Title Solid phase extraction and fast gas chromatography for a residue analysis of sedative-hypnotic drugs in biological samples /
Translation of Title Raminamųjų-migdomųjų vaistų likučių kietafazė ekstrakcija iš biologinės kilmės bandinių ir nustatymas sparčiosios dujų chromatografijos metodu.
Authors Karlonas, Nerijus
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Pages 120
Keywords [eng] Solid phase extraction ; gas chromatography ; sedative-hypnotic drugs
Abstract [eng] A method for simultaneous determination of benzodiazepines in blood using fast gas chromatography with negative-ion chemical ionization mass spectrometry (GC/NICI-MS) was investigated. A mixed-mode Oasis MCX sorbent was used for solid phase extraction (SPE). This SPE method has been used for the first time for the optimization of sample preparation at pH 1.0. Different extraction solvents or mixtures of solvents of different compositions for elution of the adsorbed analytes, and washing steps for eliminating interferences in the sorbent were tested. An SPE-GC/NICI-MS method was fully validated for simultaneous determination of 15 benzodiazepines. The SPE method for determination of zaleplon and zopiclone in hemolyzed blood using fast GC/NICI-MS was investigated. The adsorption-related behaviour of zaleplon and zopiclone on the mixed-mode SPE Oasis MCX sorbent was dependent on the sample pH and due to different pKa values of both analytes. Both analytes were well retained on Oasis MCX and Oasis HLB sorbents, and sufficient extraction efficiency up to 82.7 % was achieved at sample pH 9.0. Fast GC/NICI-MS technique for the separation of 15 benzodiazepines, zaleplon and zopiclone are more selective and faster in comparison to the conventional techniques. New fully validated SPE-GC/NICI-MS methods can be used for extraction of complex biological samples, such as whole blood or hemolyzed blood.
Dissertation Institution Vilniaus universitetas.
Type Doctoral thesis
Language English
Publication date 2015