Abstract

Optimum conditions for the determination of the herbicides paraquat, diquat and difenzoquat by micellar electrokinetic chromatography (MEKC) using sweeping and cation-selective exhaustive injection (CSEI) as on-line concentration methods were developed. Sodium dodecyl sulfate (80 m M) in 50 m M phosphate buffer (pH 2.5) with 20% acetonitrile was used as a background electrolyte for the methods studied. The limits of detection, based on a signal-to-noise ratio of 3:1, were about 2.6–5.1 mg l −1 in purified water when MEKC was applied for the standards. By using an on-line preconcentration method known as sweeping–MEKC, up to a 500-fold increase in detection sensitivity was obtained whereas up to a 50 000-fold increase for CSEI–sweeping–MEKC was achieved. The limits of detection using optimum CSEI–sweeping–MEKC were lower than 1 μg l −1 and the method was validated obtaining good reproducibility (relative standard deviation lower than 22%) and linearity. CSEI–sweeping–MEKC was successfully applied to the determination of the three herbicides in spiked tap water below the levels established by the US Environmental Protection Agency.

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