This study identified, quantified, and compared the phytochemical contents and antioxidant capacities of Aloe ferox lyophilized leaf gel (LGE) and 95% ethanol leaf gel extracts (ELGE) using GC-MS and spectrophotometric methods. Analytically, 95% ethanol is less effective than ethyl acetate/diethyl ether or hexane (in the case of fatty acids) extractions in separating phytochemicals for characterization purposes. However, although fewer compounds are extracted in the ELGE, they are approximately 345 times more concentrated as compared to the LGE, hence justifying ELGE use in biological efficacy studies in vivo. Individual phytochemicals identified included various phenolic acids/polyphenols, phytosterols, fatty acids, indoles, alkanes, pyrimidines, alkaloids, organic acids, aldehydes, dicarboxylic acids, ketones, and alcohols. Due to the presence of the antioxidant polyphenols, indoles, and alkaloids, the A. ferox leaf gel shows antioxidant capacity as confirmed by ORAC and FRAP analyses. Both analytical methods used show the non-flavonoid polyphenols to contribute to the majority of the total polyphenol content. Due to its phytochemical composition, A. ferox leaf gel may show promise in alleviating symptoms associated with/or prevention of cardiovascular diseases, cancer, neurodegeneration, and diabetes.