Summary A robust method for analysing acrylamide in plantain and cassava snacks was developed using SPME and GC‐FID. Optimised via Box–Benkhen design, the method met European standards with a calibration curve R 2 > 99%, detection limit 63 μg kg −1 , and quantification limit 212 μg kg −1 . Precision was <17.76% as per Horwitz equation. Acrylamide levels in fried ripe plantain were 894.40 ± 56.35 μg kg −1 and in cassava snacks 59.42 ± 2.46 μg kg −1 . This validated method offers an efficient means for acrylamide control in thermally processed foods.