New method of liquid/liquid/liquid hollow fibre based microextraction of vanillylmandelic acid coupled with voltammetric determination is being developed. Selected liquid membranes based on alcohols, aliphatic hydrocarbons and esters were tested.
Highest enrichment factor of 2.52 after 30 minutes of extraction was obtained using propyl benzoate, RSD = 18.2 % (n=5). Mechanically and cathodically pretreated (-1000 mV vs.
Ag/AgCl/3M KCl, 15 s) boron doped diamond electrode in a miniaturized arrangement was used for DPV determination. LOD = 1.2 μmol/l, RSD = 5.9% (n=10) for a 10 μl extract.