RESUMO
This study involved the development, validation and application of a three-phase hollow-fiber liquid-phase microextraction (HF-LPME) and liquid chromatography with diode array detection (LC-DAD) method for the simultaneous determination of the proton pump inhibitor (PPI) drugs omeprazole, pantoprazole and lansoprazole in human plasma. The evaluation of the HF-LPME parameters was crucial for the determination of the drugs and the conditions selected were: 1-octanol as solvent; phosphate buffer at pH 5 as donor phase; borate buffer at pH 10 as acceptor phase; extraction time of 15 min; stirring at 750 rpm and NaCl was added at 5% (w/v). Validation of the method according to US-FDA recommendations showed a good linear range (0.2-2.0 µg/mL) for all analytes, with a determination coefficient >0.9910. Precision was evaluated using intra- and inter-day assays, which showed relative standard deviations (RSD), <15% for all concentrations, with a limit of quantification (LOQ) of 0.2 µg/mL. Accuracy was also assessed at these concentration levels and was in the range from 80 to 130%. Finally, the sensitive, selective and reproducible HF-LPME/LC-DAD developed method was successfully applied to human plasma samples from patients undergoing therapy with the PPI drugs.
Assuntos
Cromatografia Líquida/métodos , Microextração em Fase Líquida/métodos , Inibidores da Bomba de Prótons/sangue , Humanos , Modelos Lineares , Reprodutibilidade dos Testes , Sensibilidade e EspecificidadeRESUMO
In this work a procedure for mercury determination by Flow Injection-Cold Vapor Generation-Inductively Coupled Plasma Optical Emission Spectrometry (FI-CVG-ICP OES) has been developed. The system uses a small homemade glass separator constructed to drive the Hg vapor to the plasma. An evolutionary operation factorial design was used to evaluate the optimal experimental conditions for mercury vapor generation, aiming at the low consumption of reagents, the improvement of the analytical signal and consequently greater sensitivity. The procedure allowed the determination of mercury and showed excellent linearity for the concentration range from 0.50 µg L(-1) to 100.0 µg L(-1), with Limits of Detection (LOD) and Quantification (LOQ) of 0.11 µg L(-1) and 0.36 µg L(-1), respectively, and a sampling rate of 36 analyses per hour. The optimized procedure showed good accuracy and precision, and the method was validated by the analysis of two certified reference materials: Buffalo River Sediment (NIST 2704) and human hair (IAEA 085). A good agreement with the certified values was achieved, with recovery values of 99% and 98% and relative standard deviation close to 2%.