Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1–90 ng L−1 for deposition times of 50 s. LOD of 1.4 ng L−1 and LOQ of 4.3 ng L−1 were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane.