title: Determination of total nitrofuran metabolites in shrimp muscle using liquid chromatography/tandem mass spectrometry in the atmospheric pressure chemical ionization mode.
abstract: The method of MacMahon and Lohne for analysis of nitrofuran metabolites in shrimp was optimized to streamline the extraction processes and the LC analysis. This revised method includes 16 h of mild acid hydrolysis/derivatization followed by ethyl acetate extraction and analysis by LC/MS/MS in the atmospheric pressure chemical ionization mode. This revised method was validated in shrimp for concentrations of 0.25 to 2.0 ng/g. The LOQ was 0.25 ng/g for all metabolites. The LOD was 0.052 nglg for 1-aminohydantoin (AHD), 0.206 ng/g for 3-amino-2-oxazolidinone (AOZ), 0.108 ng/g for semicarbazide (SC), and 0.062 ng/g for 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ). The spike recoveries with RSD into negative matrix at 1 ng/g were 100.2% (3.2%) for AHD, 102.5% (1.0%) for AOZ, 103.7% (2.3%) for SC, and 104.0% (3.3%) for AMOZ. The spike recoveries at 1 ng/g into unknown samples (n=108) containing varied levels of nitrofuran metabolites were 112.6% (25.7%) for AHD, 108.1% (12.1%) for AOZ, 103.0% (12.0%) for SC, and 100.3% (6.9%) for AMOZ. Interday precision with samples containing incurred AOZ concentrations of 0.92 to 17.8 ppb performed over a year was 10.4% RSD. The method is accurate and precise for determining nitrofuran concentrations in the edible tissue of shrimp.
authors.affiliation: U.S. Food and Drug Administration, Pacific Regional Laboratory-Southwest, Irvine, CA 92612, USA. Haejung.An@fda.hhs.gov
authors.forename: Haejung
authors.initials: H
authors.lastname: An
authors.forename: Mark
authors.initials: M
authors.lastname: Henry
authors.forename: Teresa
authors.initials: T
authors.lastname: Cain
authors.forename: Bichsa
authors.initials: B
authors.lastname: Tran
authors.forename: Han Chol
authors.initials: HC
authors.lastname: Paek
authors.forename: Dennis
authors.initials: D
authors.lastname: Farley
mesh_terms: D000818:Animals; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D006827:Hydantoins / Q000032:analysis; D006868:Hydrolysis; D007477:Ions; D009025:Morpholines / Q000032:analysis; D009132:Muscles / Q000378:metabolism*; D009581:Nitrofurans / Q000032:analysis*; D023303:Oxazolidinones / Q000032:analysis; D033561:Penaeidae; D011312:Pressure; D015203:Reproducibility of Results; D012663:Semicarbazides / Q000032:analysis; D012758:Shellfish / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: C504350:1-aminohydantoin; C504349:3-amino-5-morpholinomethyl-2-oxazolidinone; D006827:Hydantoins; D007477:Ions; D009025:Morpholines; D009581:Nitrofurans; D023303:Oxazolidinones; D012663:Semicarbazides; C010059:carbamylhydrazine; C000209:3-amino-2-oxazolidinone