The use of plants as sources of drug agents is attributed by factors among which are the easyaccessibility to plants, less toxicity and little or no drug resistance. An improvement in both traditionalmedicine and drug discovery field necessitates investigation of pure compounds in any plant withmedicinal value. Synadenium glaucescens Pax of the family Euphorbiaceae is among the medicinal plantin Tanzania which are proven to contain bioactive compounds against microbial infections. Analysis ofethanolic and methanolic extracts of root and stem barks respectively aided to isolated six purecompounds (SG1- 6). These compounds were analyzed by both 1D, 2D NMR and GC-MS while theirspectral processing was achieved in the Bruker TopSpin 3.6.2. Among these compounds, one was aphenolic (hemicosanyl ferulate-SG1), three triterpenoids, (lupeol- SG2, epifriedelanol- SG4 and eupholSG5), one steroid (?-sitosterol- SG6) and a long chain alkene (1-nonacosene- SG2). Cytotoxicityevaluation by Brine shrimp lethality test (BLST) indicated the compounds under report were practicallynon-toxic.