Technical Abstract: The rapid analysis of plant extracts for bioactive compounds was performed using a combination of UHPLC-MS and GC-TOFMS. Both techniques generate mass spectra that are useful for the determination of natural product structures. Alcohol extracts were obtained from Maclura pomifera (osage orange), a species known to contain numerous bioactive compounds, and analyzed with an Accela UHPLC-MSQ-PDA system (ThermoFisher Scientific, Waltham, Massachusetts, USA). Separations were performed using a C18 column. The MS detector was operated in negative mode with the electrospray interface. The diode array detector scanned between 200 and 400 nm. Samples were also analyzed by a Leco GC equipped with the Pegasus IV TOF detector (Leco Corp., St. Joseph, Michigan, USA). Spectral data were collected by both instruments and correlated to develop a library for the routine analysis of samples by LC-MS. This approach provided the sensitivity of the TOF system to identify target compounds with the use of LC-MS to quickly screen samples.