Abstract: Gas chromatography-quadrupole time-of-flight mass spectrometry (GC-Q-TOF MS), high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry (HPLC-LTQ/Orbitrap MS) and nuclear magnetic resonance (NMR) were used to qualitative analysis the captured unknown sample. The sample was dissolved in methanol. After vortex and centrifugation, the supernatant was used for GC-Q-TOF MS detection. The values of mass-to-charge ratio (m/z) of main characteristic fragment ions showed by the component with retention time of 27.92 min were 286.203 7, 215.154 0, 195.149 0, 172.111 8, 117.069 6 (base peak). HPLC-LTQ/Orbitrap MS analysis showed that the protonated molecular ion was m/z 287.212 1. The corresponding MS information of the national controlled narcotic drug bucinnazine with the main characteristic fragment ions of m/z 272.188 1, 201.138 4, 181.133 3, 172.111 8, 117.069 6 (base peak) and the protonated molecular ion of m/z 273.196 5 were compared. The unknown sample was inferred as methyl derivative of bucinnazine, and its molecular formula was C₁₈H₂₆N₂O. After NMR analysis, the unknown sample was confirmed as the new opioid psychoactive substance 2-methyl-bucinnazine.