Objective: Cyanide is a highly toxic compound, and the consumption of products containing cyanide is a significant public health concern. Conversely, β-carotene possesses essential nutritional attributes for human health, therefore the characterisation and quantification of both compounds in food products is fundamental. Herein, cyanide and β-carotene levels in two flours produced from the roots of two varieties of cassava (Manihot esculenta crantz), namely UMUCASS-38(TMS 01/1371) and NR-8082, and their associated food products were detected and quantified. Results: The cyanide content of NR-8082 and UMUCASS-38 flours was determined at 18.01 ± 0.01 ppm and 17.02 ± 0.02 ppm (mean ± SD), respectively. These flours contained significantly higher (p < 0.05) than the residual cyanide levels determined in the cookies and cake produced therefrom with levels of 10.00 ± 0.00 ppm and 7.10 ± 0.14 ppm (mean ± SD), respectively. The levels of β-carotene determined in both the cake and cookie samples varied significantly (p < 0.05). The highest levels of β-carotene at 6.53 ± 0.02 μg/g (mean ± SD) were determined in raw roots of UMUCASS-38. While NR-8082 levels of β-carotene were less than UMUCASS-38 at 1.12 ± 0.02 μg/g (mean ± SD). Processing the roots into flour reduced the β-carotene content to 4.78 ± 0.01 μg/g and 0.76 ± 0.02 μg/g (mean ± SD) in UMUCASS-38 and NR-8082 flours, respectively. Cookies and cake produced from flour derived from the UMUCASS-38 variety had (mean ± SD) 2.15 ± 0.01 μg/g and 2.84 ± 0.04 μg/g of β-carotene, respectively.