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Hoodia gordonii, a succulent plant growing in African arid regions, is used as a botanical dietary supplement for weight loss. The increasing concerns on the quality and safety of Hoodia products call for the needs of more science-based information, as well as objective and efficient tools for inspection. In the present study, NMR fingerprinting and multivariate analysis techniques were applied for the identification, discrimination, and quality analysis of Hoodia plant materials and commercial products. Four Hoodia species, namely H. gordonii (five authenticated samples), H. currorii (one authenticated sample), H. parviflora (three authenticated samples), and H. rushii (one authenticated sample), were investigated; the chemicals and characteristic spectral signals that made most contributions for their differentiations were revealed. With the aid of NMR fingerprint analysis, ten Hoodia products sold on the dietary supplement market were assessed for their chemical composition and quality. The study demonstrated that the NMR fingerprinting approach could be a promising and efficient tool for the authentication of botanicals.