To establish a method to identify an unknown substance based on the combined use of gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q/Orbitrap HRMS)and nuclear magnetic resonance (NMR) techniques.The unknown substance was dissolved in methanol and was detected by GC-QTOF-MS and UPLC-Q/Orbitrap HRMS, and was dissolved in methanol-d4 to be detected by NMR.The main characteristics ion peaks of components with retention time of 9.67 min in GC-QTOF-MS measured were 84.080 8, 110.999 7, 128.107 0 (base peak), 138.994 7, etc. The protonated molecular ion peak m/z in UPLC-Q/Orbitrap HRMS was 268.109 3. It was inferred that the unknown substance was an analog of the synthetic cathinone substance 2-methyl-1-[4-(methylthio)phenyl]-2-morpholinopropan-1-one (MTMP) by comparing the mass spectrum information and molecular structure of MTMP. NMR analysis confirmed it as a novel N-morpholine substituted synthetic cathinone substance 1-(4-chlorophenyl)-2-methyl-2-morpholinopropan-1-one (CMMP).The method established in this study can be used for structural confirmation of CMMP.