RESUMO
Two-phase micro-electrodriven membrane extraction (EME) procedure for the pre-concentration of selected non-steroidal anti-inflammatory drugs (NSAIDs) in aquatic matrices was investigated. Agarose film was used as interface between donor and acceptor phase in EME which allowed for selective extraction of the analytes prior to high performance liquid chromatography-ultraviolet detection. Charged analytes were transported from basic aqueous sample solution through agarose film into 1-octanol as an acceptor phase at 9 V potential. Response surface methodology in conjunction with the central composite design showed good correlations between extraction time and applied voltage (R2 > 0.9358). Under optimized extraction conditions, the method showed good linearity in the concentration range of 0.5-500 µg L-1 with coefficients of determination, r2≥ 0.9942 and good limits of detection (0.14-0.42 µg L-1) and limits of quantification (0.52-1.21 µg L-1). The results also showed high enrichment factors (62-86) and good relative recoveries (72-114%) with acceptable reproducibilities (RSDs ≤ 7.5% n = 3). The method was successfully applied to the determination of NSAIDs from tap water and river water samples. The proposed method proved to be rapid, simple and requires low voltage and minute amounts of organic solvent, thus environmentally friendly.
Assuntos
Anti-Inflamatórios não Esteroides , Cromatografia Líquida de Alta Pressão/métodos , Poluentes Químicos da Água , 1-Octanol , Anti-Inflamatórios não Esteroides/análise , Anti-Inflamatórios não Esteroides/isolamento & purificação , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Desenho de Equipamento , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificaçãoRESUMO
The aim of this study was to investigate and apply supported ionic liquid membrane (SILM) in two-phase micro-electrodriven membrane extraction combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) for pre-concentration and determination of three selected antidepressant drugs in water samples. A thin agarose film impregnated with 1-hexyl-3-methylimidazolium hexafluorophosphate, [C6MIM] [PF6], was prepared and used as supported ionic liquid membrane between aqueous sample solution and acceptor phase for extraction of imipramine, amitriptyline and chlorpromazine. Under the optimized extraction conditions, the method provided good linearity in the range of 1.0-1000µgL-1, good coefficients of determination (r2=0.9974-0.9992) and low limits of detection (0.1-0.4µgL-1). The method showed high enrichment factors in the range of 110-150 and high relative recoveries in the range of 88.2-111.4% and 90.9-107.0%, for river water and tap water samples, respectively with RSDs of ≤7.6 (n=3). This method was successfully applied to the determination of the drugs in river and tap water samples. It is envisaged that the SILM improved the perm-selectivity by providing a pathway for targeted analytes which resulted in rapid extraction with high degree of selectivity and high enrichment factor.