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Anal Chim Acta ; 637(1-2): 135-43, 2009 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-19286022

RESUMO

Aminoglycosides (AGs) are a large and diverse group of antibiotics. Although AGs may cause side effects of nephrotoxicity and ototoxicity, they are still occasionally being used for the treatment of serious infections. In this study the development of a method is described for the quantitative determination and confirmation of seven aminoglycosides (and relevant isomers) and spectinomycin in animal tissues. The extraction was based on an extraction followed by a concentration and clean-up step using weak cation exchange solid phase extraction. The separation was performed by ion-pair liquid chromatography on a C(18) column followed by mass spectrometric detection. The method was validated according to the EU requirements for a quantitative confirmatory method. Permethylated aminoglycosides (in-house synthesised internal standards) were used for accurate quantification. The accuracy of the analyses of AGs in kidney ranged from 94 to 111%, intra-day precision ranged between 2.5 and 7.4% (R.S.D.(r)) and inter-day precision ranged between 2.2 and 17.3% (R.S.D.(RL), n=21, MRL level). Accuracy (muscle tissue) varied from 83 to 128% with an intra-day precision between 2.2 and 17.3% (R.S.D.(r), n=7, MRL level). From the results it was concluded that the method was able to monitor MRL levels which ranged from 750 to 20,000 microgkg(-1) for kidney and from 50 to 10,000 microgkg(-1) for muscle tissue.


Assuntos
Aminoglicosídeos/análise , Antibacterianos/análise , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Espectinomicina/análise , Espectrometria de Massas em Tandem/métodos , Aminoglicosídeos/isolamento & purificação , Animais , Antibacterianos/isolamento & purificação , Resíduos de Drogas/isolamento & purificação , Padrões de Referência , Reprodutibilidade dos Testes , Espectinomicina/isolamento & purificação , Suínos , Espectrometria de Massas em Tandem/normas
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