This paper described a new method for the enrichment and determination of pyrethroid pesticides from environmental water samples with ordered TiO2 nanotube array micro-solid phase equilibrium extraction (μ-SPEE) prior to gas chromatography (GC) with electron capture detection (ECD). Several factors such as the anodization voltage, the kind of organic solvents, sample pH, equilibrium extraction time, desorption time and salting-out effect were optimized. Under the optimal conditions, ordered TiO2 nanotube arrays demonstrated excellent merits on the preconcentration of pyrethroid pesticides and good detection limits were achieved as 0.018, 0.020, 0.031, 0.041, and 0.070 μg L−1 for bifenthrin, fenpropathrin, cyhalothrin, fenvalerate, and deltamethrin, respectively. Four real water samples were used to validate the proposed method and the spiked recoveries were over the range of 81.9–110.6%. Compared to conventional solid phase extraction (SPE), the present method showed better recoveries and good reproducibility. These results showed that this μ-SPEE technique could be an important alternative to multistep SPE for the extraction and determination of such analytes in complex samples and become a useful tool in monitoring such analytes in the environment.
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