The increasing use of the potent hallucinogenic drug d-lysergic acid diethylamide (LSD) makes the application of highly sensitive analytical techniques necessary. For an effective analysis of biological specimens a limit of detection in the sub-ng/ml range is required. Using capillary electrophoresis (CE) with laser-induced fluorescence detection it was possible to determine 0.1–0.2 ng LSD/ml blood. The conventionally used immunoassays and gas and high-performance liquid chromatographic methods have cut-off values and limit of detection, respectively, in the same range. Only tandem mass spectrometry techniques can be more sensitive. Therefore, CE can be considered a good complementary method to conventional immunological and chromatographic techniques for the forensic analysis of biofluids.