The ultrasound assisted-dispersive solid-liquid multiple phase microextraction method was introduced. Bulky amine-functionalized bimodal mesoporous silica (NH2-UVM7) and [HMIM][PF6] were used as extraction phases. Reliable method for preconcentration and speciation of trace amounts of arsenic was presented. As(V) anions were complexed with amine group on surface of the UVM7.