RESUMO
This paper describes a new approach for the determination of carbamazepine and lamotrigine in biological samples by ionic liquid dispersive liquid-phase microextraction prior to high-performance liquid chromatography with ultraviolet detection. The effects of different ionic liquids (ILs) on the extraction efficiency of carbamazepine and lamotrigine were investigated. The highest extraction efficiencies of carbamazepine and lamotrigine were obtained using 30 ?L of 1-me-thyl-3-octylimidazolium hexafluorophosphate [C8MIM][PF6]. Several factors affecting the microextraction efficiency, such as the type and volume of extracting solvent, type and volume of disperser solvent, salt concentration, and pH of the sample solution have been optimized. The calibration plots were linear in the range of 0.1-20 mg L-1 for carbamazepine and 0.3-40 mg L-1 for lamotrigine with detection limits of 0.04 mg L-1 for carbamazepine and 0.07 mg L-1 for lamotrig-ine in plasma samples. The results confirm the suitability of the presented method as a sensitive method for the analysis of the target analytes in urine and plasma samples.
Assuntos
Carbamazepina/análise , Líquidos Iônicos/química , Lamotrigina/análise , Carbamazepina/sangue , Carbamazepina/isolamento & purificação , Carbamazepina/urina , Cromatografia Líquida de Alta Pressão , Humanos , Imidazóis/química , Lamotrigina/sangue , Lamotrigina/isolamento & purificação , Lamotrigina/urina , Limite de Detecção , Microextração em Fase Líquida/métodos , Octanos/químicaRESUMO
In this work, the molecularly imprinted polymer nanoparticles (MIP-NPs) for the selective determination of fluvoxamine have been described. The polymer nanoparticles were synthesized by the polymerization of methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, 2,2-azobisisobutyronitrile as an initiator and fluvoxamine as a template molecule. The MIP-NPs were characterized using techniques that included Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Imprinted fluvoxamine molecules were removed from the polymeric structure using acetonitrile in methanol (2:8; v/v) as the eluting solvent. The linear dynamic range for fluvoxamine was 10-1200 µg L-1. The developed method was successfully applied to the extraction of fluvoxamine in complex biological samples.
Assuntos
Fluvoxamina/sangue , Fluvoxamina/urina , Polímeros Molecularmente Impressos/química , Nanopartículas/química , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Reagentes de Ligações Cruzadas/química , Humanos , Concentração de Íons de Hidrogênio , Metacrilatos/química , Microscopia Eletrônica de Varredura , Polímeros Molecularmente Impressos/síntese química , Nitrilas/química , Extração em Fase Sólida/instrumentação , Solventes/química , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
In this study microwave-assisted hydrodistillation (MAHD) has been compared with the conventional method of hydrodistillation for the extraction of the essential oils from two Iranian Lamiaceae species: Nepeta crispa Willd and N. racemosa Lam. The essential oils extracted by MAHD for 40 min were quantitatively and qualitatively (aromatic profile) similar to those obtained by conventional hydrodistillation for 3.5 h. The MAHD method yields an essential oil with higher amounts of more valuable oxygenated compounds, and allows substantial savings of costs in terms of time, energy and plant material.