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Leis, HJ; Windischhofer, W.
Gas chromatography-negative ion chemical ionisation mass spectrometry using o-(pentafluorobenzyloxycarbonyl)-2,3,4,5-tetrafluorobenzoyl derivatives for the quantitative determination of methylphenidate in human plasma.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011; 879(23): 2299-2303.
Doi: 10.1016/j.jchromb.2011.06.017
Web of Science
PubMed
FullText
FullText_MUG
- Führende Autor*innen der Med Uni Graz
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Leis Hans-Joerg
- Co-Autor*innen der Med Uni Graz
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Windischhofer Werner
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- Abstract:
- A novel electrophoric derivatisation procedure using o-(pentafluorobenzyloxycarbonyl)-2,3,4,5-tetrafluorobenzoyl chloride for the quantitative determination of methylphenidate in human plasma is described. The drug can be quantitatively measured down to 0.006 pg/mL plasma due to the extraordinary sensitivity of the derivatives under negative ion chemical ionisation mass spectrometry. Plasma samples were made alkaline with carbonate buffer and treated with extraction solvent (n-hexane) and reagent solution for 15 min, which, after concentration was measured by GC-NICI-MS. The method is rapid as extraction and derivatisation occur in one single step. A stable isotope labelled internal standard was used. Validation data are given to demonstrate the usefulness of the assay, including selectivity, linearity, accuracy and precision, autosampler stability, aliquot analysis, robustness, and prospective analytical batch size accuracy. The method has been successfully applied to pharmacokinetic profiling of the drug after oral administration.
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Chromatography, Gas - instrumentation
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Humans -
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Mass Spectrometry - instrumentation
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Methylphenidate - blood
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Phthalic Acids - analysis
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NICI
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Methylphenidate
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PBTFBCI
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Derivatisation