The sex pheromones of Ectropis grisescensWarren and Ectropis obliqua Prout were both reported to contain (Z,Z,Z)-3,6,9-octadecatriene (Z3,Z6,Z9-18:H) and (Z,Z)-3,9-cis-6,7-epoxy-octadecadiene (Z3,epo6,Z9-18:H). To clarify how these two sibling geometrids maintain premating isolation, the female sex pheromones of the two species were reexamined. Gas chromatography–electroantennographic detection (GC-EAD) and gas chromatography–mass spectrometry revealed two GC-EAD-active compounds, Z3,Z6,Z9-18:H and Z3,epo6,Z9-18:H, in E. grisescens female pheromone glands as well as an additional GC-EAD-active compound, (Z,Z)-3,9-cis-6,7-epoxy-nonadecadiene (Z3,epo6,Z9-19:H), in E. obliqua female pheromone glands. Synthesized Z3,Z6,Z9-18:H and Z3,epo6,Z9-18:H elicited dose-dependent electroantennogram (EAG) responses from male antennae of both E. grisescens and E. obliqua. However, Z3,epo6,Z9-19:H only elicited dose-dependent EAG responses from E. obliqua and limited EAG responses from E. grisescens at all doses. In wind-tunnel studies, lures that contained Z3,Z6,Z9-18:H and Z3,epo6,Z9-18:H attracted E. grisescens males and had no effect on E. obliqua males.The addition of Z3,epo6,Z9-19:H to the blend of Z3,Z6,Z9-18:H and Z3,epo6,Z9-18:H strongly attracted E. obliqua males but had a limited attraction for E. grisescens males. Thus, Z3,Z6,Z9-18:H and Z3,epo6,Z9-18:H were sex pheromone components of E. grisescens, whereas Z3,Z6,Z9-18:H, Z3,epo6,Z9-18:H and Z3,epo6,Z9-19:H were sex pheromone components of E. obliqua.The presence or absence of Z3,epo6,Z9-19:H played a central role in the premating isolation of these two sibling species.