This study evaluated the effect of Hibiscus sabdariffa (HS) (Malvaceae) calyces on fermentation kenetics, phytochemical constituents, volatile organic compounds (VOCs) and sensory profile of beer. Single infusion method of mashing was utilized, and the resulting beers were compared to industrial beers. HS supplementation did not alter the fermentation kenetics as a general decrease in extracts (oBrix) was observed in treated and the control fermentations. The HS beer (HSB) showed higher polyphenols and antioxidant activities than the control Belgian ale beer (BAB) including the industrial beers. One of the industrial beers, BRB showed slightly higher total flavonoid than HSB but not statistically different (p >.05). The peak response of ethyl acetate in HSB (199.61 ± 2.51 × 105 TIC) was significantly (p <.05) higher compared to BAB (22.86 ± 2.01 × 105 TIC). Generally, sensory panelists preferred HSB and BAB over the industrial beers. Therefore, we have demonstrated that supplementing wort with HS during brewing will not alter fermentation performance but augment beer with health promoting phytochemicals. © 2021 The Authors. Food Frontiers published by John Wiley & Sons Australia, Ltd and Nanchang University, Northwest University, Jiangsu University, Zhejiang University, Fujian Agriculture and Forestry University. ; Ministry of Education and Science of the Russian Federation, Minobrnauka, (FEUZ‐2020‐0058, H687.42B.223/20) ; This work was carried out with financial support from the Ministry of Science and Education of the Russian Federation, State Contract No. FEUZ‐2020‐0058 (H687.42B.223/20).