This paper describes the development of a new multisyringe flow injection analysis set-up that enables the complete automation of the dispersive liquid–liquid microextraction (DLLME) technique using solvents lighter than water. Its hyphenation with a liquid chromatographic separation is implemented using a single multisyringe pump obtaining a compact, simple, easy to operate, and fast instrument. DLLME is carried out with a throughput of 42 h−1 and DLLME for the extraction of benzo(a)pyrene and its subsequent chromatographic determination can be carried out with an analysis throughput of 7 h−1.