The weevil Metamasius spinolae (Gyllenhal) is the most important insect pest of cultivated prickly pear in Mexico. A previous work reported that the pheromone of this weevil species was composed by three components. In this study, we reinvestigated the aggregation pheromone of M. spinolae using gas chromatography-electroantennography and gas chromatography–mass spectrometry to locate and identify new potential pheromonal compounds. The behavioral activity of identified compounds was evaluated in laboratory and field trials. Metamasius spinolae males released four compounds: 2-methyl-4-heptanone, 6-methyl-2-hepten-4-one, 2-methyl-4-octanone, and 2-hydroxy-2-methyl-4-heptanone. In the laboratory assays, depending on the concentration, the compounds were attractive, neutral, or repellent to M. spinolae. Field evaluation showed that traps baited with 2-hydroxy-2-methyl-4-heptanone singly or in most of the binary or tertiary blends where this compound was present captured a higher number of M. spinolae compared to live males and the other compounds identified. In conclusion, our results indicate that 2-hydroxy-2-methyl-4-heptanone is the main component of the aggregation pheromone of M. spinolae. We suggest that this compound should be used for developing a monitoring or a mass-trapping system for M. spinolae.