Development and Validation of a Liquid Chromatography-UV Detection Method for the Determination of Sulfonamides in Fish Muscle and Shrimp According to European Union Decision 2002/657/EC

作者:Granja Rodrigo H M M*; de Lima Andreia C; Salerno Alessandro G; Wanschel Amarylis C B A
来源:Journal of AOAC International, 2013, 96(1): 212-215.
DOI:10.5740/jaoacint.11-541

摘要

Sulfonamides are one class of antimicrobial agents used in aquaculture production. Sulfonamides are often overused because they are inexpensive and readily available. Their presence at a concentration above the legal limits is a potential hazard to human health. Brazilian authorities have included in the National Regulatory Monitoring Program the control of the three most widely used sulfonamides in aquaculture production, i.e., sulfathiazole, sulfamethazine, and sulfadimethoxine. An LC method with UV detection for the determination of residual sulfonamides in fish muscle, using sulfapyridine as an internal standard has been developed and validated. The validation was performed according to the Brazilian Regulation 2412009 (equivalent to European Union Decision 2002/657/EC). The method meets the Brazilian regulatory requirement that establishes criteria and procedures for determination of parameters such as decision limit (CC alpha), detection capability (CC beta), precision, and recovery. For fish muscle, CC alpha was determined at 3.63, 2.91, and 7.46 mu g/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. CC beta was 9.39, 14.54, and 9.39 mu g/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. For shrimp, CC alpha was 11.5, 8.67, and 4.46 mu g/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. CC beta was 18, 11.93, and 5.24 mu g/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. A complete statistical analysis was performed on the results obtained. The results indicate that the method is robust when subjected to day-to-day analytical variations.

  • 出版日期2013-2