Determination of Nitrofuran Metabolites in Aquatic Products by HPLC-MS/MS

In this paper,a method of HPLC-MS-MS for the determination of nitrofuran metabolites in aquatic products was proposed.The sample was hydrolyzed with dilute hydrochloric acid then derivatized with 2-nitrobenzene formaldehyde (2-NBA).The derivatized solution was adjusted to pH 7.0-7.5 then separated by centrifugation.The supernatant was introduced into the Oasis HLB microcolumn (6 mL) and eluted with ethyl acetate.The eluate was dried in a nitrogen flow at 40 ℃,and dissolved with a mixture of acetonitrile and acetic acid (1+99) which were mixed in the ratio of 3 to 7 by volume.The metabolites were determined by HPLC-MS/MS using deuterium reagent as internal standard.Linearity of the calibration curves was in the range within 4.5 μg·L-1.Determination limit (10S/N) of the method was 0.25 μg·kg-1.Recovery was ranged from 80.2% to 98.4%,and RSD′s (n=8) from 3.75% to 8.12%.