Determination of nitrofuran metabolites in seafood by ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry

A new analytical method has been developed for, the simultaneous determination of 4 nitrofuran metabolites in seafood by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS). The extraction procedure was based on a simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA), followed by a solid-phase extraction (SPE). Recovery was studied by spiking blank samples at two concentration levels (I and 10 mu g/kg) and recoveries ranged from 73 to 100% and 79 to 103%, respectively. Precision values, expressed as relative standard deviation (RSD) were <= 19% and <= 23% for intra-day and inter-day precision, respectively. Linearity was studied in the range 1-50 mu g/kg and the obtained determination coefficients (R-2) were >= 0.9900 for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were 0.5-0.8 mu g/kg and limits of quantification (LOQs) were established at 1 mu g/kg, whereas decision limit (CC alpha) and detection capability (CC) ranged from 1.5 to 2.6 mu g/kg and 1.6 to 3.1 mu g/kg, respectively. Finally, the method was applied to real food samples, but nitrofurans were not found. (C) 2013 Elsevier Inc. All rights reserved.