RESUMO
Herein, the development of an ion-pair hollow fiber liquid-phase microextraction (IP-HF-LPME) procedure followed by capillary electrophoresis (CE) with indirect UV detection for the simultaneous extraction and determination of aliphatic biogenic amines including spermidine, spermine, and cadaverine in tissue samples of rat is described. In this study, tissue samples were firstly homogenized with a cold trichloroacetic acid solution then the developed method was applied to the supernatant resulting from tissue homogenization. Different CE separation and indirect UV detection conditions, as well as IP-HF-LPME extraction conditions were studied in detail and optimized. A 11 mmol L-1 imidazole solution containing 13 % (v/v) ethanol adjusted at pH 3.3 (by acetic acid) was the best running buffer for indirect UV detection of non-UV-absorbing amines. 1-Octanol in combination with salicylic acid, respectively as the membrane solvent and ion-pair reagent provided the highest extraction recovery for the studied amines. Method performances were established and good results of linearity, recovery, sensitivity, and repeatability were achieved for all the studied amines. Limits of detection were found to be between 2.8 and 4.5 ng mL-1 and limits of quantification were 15 ng mL-1 and the dynamic range was 15-2000 ng mL-1 for all three analytes.
