Microextração líquido-líquido dispersiva (DLLME) utilizando líquido iônico (IL) como solvente extrator foi desenvolvida com uma nova abordagem para a determinação de quatro pesticidas piretróides em amostras ambientais de água e solo. Cromatografia líquida de alto rendimento com detector de UV (HPLC-UV) foi empregada na análise cromatográfica. Este método é rápido, fácil de operar e ambientalmente correto. O solvente clorado altamente tóxico foi substituído pelo IL hexafluorofosfato de 1-hexil-3-metilimidazólio ( [C 6 MIM][PF 6 ]), para o qual elevados valores de recuperação de extração e fatores de enriquecimento foram obtidos. Os efeitos do volume de IL, tipo e volume do solvente dispersor, adição de sal, pH e tempo de extração foram investigados e otimizados. Nas condições ideais, o método mostrou boa resposta linear com valores de coeficiente de correlação (R 2 ) no intervalo de 0,9943 a 0,9986. Desvio padrão relativo (RSD) variou de 3,9 a 10,1%. Fator de enriquecimento, limite de detecção e recuperação variaram de 260 a 319, de 0,94 a 1,97 μg L -1 e de 89 a 98%, respectivamente. Para amostras de água reais, RSD variou de 3,8 a 10,8%, e recuperação de 83 a 99%. Para análise de amostra de solo, RSD e recuperação variaram de 3,7 a 8,9% e 88 a 98%, respectivamente.Dispersive liquid-liquid microextraction (DLLME) using ionic liquid (IL) as extraction solvent was developed as a new approach for the determination of four pyrethroid pesticides in environmental water and soil samples. High-performance liquid chromatography with ultraviolet detection (HPLC-UV) was employed on chromatographic analysis. The method is rapid, easy to operate and enviromentally-friendly. The highly toxic chlorinated solvent was replaced by the IL 1-hexyl-3-methylimidazolium hexafluorophosphate ([C 6 MIM][PF 6 ]), in which high extraction recovery and enrichment factors were obtained. The effects of IL volume, type and volume of disperser solvent, salt addition, pH and extraction time were investigated and optimized. Under optimum conditions, the method showed good linear response with correlation coefficient (R 2 ) values in the range of 0.9943 to 0.9986. Relative standard deviation (RSD) varied from 3.9 to 10.1%. Enrichment factor, limit of detection and recovery ranged from 260 to 319, 0.94 to 1.97 μg L -1 and 89 to 98%, respectively. For real water samples, RSD ranged from 3.8 to 10.8%, and recovery from 83 to 99%. For soil sample analysis, RSD and recovery ranged from 3.7 to 8.9% and 88 to 98, respectively.Keywords: ionic liquid dispersive liquid-liquid microextraction, pyrethroid pesticides, HPLC-UV, environmental sample
IntroductionPyrethroid pesticides are synthesized through biomimetic synthesis method based on the natural pyrethrin structure. They have been widely applied in controlling agricultural and sanitary pests 1 because of their excellent insecticidal activity, fast knockdown capability and relatively low mammalian toxicity, 2,3 and have been gradually taking the place of organophosphorus and carbamate pesticides. [4][5]...