tSupercritical fluid extraction combined with two fractionation methods, sorption and series of separators,was applied on Eucalyptus globulus leaves in order to maximize the insecticidal activity of extracts againstLeptinotarasa decemlineata larvae. The yields and composition of eucalyptus extracts and essential oilwere compared. The major compounds in the essential oil isolated with the yield 26.7 mg/g were 1,8-cineole (42.6 wt%), -pinene (10.7 wt%) and globulol (5.9 wt%). The concentration of total volatiles inthe extracts varied from 2.8 to 59.5 wt%, depending on the extraction and fractionation conditions. Theextract obtained at 50◦C and 9 MPa exhibited the highest acute toxicity with LD50 = 38 g. ScCO2extractsexhibited several times stronger insecticidal activity in terms of chronic toxicity, antifeedant activity andgrowth inhibition than essential oil. Increase in the concentration of volatiles in isolates resulted intoincrease of chronic toxicity and antifeedant activity while growth inhibition decreased.