Gas chromatography (GC) is a widely used technique for compounds separation, identification, and characterization. However, GC is known to be limited to the analyses of volatile and thermally stable substances. Therefore, special techniques were developed to allow the analysis of thermally labile and high boiling compounds. Some make use of special injectors such as cold on-column, programmable-temperature vaporizing injector, and direct sample interface, other rely on special interface and ionization hardware as field ionization, matrix-assisted laser desorption/ionization, and supersonic molecular beams. There is also the possibility of derivatize high boiling and thermally labile compounds to a more volatile and stable ones, but derivatization techniques are not universal, and some previous knowledge of the analytes is important for the success of the approach. As an example, tertiary amines and ethers do not react with trimethylsilylating reagents, one of the commonly used derivatizing reagents. In this work, we benefit from the features of short-column chromatography to analyze thermally labile and high boiling compounds of forensic interest in a standard gas chromatograph–mass spectrometer (GC-MS 7890A / 5975C models, Agilent). A 7.5-fold reduction in analytical column length (from the standard 30 meters to 4 meters) drastically reduced the harsh interactions of thermally labile compounds with the column, while decreasing the method’s resolution by only 2.7 times. The use of short-column reduced the pressure of the system allowing for a higher column carrier gas flow rate which resulted in a lower elution temperature of the analytes. Flow rates up to 4 mL/min of helium associated with split (20:1) injection also reduced the residence time in the injection port and promoted the detection of intact 25R-NBOH (R= Br, Cl, I, Et), a phenethylamine derivative drug known to be incompatible with GC-MS analysis due to its degradation during chromatography.