This study was aimed at evaluating the effi cacy of different mineral separation procedures to validate the EN1788 (2001) European Union standard protocol for better identifi cation of irradiated fi sh and shellfi sh. The silicate minerals were isolated with physical density separation method from two types of non-irradiated freeze-dried fi sh and shellfi sh that included Pacifi c saury (Cololabis saira), mackerel (Scomber japonicus), shrimp (Penaeidae metapenaeus), and mussel (Mytilus coruscus). Radiation-specifi c thermoluminescence (TL) peaks (glow curve 1) were observed between 150-250 °C. The peaks are typical for the irradiated food; despite the samples being not irradiated. Apparently it showed that the isolated minerals were contaminated with organic materials such as bone, etc. Acid-hydrolysis digestion was employed to remove the possible contaminants. The minerals obtained through alternative pre-treatment showed no TL curves in radiation specifi c temperature range. Moreover, acid hydrolysis extraction resulted in producing higher mineral yields and lower background luminescence. Results were also confi rmed by calculating TL ratios (glow curve 1/glow curve 2) to confi rm the irradiation history of samples. Furthermore, different time and temperature treatments on TL intensity of irradiated standard quartz (SiO 2 ) minerals showed that the acid-hydrolysis can be adjusted to 50 °C and 3 h for better luminescence determinations.