In this paper, a combined hollow fiber-based liquid three-phase microextraction and voltammetric method are applied for the first time as a highly selective and sensitive method of electrochemical analysis. Desipramine, used as a model compound was extracted from 8 mL aqueous solution (donor phase, 0.10 mol L(-1) NaOH) through a thin phase of propyl benzoate inside the pores of a polypropylene hollow fiber and finally into a 10 microL acidic acceptor solution inside the hollow fiber. Three microelectrodes designed and constructed for the purposes of this study were placed into the two ends of the hollow fiber inside the acceptor solution, and voltammetric analysis was performed in-situ during the extraction. After 15 min, the final stable signal was used for analytical applications. Under the optimized conditions, an enrichment factor of 301 was achieved and the relative standard deviation (R.S.D.) of the method was 6.2% (n=5). The calibration curve was obtained in the range of 5-5000 nmol L(-1) with a reasonable linearity (R(2)>0.988) and the limit of detection (LOD) was found to be 0.8 nmol L(-1). Finally, the applicability of the proposed method was evaluated by extraction and determination of desipramine in plasma and urine samples without any dilutions.
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