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Euphorbia hirta and Euphorbia jolkinii are two plant species belonging to the Euphorbiaceae family, which is distributed mainly in Asia, Africa, and Latin America. E. hirta has been traditionally used in folk medicine for the treatment of several pathologies, such as pulmonary and digestive diseases, gonorrhea, eczema and acne, while E. jolkinii has shown grassland degradation capacity. All these properties are linked with the presence of bioactive phytochemicals. Therefore, this study aimed to determine the phenolic compounds present in the whole part of E. hirta and E. jolkinii through LCDAD-ESI-MSn after extraction of dried whole plants with a mixture of H2O:MetOH, v/v 80:20, 1h, at room temperature. A total of 26 and 24 phenolic compounds were identified in E. hirta and E. jolkinii, respectively. Whereas both extracts presented a good number of phenolic compounds, E. jolkinii presented a higher concentration of compounds than E. hirta, with 85.72 and 59.77 mg/g extract of dried weight (d.w)., respectively. The primary phenolic compounds present in E. hirta were protocatechuic acid hexoside and quercetin-O-rhamnoside isomer (12.92 ± 0.04 and 12.53 ± 0.73 mg/g extract d.w., respectively), glycosides of a phenolic acid and a flavonoid. Regarding E. jolkinii extract, an isomer of the tannin galloyl-HHDP-hexoside and quercetin-O-rhamnoside predominated with 47.08 ± 0.02 and 12.42 ± 0.62 mg/g extract d.w., respectively. Considering the results achieved, the phenolic compounds found in both Euphorbia species are suggested to apply in the food industry for the formulation of functional foods and pharmaceuticals in the preparation of nutraceuticals. [ABSTRACT FROM AUTHOR]