm) columns in capillary gas chromatography. One of them allows liquid on-column injection, based on liquid splitting, of only a few nl onto small bore (≦ 100 ◂m) fused silica columns. For gases, input band widths as low as 1 ms are obtained with this system. The other one is part of a miniaturized gas chromatograph with extremely low dead volume interfaces and detector volumes. It allows input band widths for gases of a few ms. Without any preconcentration ppm concentrations are measured in gaseous samples with a 80 ◂m thick film capillary column. It will be shown that a further reduction of the minimum detectable amount and analysis time is possible with this equipment.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100512
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  • 194
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    Siloxane/silarylene copolymers as stationary phases for capillary gas chromatography part I: Evaluation of silanol terminated dimethyl substituted polymers (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 302-318 
    Details
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Silanol terminated dimethylsiloxane/silarylene copolymers ; Silanol terminated dimethylpolysiloxane ; Thermal immobilization ; High temperature columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermal stability of silicones can be improved on replacement of certain of the oxygen atoms in the polymer backbone by phenyl groups. Such a polymer has been synthesized and evaluated for use as stationary phase in fused silica capillary gas chromatography; the polymer was dimethyl substituted and silanol terminated. A selectivity was provided by the phenyl groups in the backbone. For comparative purposes, a silanol-terminated dimethylpolysiloxane has also been evaluated.Both stationary phases gave columns of highest separation efficiency and the supporting fused silica surface was deactivated by the stationary phases on thermal treatment. Further, low column bleeding was observed at the maximum temperature tested, 370°C. The phenyl-containing phase could be immobilized to 60% by heat treatment, but the pure dimethylpolysiloxane was 10% immobilized. The influence on immobilization of factors such as nature of the supporting surface, stationary phase silanol content, reaction temperature and atmosphere in the column during reaction has been studied.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100516
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  • 195
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    An off-line two-dimensional analytical procedure for determination of polycyclic aromatic hydrocarbons in smoke aerosol (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 342-347 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Two-dimensional HPLC ; Smoke aerosol ; Polycyclic aromatic hydrocarbons ; Stoves ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Smoke aerosol from stoves consists of a wide variety of chemical substances of which a number have toxic properties. To study the impact of aerosol emissions on health and environment reliable analytical procedures must be available for these samples. An off-line two-dimensional HPLC method is described for the determination of a number of polycyclic aromatic hydrocarbons (PAH). The method consists of a HPLC clean-up step yielding distinct fractions on activated silica and followed by analysis of each of the fractions by isocratic reversed phase HPLC. Detection is by UV and fluorescence monitors in series. Combination of the chromatographic data obtained from both the clean-up and analytical step provides additional qualitative information.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100605
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  • 196
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    Electronic Resource
    The “disturbing zone” in overpressure layer chromatography (OPLC) (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 352-356 
    Details
    ISSN: 0935-6304
    Keywords: Overpressure layer chromatography, OPLC ; Disturbing zone ; “PRISMA” model ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the fundamental factors causing the “disturbing zone” in OPLC. This phenomenon of distorted substance zones appears when the OPLC separation is started with a dry layer and is due to interaction between the gas that is physically bound to the surface of the sorbent (ma) and the gas molecules dissolved in the eluent (ms). Possibilities for elimination of the adverse effects of disturbing zones ultimately depend on the establishment of operating conditions that inhibit their initial formation. Since modification of the location of the disturbing zone is only possible within a very narrow range, the sole solution to this problem is to conduct a pre-run, which may be carried out with hexane in the case of separation of apolar compounds. For separation of polar substances, the pre-run may also be performed with hexane or with a solvent of the mobile phase in which the components are unable to migrate. The selection of this solvent may be considered during the optimization of the eluent system.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100607
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  • 197
    Electronic Resource
    Electronic Resource
    A simple and efficient cryogenic trapping device for odor evaluation of aroma fractions (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 369-370 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cryogenic effluent trap ; Odor evaluation ; Aroma fractions ; 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/jhrc.1240100613
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  • 198
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    Electronic Resource
    Masthead (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987) 
    Details
    ISSN: 0935-6304
    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/jhrc.1240100701
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  • 199
    Electronic Resource
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    Comparison of methods to enhance flame ionization detector (FID) signals in gas chromatography (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 392-397 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; FID signals ; Signal handling ; Signal enhancing ; Data acquisition ; Smoothing filtering correlation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The performances of some numerical methods to improve the signal to noise ratio are compared and applied to enhance noisy signals obtained in gas chromatography with capillary columns and a flame Ionization detector. Several methods have been considered: cutoffs In the Fourier transform of the recorded signal; real time numerical filtering; theoretical model curve fitting; and the correlation of a chromatogram recorded from a pseudorandomly injected sample with the pseudorandom injection function. Numerical real time filtering is shown to be the most convenient method when the main periodic component of the noise has been determined by Fourier analysis.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100705
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  • 200
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    Liquid chromatographic trace enrichment with on-line capillary gas chromatography for the determination of organic pollutants in aqueous samples (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 17-24 
    Details
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Retention gap ; LC trace enrichment ; Aqueous samples ; Organic pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trace enrichment for the GC analysis of a series of chlorinated pesticides and polychlorinated biphenyls (PCBs) in aqueous samples has been achieved through a simple on-line technique involving sorption on an LC micro-precolumn followed by direct elution into a gas chromatograph with hexane. A 5-m retention gap coupled to the capillary GC column served as the recipient of a relatively large sample volume (ca. 100 μl) introduced into the GC. Partially concurrent solvent evaporation during sample introduction allowed a large sample capacity. Recoveries of more than 95% were observed for the majority of the compounds studied. Using 1.0 ml aqueous samples, detection limits of less than 1 ppt were found. The applicability of the developed method was demonstrated for a river water sample.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100104
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