Dithiocarbamate (DTC) is one of the oldest and worldwide used classes of organic fungicides. DTC has been used to control fungal diseases on a large variety of crops, along with or without other modern fungicides. The toxicological importance of DTC is related to their metabolites: CS2 and ETU. However, DTC is one of the most difficult pesticides to be determined, because they are not amenable to multi-residue extraction with other pesticides classes. Thus, this work reports two methods suitable for DTC metabolites determination in polished rice – one of the most consumed food worldwide. For the method validation studies, linearity of the analytical curves, limit of detection (LOD), limit of quantification (LOQ), matrix effect (%), trueness (as recovery%) and precision (RSD%) were assessed via recovery experiments. Blank polished rice samples were spiked with thiram at equivalent CS2 concentrations of 50, 100 and 500 µg kg-1 for determination by GC-PFPD and GC-ITD-MS. Considering the maximum residue limit (MRL) for DTC in Brazil (0.8 mg CS2 kg-1), the accuracy (trueness and precision) and method LOQ (50 µg CS2 kg-1) are very satisfactory to determine DTC residues in rice. To ETU determination by LC-MS/MS, spiking concentrations were 5, 10, 20 and 50 µg kg-1. The method performed remarkably well under optimal conditions based on LOQ (5 µg kg-1), recovery (78.1-90.9%), repeatability ≤18.5% and intermediate precision ≤15.4%. The methods presented reliable results for real samples analysis. In total, 48 samples were analyzed, neither CS2 nor ETU was detected.