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Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME‐SFO) with simultaneous derivatization followed by high‐performance liquid chromatography‐diode array detection (HPLC‐DAD) was applied for preconcentration and determination of primary and secondary aliphatic amines in environmental water samples. A ternary mixture consisting of a disperser, an extractant and a derivatization reagent was used for the simultaneous derivatization and extraction of aliphatic amines in different water samples. The effects of various experimental parameters on derivatization and extraction efficiency were studied simultaneously using experimental design. A Plackett–Burman design was performed for screening of variables in order to determine the significant variables affecting the extraction efficiency. Then, the significant factors were optimized by using a Box–Behnken design …