"Analysis of pharmaceutical compounds in biological fluids using on-line SPME-LC/MS" / "Análise de fármacos em fluidos biológicos empregando o acoplamento SPME-LC/MS"

AUTOR(ES)

Claudete Alves

DATA DE PUBLICAÇÃO

2006

RESUMO

Conventional methods used for the determination of drugs in biological fluids are based on chromatographic and immunochemical techniques. The biological samples treatment - which includes extraction, pre-concentration and clean up steps – has been required in drugs analysis in order to increase both analytical sensitivity and selectivity. Nevertheless, lately, within the advancements in instrumentation, different techniques have been evaluated for the analysis of different drugs in biological fluids, such as: solid phase microextraction (SPME) and liquid chromatography coupled to mass spectrometry (LC/MS). SPME presents many advantages towards the conventional extraction techniques (soxhlet, LLE and SPE), which include: use of simple analytical instrumentation, analysis automation, reuse of extractor fibers and integration of extraction, concentration and sample introduction in the same chromatographic system. In this work, a versatile and low cost interface was developed, which allows the coupling of SPME-LC/MS techniques to tricyclic antidepressants and anticonvulsivant drugs analysis. The employed factorial design has shown to be a simple and useful statistical tool. With this device more information could be obtained with fewer experiments by evaluating not only the main interaction effects but also the interaction effects of all variables on the results. The optimized chromatographic conditions were adequate for LC/MS analysis. The obtained detection levels highlight the importance of high performance liquid chromatography coupled to mass spectrometry (LC/MS). The developed method, for both tricyclic antidepressants and anticonvulsivants drugs, has presented specificity, accuracy, linearity and adequate limit of detection for this analysis.

ASSUNTO(S)

cromatografia líquida - espectrometria de massas pharmaceutical compounds liquid chromatography - mass spectrometry análise de fármacos solid-phase micro extraction micro extração em fase sólida

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