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  • Articles  (97)
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  • Analytical Chemistry and Spectroscopy  (97)
  • 1985-1989  (97)
  • 1975-1979
  • 1970-1974
  • 1986  (97)
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  • Articles  (97)
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  • 1985-1989  (97)
  • 1975-1979
  • 1970-1974
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  • 1
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Nitrogen/phosphorus detector ; Doxylamine metabolites ; Antihistamines ; Rhesus monkey ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A high resolution gas chromatographic method is described for the separation of rhesus monkey urinary metabolites of doxylamine with the use of on-column injection, a fused silica column (DB-1701), and nitrogen/phosphorus detection. An ancillary separation of doxylamine and six other antihistamines is also presented.
    Additional Material: 5 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 506-514 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Deactivation ; Gas chromatography, GC ; Small diameter capillary columns ; Organosilicon hydrides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Small diameter fused silica capillary columns (50-75 μm i.d.) were deactivated at relatively low temperatures (250-300°C) with a mixture of polymethylhydrosiloxanes and several lowmolecular-weight organosilicon hydrides. Reproducible surface deactivations of highest quality were achieved with the polymethylhydrosiloxane (PMHS) reagent. Deactivations performed with PMHS via dynamic coating with neat or diluted reagent were evaluated by gas chromatography. Deactivations achieved with organosiloxane mono-, tri-, and tetrahydrides were also evaluated and compared. Low-molecular-weight organosilicon hydride deactivations were less time consuming and required lower head pressures for filling and coating columns with the reagent. Critical surface tensions of capillary surfaces modified with PMHS and the low-molecular-weight organosilicon hydrides gave support to the dehydrocondensation reaction between silica surface silanols and silyhydride bonds of the reagents. Slopes from Zisman plots indicated that coverage of the surface ranged from highest for the polymer (PMHS) to lowest for the monomers (TMS and PMDS). Efficiency measurements showed the influence that surface modification had on the uniformity and stability of the coated capillary columns. Well-deactivated capillary columns permitted the chromatography of polar solutes using supercritical carbon dioxide as mobile phase.
    Additional Material: 5 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 199-204 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive- and negative-ion mass spectra of five glycoconjugates were obtained using laser desorption/Fourier transform mass spectrometry. These were the glycoalkaloids α-solanine and α-tomatine and the steroid glycosides gitoxin, lanatoside A and digitonin. Doping with KCl yielded both potassium- and chloride-attachment ions. Few fragment ions were observed for these species, with the exception of digitonin, although the negative-ion spectra showed relatively more fragmentation than the positive-ion spectra. All major fragments appeared to arise from losses of sugar groups due to cleavages at the glycosidic linkages. This contrasted sharply with the behavior of the malto-oligosaccharides studied in this laboratory.
    Additional Material: 6 Ill.
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  • 4
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A study of the positive and negative ion, ammonia (NH3 and N2H3) direct chemical ionization mass spectrometry of highly purified prostaglandin endoperoxide (PGH2) is presented. The positive ion spectra were characterized by an intense [M+NH4]+ adduct at m/z 370 and several fragment ions, most notably a [M+NH4 - H2O]+ ion at m/z 352 and an ion at m/z 298, assigned as the [M+NH4 - 72]+ ion of 12-hydroxy-5,8,10-heptadecatrienoic acid formed from PGH2 in the spectrometer. The negative ion spectra of PGH2 were characterized by a base peak at m/z 352 [M]- and by an ion at m/z 334 corresponding to the loss of water from the parent ion. A combination of negative ion and deuterated ammonia reagent gas was used in making assignments and in demonstrating that the spectra observed were due to intact PGH2 and its stable PGE2 and PGD2 isomers formed in the spectrometer. In addition, use of the latter reagent gas was shown to clearly distinguish between several arachidonic acid metabolites, differing in their number of exchangeable protons. Furthermore, preliminary results with several stable prostaglandins indicate that the spectra are sensitive to different functional groups that are present. Consequently, it would appear that negative and positive ion, NH3 (N2H3) direct chemical ionization mass spectrometry would be useful in the analysis of labile arachidonic acid metabolites, without the need for prior derivatization.
