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  • 1
    ISSN: 1612-1112
    Keywords: Single short-column LC ; On-column sample enrichment ; Atmospheric pressure chemical ionization ; LC-tandem MS ; Environmental analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Single short, i.e. ca 2-cm long, high-pressure-packed columns coupled with mass spectrometric (MS) or tandem MS detection enable rapid trace-level determination and identification of environmental pollutants in water samples. In this study an atmospheric pressure chemical ionization (APCI) interface has been used and the overall set-up was tested with a mixture of seventeen pesticides, including organophosphates, carbamates, phenylureas and triazines. For the majority of the test analytes, the most prominent peaks in the positive-ion APCI-MS spectra resulted from protonated molecules. For fifteen out of the seventeen pesticides short-column liquid chromatography (LC)-APCI-MS of water samples as small as 15 mL resulted in detection limits between 0.03 and 5 μg L−1 in full-scan mode and between 2 and 750 ng L−1 by selected ion monitoring (SIM), both recorded in the positive-ion mode. Production spectra from protonated molecules of the majority of the selected pesticides present at a level of 0.1 μg L−1 in tap water are successfully identified from a search against a pesticide MS-MS library compiled in-house. This short-column LC-APCI-MS(-MS) approach has, on the basis of full-scan positive-ion data and their product-ion spectra, also been used to confirm the identity of target compounds and to identify unknown organic micropollutants in environmental waters.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Atmopheric Pressure Chemical Ionization (APCI) mass ; spectrometry ; Glucuronide-conjugates ; Toxicological compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new chromatographic method for the direct determination of metabolites (glucuronide-conjugates) of molecules of toxicological relevance in biological media with the minimum sample pre-treatment has been developed. A high performance liquid chromatographyatmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) system was used for this purpose. The separation of four glucuronides Aminophenylglucuronide (APhG), Phenylglucuronide (PhG),p-Nitrophenylglucuronide (NPhG) and α-Naphthylglucuronide (NG) was obtained under ion-suppressed reversed-phase chromatography conditions, by using high-speed (3 cm, 3 μm) columns and formic acid (2 mM) as the acid modifier in the mobile phase. Different C-18 stationary phases (partially endcapped and non-endcapped) were evaluated in order to obtain retention for these very polar, water soluble molecules. The ionization of the analytes was obtained in negativeion (NI) mode. Detection limits were in the range 1–5 mg L−1 and calibration curves were linear over two order of magnitude. Intra-day and inter-day precision were in the range 2.9–10.6% for all the compounds. The method was successfully applied for the determination of PhG in a urine sample of a European Quality Assurance Programme for Organic Solvent Metabolites.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Short-Column LC ; Environmental water samples ; MS-MS detection ; Pesticide degradation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The applicability of solid-phase extraction-LC using two short columns (SPE-LC) and/or single-short-column liquid chromatography (SSC) combined on-line with tandem mass spectrometry (MS) was demonstrated for the rapid study of pesticide degradation. A fast analytical procedure was developed to provide preliminary information concerning experimental conditions, approximate rates of degradation and identity of the degradation products. Surface water samples were spiked at relevant concentration levels with well-known microcontaminants and photolysis was used to transform parent compounds into their degradation products. In general, the strategy was as follows: at 30-min intervals 10-mL samples were on-line enriched, separated by short-column LC and recorded in full-scan MS to obtain information on the disappearance of the parent compound and the appearance of breakdown products. To obtain structural information, product-ion spectra of selected compounds appearing in the full-scan MS chromatogram were recorded; this enabled the identification of several degradation products. Total analysis time of enrichment/separation and detection was about 10–15 min.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 357-364 
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The application of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) for quantitative analysis was investigated with the use of internal standards. Three peptides/proteins in the mass range 1000-12000 were tested and the effect of various internal standards was evaluated. Horse cytochrome c was used as an internal standard for bovine cytochrome c, melittin for renin and an undecapeptide B analogue was employed as an internal standard for the decapeptide A. A linear response was found between the measured peak height ratio and the applied amount of analyte when an appropriate internal stanard was used. The quantitative abilities of MALDI-MS were finally applied to the determination of the drug amperozide in plasma. The biological samples were prepared for analysis using liquid-liquid extraction prior to MALDI-MS. A linear calibration graph was obtained using the 13C4 stable isotopically labelled amperozide as an internal standard.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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