Determination of delorazepam in urine by solid-phase microextraction coupled to high performance liquid chromatography.
An SPME-HPLC-UV method for the determination of delorazepam, a representative benzodiazepine, in spiked human urine samples was developed for the first time. The performances of two commercially available fibers, a carbowax/templated resin (Carbowax/TPR-100) and a polydimethylsiloxane/divinylbenzene (PDMS/DVB), were compared, indicating the latter as the most suitable for urine samples analysis. All the aspects influencing adsorption (extraction time, pH, temperature, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analyte on the fiber have been investigated. In particular, short extraction times were necessary to reach the equilibrium and very short desorption times were employed. The procedure required simple sample pre-treatment and was able to detect 5 ng/ml in spiked urine, regardless of the complexity of the matrix.
Aresta
Antonella
A
Università degli Studi di Bari, Dipartimento di Chimica, Via E. Orabona, 4, 70100, Bari, Italy.
Monaci
Linda
L
Zambonin
Carlo Giorgio
CG
D014151:Anti-Anxiety Agents / Q000652:urine*; D001569:Benzodiazepines; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D006863:Hydrogen-Ion Concentration; D003708:Nordazepam / Q000031:analogs & derivatives / Q000652:urine*; D012997:Solvents; D013056:Spectrophotometry, Ultraviolet; D013696:Temperature
D014151:Anti-Anxiety Agents; D012997:Solvents; D001569:Benzodiazepines; D003708:Nordazepam; C013434:chlordesmethyldiazepam