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TITLE:  Determination and confirmation of nitrofuran residues in honey using LC-MS/MS
 
AUTHORS:  Lopez MI;Feldlaufer MF;Williams AD;Chu PS;
 
YEAR:  2007
 
JOURNAL ABBREV:  J Agric Food Chem
 
MONTH:  Feb
 
TYPE:  JOUR
 
REFMAN INDEX:  70
 
JOURNAL FULL:  Journal of agricultural and food chemistry
 
VOLUME:  55
 
ISSUE:  4
 
START PAGE:  1103
 
END PAGE:  1108
 
KEYWORDS:  analysis;Anti-Infective Agents;Calibration;Carcinogens;Chromatography,Liquid;Food;Food Contamination;Honey;Hydrolysis;Mass Spectrometry;Mutagens;Nitrofurans;Sensitivity and Specificity;Solid Phase Extraction;Spectrometry,Mass,Electrospray Ionization;standards;veterinary;Veterinary Medicine;
 
ABSTRACT:  A method was developed for the determination and confirmation of furazolidone, nitrofurazone, furaltadone, and nitrofurantoin as their side-chain residues 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 side-chain residues 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 method was validated at concentrations ranging from 0.5 to 2.0 ppb with accuracies of 92-103% and coefficients of variation of < or =10%. The lowest calibration standard used (0.25 ppb) was defined as the limit of quantitation for all four nitrofuran side-chain residues. The extracts and standards were also used for confirmatory purposes. Honey from dosed beehives was assayed to study the stability of the nitrofuran residues and to demonstrate the effectiveness of the method
 
AFFILIATIONS:  Center for Veterinary Medicine, U.S. Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, USA. mayda.lopez@fda.hhs.gov
 
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