Problems of Forensic Sciences 2007 Vol. 70 (LXX) 187-197
APPLICATION OF MICROWAVE-ASSISTED EXTRACTION IN ISOLATION OF PSYCHOTROPIC DRUGS FROM BIOLOGICAL MATERIAL
Renata WIETECHA-POSŁUSZNY1, Michał WOŹNIAKIEWICZ1, Aneta GARBACIK1, Paweł KOŚCIELNIAK1,2
1Faculty of Chemistry, Jagiellonian University, Krakow, Poland
2Institute of Forensic Research, Krakow, Poland
Streszczenie
The aim of the presented research was to work out a complete analytical procedure for the determination of selected tricyclic antidepressant drugs (TCAD) in blood, encompassing the liquid-liquid extraction supported by the microwave-assisted extraction (MAE), and evaluation of the validation parameters of the method of determination of these drugs by high performance liquid chromatography. The research covered optimisation of conditions of extraction of the analysed compounds – amitryptyline, imipramine, doxepine, nortryptyline, desipramine, nordoxepine, clomipramine (IS) – from aqueous solutions by classical liquid-liquid extraction (LLE), supported by microwaves. Apparatus conditions of the microwave process were also optimised. The HPLC-DAD technique was used in the evaluation of the efficiency of the extraction process. On the basis of these results, an extraction procedure was developed, encompassing application of a mixture of hexane and isoamyl alcohol (99:1, v/v) as an extraction solvent and performance of microwave extraction at 60°C for 3 minutes. The procedure was applied in the extraction of selected psychotropic drugs in blood. The complete method of TCAD drugs determination in blood was validated and validation parameters for each compound were determined: detection limit (0.03–0.09 μg/ml), quantification limit (0.11–0.22 μg/ml), repeatability for two different concentrations (0.2 μg/ml: 4.28–18.05 RSD%; 0.8 μg/ml: 2.43–10.18 RSD%) and linearity (0.15–2.00 μg/ml). It was found that liquid-liquid extraction supported by microwaves allows a higher extraction efficiency (80–100%) to be obtained than classical liquid-liquid extraction (60–70%), and that all drugs are extracted at the same level.
Słowa kluczowe
Liquid-liquid extraction (LLE); Microwave-assisted extraction (MAE); Psychotropic drugs; Biological material.