New reagent for trace determination of protein-bound metabolites of nitrofurans in shrimp using liquid chromatography with diode array detector.
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 microm) 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 microg/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 microg/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.
Chumanee
Saowapa
S
Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Kasetsart University, Bangkok 10903, Thailand.
Sutthivaiyakit
Somyote
S
Sutthivaiyakit
Pakawadee
P
D000818:Animals; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D033364:Decapoda / Q000737:chemistry* / Q000378:metabolism; D009581:Nitrofurans / Q000032:analysis* / Q000378:metabolism*; D011485:Protein Binding; D011506:Proteins / Q000378:metabolism*
D009581:Nitrofurans; D011506:Proteins