Title: DETERMINATION AND CONFIRMATION OF NITROFURAN RESIDUES IN HONEY USING LC-MS/MS.
Lopez, Mayda - FDA - CNT FOR VET MED.
Feldlaufer, Mark - USDA-ARS-PSI-CAIBL
Williams, Anthony - FDA - OFC. REG. AFFAIRS
Chu, Pak-Sin - FDA - CNT FOR VET MED.
Submitted to: Journal of Agricultural and Food Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: December 11, 2006
Publication Date: N/A
Interpretive Summary: There is a need to develop analysis methods to insure imported foods do not contain harmful substances. A method was developed by government scientists to detect certain antibiotics (“nitrofurans”) in honey. The method developed complies with the performance criteria established by the U. S. Food & Drug Administration’s Center for Veterinary Medicine for the analysis of veterinary drug residues in animal products. This method of analysis, therefore, can be used for U. S. regulatory purposes and by scientists interested in monitoring the presence of nitrofurans in honey.
A method was developed for the determination and confirmation of furazolidone, nitrofurazone, furaltadone, and nitrofurantoin residues as their metabolites in honey using liquid chromatography tandem mass spectrometry (LC-MS/MS). An initial solid-phase-extraction cleanup of the honey samples was followed by overnight hydrolysis and derivatization of the nitrofuran metabolites with 2 nitrobenzaldehyde. After pH adjustment and liquid-liquid extraction, the extracts were assayed by LC-MS/MS using electrospray ionization in the positive ion mode. The determinative method was validated at concentrations ranging from 0.5 to 2.0 ppb with accuracies between 92–103 and CVs of ' 10%. The lowest calibration standard used (0.25 ppb) was defined as the limit of quantitation (LOQ) for all four nitrofuran metabolites. Samples and standards prepared for the determinative method were also used for the confirmatory method. Honey from dosed beehives was assayed to study the stability of the nitrofuran residues and to demonstrate the effectiveness of the method.