Liquid Chromatography−Tandem Mass Spectrometry for the Determination of Protein-Bound Residues in Shrimp Dosed with Nitrofurans

• Published in: Journal of agricultural and food chemistry 2005-11, Vol.53 (23), p.8934-8939
• Main Authors: Chu, Pak-Sin, Lopez, Mayda I
• Format: Article
• Language: English
• Subjects: animal proteins; Animals; binding capacity; Biological and medical sciences; Chromatography, Liquid - methods; drug residues; Drug Residues - analysis; Fish and seafood industries; food analysis; food contamination; Food industries; fualtadone; Fundamental and applied biological sciences. Psychology; furazolidone; liquid chromatography; Litopenaeus vannamei; mass spectrometry; Mass Spectrometry - methods; nitrofurans; Nitrofurans - administration & dosage; Nitrofurans - analysis; Nitrofurans - metabolism; nitrofurantoin; nitrofurazone; Penaeidae - chemistry; Proteins - metabolism; seafoods; shrimp
• ISSN: 0021-8561; 1520-5118
• DOI: 10.1021/jf051615o

An analytical method was developed for the determination of bound residues of the nitrofuran drugs furazolidone, nitrofurazone, furaltadone, and nitrofurantoin with a sensitivity of 1 ppb in shrimp. In this procedure, shrimp tissue is prewashed with solvents followed by overnight acid hydrolysis, during which the side chains of the bound residues are released and simultaneously derivatized with 2-nitrobenzaldehyde. After liquid−liquid extraction cleanup, the derivatives are detected and quantitated using liquid chromatography−mass spectrometry/mass spectrometry (LC-MS/MS) with an atmospheric pressure chemical ionization interface. The method was validated using control shrimp fortified with each side-chain analyte at 1, 2, and 4 ppb. Method accuracies were >80% with coefficients of variation of