Fruit aroma, a mixture of chemical compounds with odor, is a strong attractant derived from a complex mixture of different amounts and intensities (threshold) of chemical compounds found in fruits. The odor-producing compounds of fruit aroma are derived from carbohydrates, lipids, phenolic compounds, and mono- and sesquiterpenes, among others. The identification of compounds responsible for fruit aroma is usually conducted using gas chromatography coupled with olfactometry (GC-O). This technique separates the chemical compounds from the aroma of foods using a chromatographic column and divides the resultant outflow between the physical detector and a testing outlet (sniffing port). Trained judges describe the perceived odor in terms of the intensity of the odor zones perceived according to their training method. Moreover, the use of GC-O coupled with a mass detector (GC-MS-O) allows for the retrieval of chemical information such as identification and quantification of compounds, which can be correlated to sensory information. This review aimed to demonstrate the application of GC-MS-O in the identification of precursor compounds in fruit aroma, considering important factors for the application, main results, and most recent advances in this field.