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  • Analytical Chemistry and Spectroscopy  (7)
  • Manduca sexta  (3)
  • 1985-1989  (10)
  • 1
    Electronic Resource
    Electronic Resource
    Practical considerations in the use of stable isotope labelled compounds as tracers in clinical studies (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 321-327 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Increasingly widespread usage of stable isotope tracers to aid clinical diagnosis and support basic research has stemmed from both advances in mass spectrometry and the availability of competitively priced labelled compounds. Stable isotopes have been used generally to investigate normal and abnormal metabolic pathways, to estimate energy expenditure and body composition and to quantitate substrate flux and oxidation rates. Despite the fact that the underlying principles relating to the use of stable isotopes for in vivo studies are straightforward, careful consideration must be given to all aspects of human studies. This review highlights some of these, including choice of label and tracer molecule, mode of tracer administration and sampling site, analytical instrumentation, interpretation of data and ethical constraints.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180507
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  • 2
    Electronic Resource
    Electronic Resource
    Analysis of dust and surface swab samples for octachlorodibenzo-p-dioxin and heptachlorodibenzo-p-dioxins by fused silica capillary GC with EC detection (1985)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 12-19 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Electron capture detection ; Octachlorobenzo-p-dioxin ; Heptachlorobenzo-p-dioxin ; Polychlorinated dibenzofurans ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the analysis of contaminated building dust samples and surface swab samples for octachlorodibenzo-p-dioxin (OCDD) and heptachlorodibenzo-p-dioxins (HpCDDs). The samples were analyzed by fused silica capillary GC combined with electron capture detection. Analysis was preceded by a short HPLC cleanup step designed to remove polychlorinated biphenyls (PCBs) and other compounds that might interfere. The method was found to work successfully on surface swab and dust samples known to contain PCBs, OCDD, and HpCDDs. The overall recovery of the analysis procedure for OCDD was found to be approximately 80%. The detection limit for the method was sample dependent, but for one typical set of surface swab samples was 0.2 μg/m2 of OCDD.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240080104
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  • 3
    Electronic Resource
    Electronic Resource
    Mass spectral characterization of doxylamine and its rhesus monkey urinary metabolites (1985)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1985), S. 151-158 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This study describes the use of mass spectrometry (MS), high-performance liquid chromatography (HPLC) and chemical derivatization techniques for the identification of doxylamine and five rhesus monkey urinary metabolites. The analyses were performed using chemical ionization mass spectrometry with either methane or ammonia as the reagent gas. The confirmation of the structures of two of these urinary metabolites was aided by the synthesis of doxylamine N-oxide and desmethyldoxylamine and by the use of methylation and acetylation derivatization techniques. Doxylamine N-oxide, desmethyldoxylamine, didesmethyldoxylamine, and two metabolites which resulted from the cleavage of the aliphatic tertiary nitrogen side chain to the subsequent 2-[1-phenyl-1-(2-pyridinyl)ethoxy]acetic acid or 2-[1-phenyl-1-(2-pyridinyl)ethoxy]methanol compounds were isolated and identified from rhesus monkey urine. Additional data concerning the mass spectral analysis of derivatization or reaction products from the three chloroformate reactions with doxylamine, and the synthesis and separation techniques which afforded mass spectral identification of the urinary metabolites are also presented.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200120403
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  • 4
    Electronic Resource
    Electronic Resource
