| Summary: | In this study, polydimethylsiloxane (PDMS)-coated capillary columns (TRB-5 and TRB-35), both unmodified and functionalized with single-wall carbon nanotubes (SWCNTs) or multiwall carbon nanotubes (MWCNTs), have been tested and compared for the extraction of amphetamine (AMP), methamphetamine (MET) and ephedrine (EPE) by in-tube solid-phase microextraction (IT-SPME). Prior to their extraction, the analytes were derivatized with the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC). For separation and detection capillary chromatography with fluorimetric detection has been used. The presence of carbon nanotubes in the extractive coatings enhanced the extraction efficiencies and also significantly improved the chromatographic profiles, thus resulting in a reliable option for the analysis of these drugs. As an example of application, a new method is proposed for the analysis of the tested amphetamines in oral fluid using a TRB-35 capillary column functionalized with MWCNTs. The proposed conditions provided suitable selectivity and reproducibility (CV ≤ 6%, n = 3) at low µg/mL levels, and limits of detection of 0.5–0.8 µg/mL.
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