    Additional Material: 5 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 167-170 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The interaction of nucleic acid bases with the alkylating antitumour drug thiotepa has been studied by field ionization mass spectrometry. The possibility of interaction between all four DNA bases and thiotepa in neutral aqueous solutions was demonstrated. The analysis of the data for different methylated bases made it possible to elucidate some sites of alkylation - N(1)(Cyt), N(3)(Thy), N(9)(Ade) - which are compared with data on other alkylating agents available from the literature.
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  • 6
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new method based on selected ion monitoring chemical ionization mass spectrometry was developed to measure the quaternary ammonium neuromuscular blocking agents, pancuronium and vecuronium, in serum. An ion-pair extraction procedure is utilized to separate the compounds of interest from biological fluids. The intensities of the ion currents produced by the bisamines formed from the drugs and the corresponding deuterated internal standards through thermolytic dequaternization are monitored. The assay shows good linearity over the range of 1-500 ng/ml. This assay has been utilized in a variety of clinical pharmacokinetic studies involving surgical pediatric, geriatric and obstetric patients requiring anesthesia.
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 53-56 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vitamin D3 sulphate (SD3) identification in human milk was obtained using Desorption Chemical Ionization (DCI). The chemical ionization reagent gas used was nitrogen, molecules were ionized when the emitter was heated. SD3 was obtained from lactarium human milk and purified by high-performance liquid chromatography (HPLC). A selected ion monitoring (SIM) measurement was carried out with typical ions, m/z 366 for SD3 and m/z 384 for parent vitamin D3, the intensity ratio (I366/I384) greater than 1 being related to the presence of the sulphoconjugated form of vitamin D3 in the sample analysed. The detection of small quantities of SD3 in human milk is possible using this technique.
    Additional Material: 4 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1986), S. 15-19 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multiple carbon-13 internal standards improve the precision and accuracy of the mass spectrometric analysis of polychlorinatedbiphenyl (PCB) congeners compared to analyses using a single carbon-13 internal standard. The mean percentage error in PCB congener analysis on the μg g-1 level using multiple ion detection and three carbon-13 internal standards was 6.29%. This precision in single laboratory work suggests that the method will be useful for interlaboratory studies monitoring PCB residues and contaminats of public health significance.
    Additional Material: 3 Ill.
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  • 9
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An x-ray fluorescence technique involving a 30 mCi 238Pu as a source of primary radiation and a two-channel thin NaI(Tl) crystal spectrometer was developed for the analysis of coal ash samples. The geometry of the source-target-detector assembly is described. The ash content is estimated using an x-ray backscattering method which includes compensation for iron x-ray fluorescence. About 120 Indian coal samples were analysed and the results show that the ash content varies from 10 to 40%.
    Additional Material: 7 Ill.
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  • 10
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Combining desorption ionization with tandem mass spectrometry overcomes the disadvantage of limited fragmentation accompanying desorption and permits mixtures of closely related substances to be investigated directly. These features of the combination are illustrated by completing the structure-proof of a minor component of an ornithine-containing lipid mixture isolated from Thiobacillus thiooxidans. The minor component is a homolog of the major constituent and differs from the principal component owing to the presence of a double bond in lieu of a cyclopropyl ring in one of the constituent fatty acids. Another feature of the combined method is the potentially complementary nature of collision-activated dissociation spectra of protonated and cationized biomolecules. This is illustrated by the differences in the collision-activated dissociations of the [M + Na]+ of sucrose, desorbed by field desorption, and [M + H]+, desorbed by fast atom bombardment. A third illustration is the application of field desorption and tandem mass spectrometry to an organometallic compound. The combined approach allows the ligands to be identified and the relative ligand binding energies to be approximated.
    Additional Material: 5 Ill.
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