Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 57, Issue 5, Pages 1752-1759Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jf803423r
Keywords
Protein-bound metabolites of nitrofurans; HPLC; DAD; shrimp; APCI-MS/MS
Funding
- Center for Innovation in Chemistry (PERCH: CIC),
- Commission on Higher Education
- Ministry of Education
- Kasetsart University Research and Development Institute (KURDI)
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The synthesis of derivatives of metabolites from furazolidone, furaltadone, nitrofurazone, and nitrofurantoin using a new derivatizing reagent, 2-naphthaldehyde (NTA), is described. The reaction product was used in liquid chromatography with diode array detector (LC-DAD) for determination of protein-bound metabolites of nitrofurans in shrimp followed by two steps of liquid-liquid extraction. Derivatives of nitrofuran metabolites are well separated from NTA remaining in the extract upon separation on a ChromSpher 5 Pesticide (250 x 4.6 mm, 5 mu m) column at 40 degrees C with acetonitrile/5 mM ammonium acetate adjusted to pH 7.5 gradient as the mobile phase and DAD detection at 308 nm except for naphthyl derivative of 1-aminohydantoin at 310 nm. The high absorptivity of these derivatives makes simultaneous screening of these metabolites in shrimp at 1 mu g/kg possible for the first time using LC-DAD. The method was validated using blank shrimp fortified with all four metabolites at 1, 1.5, and 2 mu g/kg. Recoveries were > 86% with relative standard deviations of < 14% for all four metabolites. Comparison between LC-DAD and APCI-MS/MS shows very good agreement for shrimp samples.
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