Determination of an irreversible inhibitor of monoamine oxidase B (MDL 72974A) in human plasma and urine by gas chromatography—positive-ion chemical ionization mass spectrometry
| Autor: | Bertrand Dulery, Josiane Schoun, K.D. Haegele |
|---|---|
| Rok vydání: | 1991 |
| Předmět: |
Detection limit
Chemical ionization Monoamine Oxidase Inhibitors Chromatography Chemistry Allyl compound Reproducibility of Results General Chemistry Butylamines Mass spectrometry Gas Chromatography-Mass Spectrometry Allyl Compounds Column chromatography Reagent Humans Gas chromatography Gas chromatography–mass spectrometry |
| Zdroj: | Journal of Chromatography B: Biomedical Sciences and Applications. 571:241-249 |
| ISSN: | 0378-4347 |
| DOI: | 10.1016/0378-4347(91)80451-h |
| Popis: | A sensitive and specific assay has been developed for the quantitative measurement in human plasma and urine of the irreversible inhibitor of monoamine oxidase B [(E)-4-fluoro-beta-fluoromethylenebenzene-butanamine HCl salt] (MDL 72974A) (I). This assay is based on gas chromatography-mass spectrometry with ammonia as the chemical ionization reagent gas. After addition of 1-fluoro-2-(4-chlorobenzene)-ethanamine HCl salt (MDL 71946A) as the internal standard, plasma (1 ml) and urine (100 microliter) samples were extracted using an automated solid-liquid extraction procedure on CN columns. The eluent was dried with a stream of nitrogen, and the residue was derivatized with pentafluoropropionic anhydride. Selected-ion monitoring of the [MNH4]+ ions m/z 361 (I) and 351 (internal standard) was used for quantification. The method yielded a linear response over the concentration range 0.25-100 pmol/ml in plasma with a limit of quantitation of 0.25 pmol/ml. The within-day reproducibility at a concentration of 5 pmol/ml was 4.6% and at a concentration of 50 pmol/ml was 1.3%. The day-to-day reproducibility was 5.2 and 7.0% at concentrations of 10 and 30 pmol/ml, respectively. The method was applied to the quantification of I in plasma and urine after the administration of 12-mg doses of I to a healthy male volunteer. |
| Databáze: | OpenAIRE |
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