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Analysis of Matrix-Bound Nitrofuran Residues in Worldwide-Originated Honeys by Isotope Dilution High-Performance Liquid Chromatography-Tandem Mass Spectrometry
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文摘
A sensitive and selective isotope dilution liquid chromatography-electrospray ionization tandem massspectrometry (LC-ESIMS/MS) method is presented for the simultaneous analysis of the metabolitesof four nitrofuran veterinary drugs, that is, furazolidone, furaltadone, nitrofurantoin, and nitrofurazone,in honey samples. The method entails a combined hydrolysis of protein-bound drug metabolites andderivatization of the resulting metabolites with 2-nitrobenzaldehyde (NBA) during an overnightincubation, followed by a liquid-liquid extraction and a cleanup on a polymeric solid-phase extractioncartridge. Mass spectral acquisition is carried out in the positive ion mode by applying multiple reactionmonitoring (MRM) of three diagnostic transition reactions for each analyte under survey. A reliablequantification is obtained by the use of one deuterated analogue per analyte (NBA-d4 derivative).The method has been validated in honey according to the European Union criteria for the analysisof veterinary drug residues in food. Expressed in underivatized nitrofuran metabolite concentrations,the decision limits (CC) ranged within 0.07-0.46 g/kg, and the detection capabilities (CC) werewithin 0.12-0.56 g/kg. The method has been successfully applied in a survey of honeys of variousgeographical origins, showing that furazolidone is the main nitrofuran antibiotic administered to treatbacterial diseases of bees.Keywords: Nitrofuran metabolites; honey; mass spectrometry; 1-aminohydantoin (AH); 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ); 3-amino-2-oxazolidinone (AOZ); semicarbazide (SC); furazolidone; furaltadone; nitrofurantoin; nitrofurazone; veterinary drugs

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