An apparatus which couples a laser microprobe with a GC–MS has recently been constructed in our laboratories to facilitate analytical micropyrolysis studies. The utility and versatility of the technique is demonstrated through the analysis of micro-sized quantities of various organic fossils. Results are reported from a torbanite coal, Green River oil shale, Tasmanite oil shale, an isolated Tasmanites microfossil and oil-bearing fluid inclusions. A diverse range of aliphatic products including distributions of n-alkene/n-alkane pairs, isoprenoids, polycyclic biomarkers and various alkylaromatics have been detected from these materials. The analytical credibility of the laser micropyrolysis GC–MS technique is confirmed by the favourable comparison of the laser derived molecular data to corresponding data obtained from more traditional methods.