Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 30, Issue 12, Pages 2114-2122Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2013.849387
Keywords
metabolites of nitrofurans; HPLC-FLD; LC-MS/MS; pork muscle
Funding
- National Natural Science Foundation of China [20971024]
- International Sea Area Resources Survey and development of the 12th Five-Year Plan of China [DY125-15-E-01]
- Natural Science Foundation of Anhui Provincial University [KJ2009A127]
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A simple and sensitive HPLC method with fluorescence detection (HPLC-FLD) is reported for the simultaneous determination of metabolites of four nitrofuran drugs (furazolidone, furaltadone, nitrofurantoin and nitrofurazone) in pork muscle. The method involves acid hydrolysis of the protein-bound drug metabolites and the conjugation of the released side-chains with a novel fluorescence agent 2-hydroxy-1-naphthaldehyde. After liquid-liquid extraction and effective separation of the derivatives on a YMC-Pack Polymer C18 column at 40 degrees C under alkaline conditions, the high fluorescence intensity of these derivatives at emission wavelength (em)=463nm enables their simultaneous determination in pork muscle at concentrations as low as 1 mu gkg(-1). The method was validated using blank pork muscle fortified with all four metabolites at 0.5, 1.0 and 2.0 mu gkg(-1). Recoveries were >92.3% with RSDs <8.5% for all four metabolites. The results obtained with HPLC-FLD and LC-MS/MS methods showed very good agreement for pork muscle samples.
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