Offline two-dimensional normal-phase × reversed-phase liquid chromatography coupled with high-resolution mass spectrometry for comprehensive analysis of chemical constituents in Euphorbia kansui

Euphorbia kansui is the dried root of Euphorbia kansui T. N. Liou ex T.P. Wang. Its main chemical components are diterpenoids, triterpenes, and volatile oil. In this study, an offline two-dimensional (2D) normal-phase × reversed-phase liquid chromatography method coupled with quadrupole time-of-flight mass spectrometry was established to comprehensively analyze the chemical constituents in E. kansui. A total of 240 compounds were identified from the E. kansui extract, including 218 diterpenoids (77 known, 141 new), 16 known volatile oils, and six known triterpenes. The relationship between the structural characteristics and tandem mass spectroscopy fragments of diterpenoids was further analyzed. Based on the characteristic fragment ions, 141 new diterpenoids were determined as 118 ingenane diterpenoids and 23 jatrophane diterpenoids. The newly identified diterpenoids may provide lead compounds for drug discovery, improving the medicinal value of E. kansui.