###### Abstract  
To analyze aroma active components in a food product, the crucial step is to select a suitable extraction technique. It should provide isolation of all components responsible for aroma creation, without the formation of any artifacts during the procedure. Preferably, the extraction method should yield analyzed compounds in detectable levels. The presented study aimed to compare three popular extraction techniques used in flavor studies: solid-phase microextraction (SPME), solvent-assisted flavor evaporation (SAFE), and simultaneous distillation extraction (SDE) in order to isolate aroma components from broccoli (_Brassica oleracea L_. var. _italica_). Obtained extracts were analyzed by gas chromatography-olfactmetry (GC-O) to determine compounds with aroma activity as well as gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC\(\times\)GC-ToFMS) to identify them. Thirty-four aroma active compounds were detected in broccoli by the applied techniques. SPME and SAFE together gave the full profile of aroma active components on chromatograms from GC-O, without artifacts that occurred in the SDE extract. SPME was particularly useful in the identification of early eluting compounds, while SAFE enabled isolating compounds with relatively low partition coefficients. Despite all the disadvantages of the SDE method, it leads to the identification of pyrazines, which were important contributors to the overall aroma. broccoli; flavor; aroma; GC-O; GC\(\times\)GC-ToFMS +
Footnote †: journal: _foods_  
0000-0001-6978-2278]M.M. temperature applied during the process, as well as long extraction time, might lead to artifact formation. Both methods require a solvent application and are relatively time-consuming. However, the extract can be stored at low temperatures for a long time and analyzed for as many times as necessary without quality changes. SPME requires the sample preparation indirectly before gas chromatography (GC) analysis. Thus, it does not make it possible to store the extract. However, it should not be forgotten that the SPME technique has also many important benefits, like simplicity, sensitivity and extremely short extraction time. This technique is commonly applied for the isolation of aroma compounds and also for quality purposes, such as to monitor changes in volatiles during storage, volatiles' profiling, or metabolomics purposes. Extracts of volatile compounds are subsequently analyzed by gas chromatography techniques. Gas chromatography-olfactometry (GC-O) to characterize an aroma profile of food products is a technique that is often described as a breakthrough in aroma research, which is caused by the association of the resolution power of capillary GC with the selectivity and sensitivity of the human nose. It is worth mentioning that the human nose is able to detect the odouriferous compound at the amount of \(10^{-17}\) g, while detectors commonly used in gas chromatography required at least \(10^{-13}\) g [11]. Gas chromatography with mass spectrometry is a technique used in order to identify aroma-active substances. In gas chromatography-mass spectrometry (GC-MS) the high separation power of GC is complemented by the identification capabilities of the MS. This technique is extremely useful, however, it has limitations, such as sensitivity and problems with coelution in complex matrices. Two-dimensional gas chromatography (GC\(\times\)GC) can overcome such limitations and is very useful as an additional technique used in aroma-active compounds' identification when coupled to high speed detectors such as time-of-flight (ToF) mass spectrometers. The aim of the presented study was to select the most appropriate technique to isolate volatiles from fresh, uncooked broccoli florets, which would be used for the identification of key aroma compounds in subsequent research. The results presented for broccoli would have broader importance for all vegetables from the _Brassicaceae_ family.