A simple dispersive solid phase micro-extraction methodology based on the application of nickel-aluminum layered double hydroxide (LDH) as an extractant was developed for the extraction and in situ determination of trace levels of dopamine (DA) by spectrofluorometry. The method is based on the extraction of DA at pH 8 using the Ni–Al(NO3) LDH sol solution as dispersed solid phase extractor. The extracted DA is quantified by spectrofluorometry at 285 nm excitation and 315 nm emission wavelengths.