A sensitive technique is described for the analysis of insect pheromones. Insect extracts are separated into fractions by column chromatography and are analyzed directly by quadrupole mass fragmentography on high-resolution glass capillary columns and by mass spectrometry. Applications are illustrated with two important pests. In the codling moth, trans-8, trans-10-dodecadien-1-ol was found to be present at a level of 3.5 ng per female, and in the European grapevine moth trans-7, cis-9-dodecadienyl acetate at a level of 1.6 ng. Both compounds appear to be present in high isomeric purity in the female insect and are absent in the corresponding males.