期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1327, 期 -, 页码 90-96出版社
ELSEVIER
DOI: 10.1016/j.chroma.2013.12.065
关键词
Nitrofuran metabolites; HPLC-FLD; LC-MS/MS; Shrimp
资金
- 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 [KJ2009Al27]
A high performance liquid chromatography with fluorescence detection (HPLC-FLD) method for the simultaneous determination of total nitrofuran metabolite residues (furazolidone, furaltadone, nitrofurantoin, and nitrofurazone) in shrimp was developed. The method involves the acid hydrolysis of protein-bound metabolites, followed by the derivatization of the freed metabolites with the new fluorescent derivatization reagent 2-hydroxy-1-naphthaldehyde (HN) and subsequent liquid-liquid extraction (LLE). Separation is achieved on a YMC-Pack Polymer C18 column under alkaline conditions, and the high fluorescence intensity of the derivatives at an emission wavelength E-m= 463 nm (E-x =395 nm) enables, for the first time, their simultaneous determination in shrimp at concentrations as low, as 1 mu g/kg by HPLC-FLD. The method was validated using blank shrimp fortified with all four metabolites at 0.5, 1.0 and 2.0 mu g/kg. Recoveries were >87% with relative standard deviations of <8.1% for all four metabolites. Furthermore, the results obtained by HPLC-FLD were in very good agreement with those obtained by LC-MS/MS analysis. (C) 2014 Elsevier B.V. All rights reserved.
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