Insect cuticular hydrocarbons are usually species-specific mixtures and may serve for species and gender recognition. They are, therefore, widely used in the chemotaxonomy and zoogeography of various insect taxa. In order to provide a basic study for further comparative analyses of cuticular hydrocarbon (CHC) profiles of cryptic species hidden within the South American fruit fly Anastrepha fraterculus complex (Diptera: Tephritidae), we analyzed the composition of the CHCs and their production with respect to age and sex in a laboratory population from Tucuman, Argentina. Several techniques of gas chromatography with mass spectrometric detection have been used in order to develop a suitable method for CHC identification, i.e., GC-MS in EI mode, GC-MS in CI mode, and GC×GC/TOFMS. Our analyses revealed a complex profile of aliphatic hydrocarbons in both males and females, consisting predominantly of n-alkanes, methyl-branched alkanes, as well as of alkenes and alkadienes. In young individuals (up to about 5 days after emergence), the CHC profiles were similar in males and females. However, in older flies, these profiles diverged and became clearly sex-specific. The temporal dynamics of the CHC patterns in both sexes were evaluated using multivariate exploratory techniques.