Recebido em 21/11/00; aceito em 8/8/01 SUPERCRITICAL FLUID EXTRACTION FOR SOME CARBAMATE INSECTICIDES IN POTATOES SAMPLES, WITH HPLC/ FLUORESCENCE DETERMINATION AND HPLC/MASS SPECTROMETRY CONFIRMATION. Six supercritical fluid extraction (SFE) methods were tested, by varying the following operational parameters: CO 2 pressure, time and temperature of extraction, type and proportion of static modifier, and Hydromatrix ® /sample rate into cell. Firstly, insecticide carbamates were extracted from spiked potatoes samples (fortification level of 0,5 mg.Kg -1 ) by using SPE procedures, and then final extracts were analyzed HPLC/fluorescence. Good performance was observed with SFE methods that operated with values of temperature and CO 2 pressure of 50 o C and 350 bar, respectively. Best efficiency was obtained when it was used acetonitrile as a modifier (3% on the cell volume), and Hydromatrix ® /sample rate of 2:1. Static time was of 1 min; total extraction time was of 35 min; dynamic extraction was performed with 15 mL of CO 2 , and it was used methanol (2 mL) for the dissolution of the final residue. In such conditions, pesticide recoveries varied from 72 to 94%, depending on the analyzed compound. In higher extraction temperatures, a rapid degradation was observed for some compounds, such as aldicarb and carbaryl; presence of their metabolites was further confirmed by HPLC-APCI/MS in positive mode. Detection limits for chromatographic analysis varied from 0,2 to 1,3 ng.