Abstract The Nuclear Magnetic Resonance (NMR) has been employed as an excellent analytical technique for analyzing mixtures. For the use of NMR as a routine experimentation, new methodologies have been developed without the use of deuterated solvents also known as No-D NMR, which keeps the intrinsic advantages of NMR as a fast, non-invasive and non-destructive technique. In this study, we used No-D NMR as a tool for analysis in 71 samples of cocaine, one of ecstasy and one of metilona seized by Police in the State of Espírito Santo. During the analysis of cocaine seizure samples, we can observe a tendency of trafficking through its adulterants such as caffeine, phenacetin and lidocaine. The No-D NMR technique was also applied in order to develop a methodology for the analysis of illicit drugs and possibly become a routine in NMR laboratories. In these analyses, we can observe the high resolution power of the No-D technique combined with lower operating costs.