Determination of 11 pesticides residues in grass carp using ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry coupled with pass-through clean-up column

A method was established for determination of 11 pesticide residues in grass carp sample based on cheap analytical filtration syringe (CAFS) clean-up column coupled with ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry (UPLC-QTRAP-MS/MS). Using acetonitrile as extraction solvent, the sample was ultrasonic, frozen and centrifuged, and the supernatant was quickly purified once by CAFS clean-up column with 50 mg PSA. After separated by UPLC, the analytes were determined by QTRAP-MS/MS. Matrix-matched calibration curves and the external standard method was employed for quantification. The results showed that the linear relationships of the 11 pesticides were good within 1.0-50.0 μg/kg, and the correlation coefficients were greater than 0.99. The limit of quantification were 1.0-2.0 μg/kg. The recoveries of 11 pesticides at different spiking levels were 83%-119%, and the intra-day and inter-day relative standard deviations were 2.6%-20% and 0.7%-15%, respectively. The method is economical, simple, efficient, sensitive and reproducible, and could be used as a routine method for the detection of pesticide residues in grass carp.