    Mass spectra of aliphatic dicarboxylic acids and their dimethyl esters: Cyclic structures for the [M - H2O]+· ions from the diacids and [M - MeOH]+· ions from the dimethyl esters (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1988), S. 723-728 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl 2-oxocycIoalkane carboxylate structures are proposed lor the [M - MeOH]+· ions from dimethyl adipate, pimelate, suberate and azelate. This proposal is based on a comparison of the metastable ion mass spectra and the kinetic energy releases for the major fragmentation reaction of these species with the same data for the molecular ions of authentic cyclic β-keto esters. The mass spectra of α,α,α′,α′-d4-pimelic acid and its dimethyl ester indicate that the α-hydrogens are involved only to a minor extent in the formation of [M - ROH]+· and [M - 2ROH]+· ions, while these α-hydrogens are involved almost exclusively in the loss of ROH from the [M - RO·]+ ions (R = H or CH3). The molecules XCO(CH2)7COOMe (X = OH, Cl) form abundant ions in their mass spectra with the same structure as the [M - 2MeOH]+· ions from dimethyl azelate.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210231009
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  • 5
    Electronic Resource
    Electronic Resource
    Structure elucidation of a spirostanol glycoside from Asparagus officinalis fruits by concerted use of two-dimensional NMR techniques (1988)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 911-918 
    Details
    ISSN: 0749-1581
    Keywords: Asparagus officinalis ; Liliaceae ; Spirostanol glycoside ; 13C NMR ; DEPT ; 2D heteronuclear chemical shift correlation ; COSY ; Relayed coherence transfer ; NOESY ; INEPT ; Indirect detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complete 13C and 1H assignments for the oligosaccharide segment of a novel spirostanol glycoside were derived, and structural proof obtained, using a combination of DEPT, heteronuclear chemical shift correlation, homonuclear relayed coherence transfer, absolute value COSY, phase-sensitive double quantum filtered COSY, NOESY, INEPT and proton-detected long-range heteronuclear shift correlation via multiple quantum coherence.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260261017
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  • 6
    Electronic Resource
    Electronic Resource
    Inductively coupled plasma mass spectrometryThis paper is dedicated to the memory of the late Alan R. Date, whose work in inductively coupled plasma-mass spectrometry was a major factor in the development of the technique from a research curiosity into a superior analytical method. His untimely death in January 1988, was a sad blow, and it is hoped that this review indicates to some extent the quality and magnitude of his contributions to this methodology. (1988)
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 7 (1988), S. 425-461 
    Details
    ISSN: 0277-7037
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mas.1280070404
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  • 7
    Electronic Resource
    Electronic Resource
    In vitro ecdysteroid conjugation by enzymes of Manduca sexta midgut cytosol (1986)
    New York, NY [u.a.] : Wiley-Blackwell
    Archives of Insect Biochemistry and Physiology 3 (1986), S. 109-126 
    Details
    ISSN: 0739-4462
    Keywords: Ecdysteroid phosphoester ; Manduca sexta ; midgut ; C18 SEP-PAK ; β-glucuronidase ; sulphatase ; acid phosphatase ; ATP:ecdysteroid phosphotransferase ; Chemistry ; Food Science, Agricultural, Medicinal and Pharmaceutical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology
    Notes: In incubations with 80,000g supernatant of Manduca sexta midgut homogenates, [3H]ecdysone was converted to 3-[3H]epiecdysone and tritiumlabeled highly polar metabolites. C18 SEP-PAK cartridges were found suitable for the separation and purification of the free ecdysteroids and of the highly polar metabolites. Eighty to ninety percent of the metabolites were hydrolyzed by enzyme mixtures (mainly β-glucuronidase, sulphatase, and acid phosphatase) from molluscs, even when β-glucuronidase activity was completely inhibited by D-saccharic acid 1,4-lactone, or various human acid phosphatases (free of sulphatase activity). In each experiment, the hydrolysate contained a much higher proportion of 3-epiecydsone than the free (unconjugated) ecdysteroid fraction. [3H]ecdysone was not metabolized in anaerobic incubations of midgut supernatant that had been filtered through Sephadex G-25. Addition of 5 mM ATP and 5 mM Mg2+ restored the conjugate formation in incubations of Sephadex-filtered supernatant. Four ecdysone conjugates and two 3-epiecdysone conjugates were resolved by reversedphase ion-pair high-performance liquid chromatography. It is concluded that the midgut cytosol contains several ATP:ecdysteriod phosphotransferases. This is the first demonstration of the formation of ecdysteroid phosphoconjugates in a cell-free system.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/arch.940030202
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  • 8
    Electronic Resource
    Electronic Resource
    Selenium-77 NMR spectral analysis of selected substituted selenanes, selenanones and 3-selena-7-azabicyclo[3.3.1]nonanes and derivatives (1986)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 24 (1986), S. 947-950 
