In this work, Evaluation of the biological activity and the chemical composition of Mesembryanthemum nodiflorum and Aptenia cordifolia growing in Egypt were carried out. The chemical composition of both plants was evaluated by GC/MS and HPLC/MS analysis. GC/MS analysis of the unsaponifiable matter of Mesembryanthemum nodiflorum and Aptenia cordifolia resulted in the identification of 17 and 13 compounds; respectively, the major compounds were octadecane and neophytadiene; respectively. GC/MS analysis of the saponifiable matter of Mesembryanthemum nodiflorum and Aptenia cordifolia resulted in the identification of 12 and 18 compounds; respectively. The palmitic acid was the most abundant saturated fatty acid in both species. HPLC/MS analysis of Mesembryanthemum nodiflorum and Aptenia cordifolia resulted in the identification of 36 and 48 compounds; respectively. Finally biological studies indicated that the extract of Mesembryanthemum nodiflorum has more potent analgesic effect and also showed significant inhibitory activity against colon, cervix, liver and normal melanocyte carcinoma. The 70% ethanol extracts of the aerial parts of plants under investigation have a significant hypoglycemic effect, anti-oxidant, anti-inflammatory and hepatoprotective activity; where Aptenia cordifolia extract was more potent than Mesembryanthemum nodiflorum extract.