Determination of Chloramphenicol and Nitrofuran Metabolites in Cobia, Croaker, and Shrimp Using Microwave-Assisted Derivatization, Automated SPE, and LC-MS/MS–Results from a U.S. Food and Drug Administration Level Three Inter-Laboratory Study

Abstract

Abstract Background An interlaboratory study was conducted to test a published, peer-reviewed manuscript in the Journal of AOAC INTERNATIONAL Vol 98, No. 3, 2015, “Quantitation of Chloramphenicol and Nitrofuran Metabolites in Aquaculture Products Using Microwave-Assisted Derivatization, Automated Solid-Phase Extraction, and LC-MS/MS.” Objective The purpose of this study was to demonstrate the performance of the method in shrimp, cobia, and croaker matrices. Method Three U.S. Food and Drug Administration laboratories participated in the collaborative study. The laboratories tested matrix blanks and laboratory-fortified matrix blanks at various levels in three separate matrices. The method evaluation included determination of the LOQ, accuracy, and precision. Results The reproducibility and repeatability of the RSD, % levels for matrix spikes fortified below the action level were < 10% for all residues in shrimp, < 13% for all residues in cobia except for 3-amino-2-oxazolidinone which was ≤ 22%, and < 16% for croaker. The RSD, % levels for all other spikes in the study were < 14%. Average percent recoveries for all matrices ranged from 81.6% – 102%. Conclusions The study demonstrated that the method is acceptable for use for the combined determination of chloramphenicol and nitrofuran metabolites in the study matrices. Highlights The study showed acceptable quantitation for the high-throughput chloramphenicol and nitrofuran metabolites method.