“…As for as solid-phase extraction method (Salvador et al, 2006) is concerned, Ura and 5FU were reportedly coeluted with other endogenous substances of plasma. Whereas HPLC/ UV (Maring et al, 2005;Deporte et al, 2006), HPLC/fluorescence (Yoshida et al, 1986;Kindberg et al, 1989), GC/MS (Shin et al, 1998;Mashiyama et al, 2008) and voltammetric methods (Mirceski et al, 2000;Liu et al, 2007) showed impressive Ura and 5FU sensitivity, integration with advanced technology such as LC/MS (Jiang et al, 2002;Salvador et al, 2006) required costly and sophisticated instrumentation. To the best of our knowledge, no work related to direct SPME for Ura and 5FU analysis in biological fluids has hitherto been reported barring a few SPME analyses of substituted Ura herbicides (Beltran et al, 2000;Krutz et al, 2003).…”