The structure elucidation of sex pheromones of Lepidoptera by a solid-sample injection technique in conjunction with capillary gas chromatography is described. The applicability of this method in GC and GC-MS modes was demonstrated by reanalyzing the sex attractants of females ofOstrinia nubilalis andBombyx mori. The pheromone complex ofMamestra brassicae was reinvestigated and (Z)-9-hexadecenyl acetate and (Z)-11-hexadecenol were found in addition to already known pheromone components of this species. By using the solid-sample injection, the exact site of pheromone release could be determined inM. brassicae.