Mycotoxin citrinin (CIT) and ochratoxin A (OTA) were simultaneously identified using immunoaffinity column-high performance liquid chromatography with fluorescence detection (IAC-HPLC-FD) (Ex.333 nm; Em:495 nm) after an optimized extraction procedure. Both mycotoxins were eluted on a C(18) RP support (250 x 4.6 mm I.D., ODS2, 5 mu m particles) using an isocratic eluent consisting of acetonitrile/water/formic acid (60/38/2, v/v/v), acidified to pH 2.5 and pumped at a flow rate of 1.0 mL min(-1). The four categories of citrinin levels [0-0.55; 1.56-2.0; 0.66-2.64; 5.76-14.55 mu g kg(-1) of CIT] and three categories of ochratoxin levels [0 - < 0.1; 0.1-0.25; 0.30- 0.46 mu g kg(-1) of OTA] were found in 88 groups of olive samples. Recovery studies [y= 21416x - 7919.4 (R(2)=0.9998) for citrinin and y= 0.0001x + 0.0074 (R(2)=0.9999) for ochratoxin A] were performed and the mean analytical recoveries detected in CIT and OTA in table olives ranged from 92.65 - 96.83% and 88.92 - 95.58%, respectively. Limit of detection (LOD) was equivalent to 0.05 mu g/kg for both CIT and OTA. With the proposed method, CIT and OTA were both quickly determined in table olives and could be used to detect of mycotoxinic risks in a HACCP quality system of olive and olive-based food products.