[Determination of pesticide residues in fugu, eel and prawn using gas chromatography-mass spectrometry with gel permeation chromatographic clean-up].

A multiresidue analytical method was developed for the determination of 191 pesticides in fugu, eel and prawn using gas chromatography-mass spectrometry (GC-MS). The samples were extracted with ethyl acetate and cyclohexane (1:1, v/v), and cleaned-up by gel permeation chromatography (GPC). The GPC eluant collected from 26 min to 44 min was concentrated to 1 mL, then analyzed using GC-MS. A DB-1701 column was used for the separation. The MS detection was performed in selected ion monitoring mode. The recoveries were determined at the two spiked levels of I LOQ and 4 LOQ (LOQ: limit of quantification). The overall recoveries were from 50.2% to 120%, and in which the recoveries of 89.5% pesticides were from 70% to 120%. The relative standard deviations (RSDs) of the recoveries were from 0.6% to 21.6%. The calibration curves of all pesticides showed good linearities in the respective ranges with the correlation coefficient above 0.97. The limits of detection and the limits of quantification were 0.002-0.3 mg/kg and 0.007-1.2 mg/kg, respectively. The sensitivity and accuracy of the method met the requirements of the multiple pesticide residues. This method was applicable to determine 191 multiple pesticide residues in fugu, eel, prawn and other fishes.