    Details
    ISSN: 0749-1581
    Keywords: 77Se NMR ; Selenanes ; Selenanones ; 3-selena-7-azabicyclo[3.3.1]nonanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of selenanes and selenanones have been examined using 77Se NMR analysis. Sharp resonances were found in all cases whether recorded at 47.7, 51.4 or 57.22 MHz or in DCCI3 or DMSO-d6. Diphenyl diselenide was used as the external reference, but all resonances were subsequently referred to dimethyl selenide (0°C, O ppm). It was observed that in the selenanone family any substituent at the α-, β- or γ-positions exerted a significant effect on the 77Se resonances. The same was true in the selenanes. Moreover, the presence of a chair-chair or chair-boat form in certain 3-selena-7-azabicyclo[3.3.1]nonan-9-ones and related 3-selena-7-azabicyclo[3.3.1]nonanes (and hydroperchlorates) induced remarkable differences in 77Se shifts. Some general observations and conclusions are delineated in terms of the influence of various groups on the 77Se resonances in these cyclic systems.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260241104
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  • 9
    Electronic Resource
    Electronic Resource
    New ecdysteroid conjugate: Isolation and identification of 26-hydroxyecdysone 26-phosphate from eggs of the tobacco hornworm, Manduca sexta (L.) (1985)
    New York, NY [u.a.] : Wiley-Blackwell
    Archives of Insect Biochemistry and Physiology 2 (1985), S. 227-236 
    Details
    ISSN: 0739-4462
    Keywords: 26-hydroxyecdysone 26-phosphate ; enzymatic hydrolysis ; ecdysteroid phosphate isolation ; ecdysteroid conjugate ; Manduca sexta ; Chemistry ; Food Science, Agricultural, Medicinal and Pharmaceutical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology
    Notes: The major ecdysteroid conjugate present in eggs (48-64 h old) of the tobacco hornworm has been purified by XAD-2 chromatography, C18 SEP-PAK separations, and ion suppression reversed-phase high-performance liquid chromatography. Enzymatic hydrolysis of the conjugate with acid phosphatase from human seminal fluid gave 26-hydroxyecdysone. The conjugate was identified as 26-hydroxyecdysone 26-phosphate by nuclear magnetic resonance and fast atom bombardment mass spectrometry. This compound is also the major conjugate of newly laid eggs (0-1 h old) of the tobacco hornworm. The role for ecdysteroid conjugates is discussed.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/arch.940020302
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  • 10
    Electronic Resource
    Electronic Resource
    Ecdysone 20-monooxygenase in mitochondria and microsomes of Manduca sexta (L.) Midgut: Is the dual localization real? (1985)
    New York, NY [u.a.] : Wiley-Blackwell
    Archives of Insect Biochemistry and Physiology 2 (1985), S. 385-396 
    Details
    ISSN: 0739-4462
    Keywords: ecdysone 20-monooxygenase ; NADPH-cytochrome c reductase ; Manduca sexta ; tobacco hornworm ; midgut ; Chemistry ; Food Science, Agricultural, Medicinal and Pharmaceutical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology
    Notes: The dual localization of ecdysone 20-monooxygenase in mitochondria and microsomes of Manduca sexta larval midgut was investigated. Cosubstrate requirements and response to osmolarity of the microsomal ecdysone 20-monooxygenase system were found to be different from those previously reported for the mitochondrial enzyme system. The microsomal monooxygenase utilized NADPH and, less efficiently, NADH as cosubstrates. NADPH and NADH effects were neither additive nor synergistic. NADPH yielded identical activities in isotonic and hypotonic incubations. Mitochondria and microsomes showed no synergistic interaction for ecdysone 20-hydroxylation. After washing of the mitochondria, a large proportion of their ecdysone 20-monooxygenase activity was lost. The extent of the loss was inversely correlated to the concentration of mitochondria in the incubation mixture. The addition of bovine serum albumin to the incubations (2 mg/ml) largely restored the original activities. The microsomal contamination in mitochondrial pellets after each of three successive washings was determined by measuring the activity of a microsomal marker enzyme, NADPH-cytochrome c reductase. At each step of the purification, the ecdysone 20-monooxgenase activity of the mitochondrial preparations far exceeded the activity attributable to the microsomal contamination. These results confirm the existence of two independent ecdysone 20-monooxygenase systems in the midgut of M. sexta larvae.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/arch.940020406
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