Validation of a high-performance liquid chromatographic method with fluorescence detection for the simultaneous determination of tetracyclines residues in bovine milk.
A high-performance liquid chromatography-fluorescence detection method was optimized and validated to determine tetracyclines residues in bovine milk. Post-column derivatization using metal complexation in non-aqueous reagent increased the fluorescence of chelates by a factor up to 2.54 compared to water (signal-to-noise ratio enhancement). Overall recoveries ranged from 61 to 115%, with RSD(r) from 5 to 15% (n=54). Detection limits ranged from 5 to 35 microg kg(-1). Limits of quantification were established at 50 microg kg(-1). Decision limits (CCalpha) were 109, 108 and 124 microg kg(-1) and detection capabilities (CCbeta) 119, 117 and 161 microg kg(-1) for oxytetracycline, tetracycline and chlortetracycline, respectively. The method was applied successfully in a national monitoring program.
Spisso
Bernardete Ferraz
BF
National Institute for Quality Control in Health, Oswaldo Cruz Foundation, Av. Brasil 4365, Rio de Janeiro, Brazil. bernardete.spisso@incqs.fiocruz.br <bernardete.spisso@incqs.fiocruz.br>
de Oliveira e Jesus
Ana Luiza
AL
de Araújo
Marcus Antônio Gonçalves
MA
Monteiro
Mychelle Alves
MA
D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D008892:Milk / Q000737:chemistry*; D013050:Spectrometry, Fluorescence / Q000379:methods; D013754:Tetracyclines / Q000032:analysis*
D013754:Tetracyclines