A rapid, sensitive and simple technique was proposed for the preconcentration and determination of gold in the presence of N-methyl-N,N,N-trioctylammonium chloride (Aliquat 336) as ion pair forming agent employing microfunnel magnetic stirring-assisted liquid-liquid microextraction (MF-MSA-LLME) and flame atomic absorption spectrometry. Parameters were optimized by full factorial and Box-Behnken design. Under the optimum conditions, the calibration graph was linear in the range of 2.5-800.0 ng mL & x207b;(1) (r(2) = 0.998). Detection limit, enrichment factor and relative standard deviation were 0.6 ng mL & x207b;(1), 240.0 and 1.4% (n = 7, C = 100 ng mL(-1)), respectively. This technique was successfully applied for the determination of gold in soil and water samples.