Chlortetracycline, Oxytetracycline, and Tetracycline in Edible Animal Tissues, Liquid Chromatographic Method: Collaborative Study

Thirteen laboratories analyzed samples of edible animal tissues for tetracycline residues. The method included extraction of analytes into buffer, elution from a C18 solid-phase extraction (SPE) cartridge, and reversed-phase liquid chromatographic (LC) analysis, including use of a confirmation column. An additional laboratory, using an alternative LC assay based on a different sample cleanup, also analyzed the samples. Results showed the 2 methods are comparable. The LC method for determination of cholortetracycline, oxytetracycline, and tetracycline in edible animal tissues has been adopted by AOAC INTERNATIONAL. Results from 13 laboratories indicate that the method under study provides generally better results at the higher concentrations tested than at concentrations near the detection limit and that there is less problem with interferences in muscle tissue than in kidney. The method can achieve reliable results for analytes and matrixes studied at concentrations from 0.1 to 0.6 ppm and above, depending on the analyte-matrix combination, with generally better performance to be expected with muscle than with kidney. The poorer performance for fortified samples, particularly kidney, was attributed to additional homogenization steps required to prepare these samples. Recovery of analytes from different lots of solid-phase extraction (SPE) cartridges was an important variable.