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

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.