A novel, simple and sensitive liquid chromatography-hydride generation online coupled with atomic fluorescence spectrometry (LC-HG-AFS) method was developed for simultaneous determination of p-arsanilic acid (p-ASA) and roxarsone in feed. 20% Methanol aqueous was used as extraction reagent, after preprocessing samples by ultrasonic oscillation, then injected into the chromatography Waters symmetry shield™ RP18 analytical column (150mm × 4.6mm, 5 μm), finally detected by an atomic fluorescence spectrometer. The calibration curves of analyses were linear over a range of concentrations (0.2–4mg L − 1) and the correlation coefficients were higher than 0.9990. The limits of detection were 0.2 mg L − 1. The method has been validated by linearity, precision and recovery. p-ASA and roxarsone in feed can be successfully and simultaneously determined using the developed method without a tedious pretreatment procedure.
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