title: Quantitative determination of four nitrofuran metabolites in meat by isotope dilution liquid chromatography-electrospray ionisation-tandem mass spectrometry.
abstract: A confirmatory method based on isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the low-level determination of residues of four nitrofuran veterinary drugs in meat, e.g., furazolidone, furaltadone, nitrofurantoin, and nitrofurazone. The procedure entails an acid-catalysed release of protein-bound metabolites, followed by their in situ conversion into the 2-nitrobenzaldehyde (NBA) imine-type derivatives. Liquid-liquid extraction and clean-up on a polymeric solid phase extraction cartridge are then performed before LC-MS/MS analysis by positive electrospray ionisation (ESI) applying multiple reaction monitoring of three transition reactions for each compound. Reliable quantitation is obtained by using one deuterated analogue per analyte (d4-NBA derivative) as internal standard (IS). Validation of the method in chicken meat was conducted following the European Union (EU) criteria for the analysis of veterinary drug residues in foods. The decision limits (CCalpha) were 0.11-0.21 microg/kg, and the detection capabilities (CCbeta) 0.19-0.36 microg/kg, thus below the minimum required performance limit (MRPL) set at 1 microg/kg by the EU. The method is robust and suitable for routine quality control operations, and more than 200 sample injections were performed without excessive pollution of the mass spectrometer or loss of LC column performance.
authors.affiliation: Department of Quality and Safety Assurance, Nestle Research Centre, Nestec Ltd, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland. pascal.mottier@rdls.nestle.com
authors.forename: Pascal
authors.initials: P
authors.lastname: Mottier
authors.forename: Seu-Ping
authors.initials: SP
authors.lastname: Khong
authors.forename: Eric
authors.initials: E
authors.lastname: Gremaud
authors.forename: Janique
authors.initials: J
authors.lastname: Richoz
authors.forename: Thierry
authors.initials: T
authors.lastname: Delatour
authors.forename: Till
authors.initials: T
authors.lastname: Goldmann
authors.forename: Philippe A
authors.initials: PA
authors.lastname: Guy
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D008461:Meat Products / Q000032:analysis*; D009581:Nitrofurans / Q000032:analysis*; D012015:Reference Standards; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D009581:Nitrofurans