The yields (solids out of dryer/solids in liquid feed) from the spray drying of hibiscus (Hibiscus sabdarifa L.) and fibre (sugar cane core fibre) slurry (ratio 50:50 hibiscus to fibre and a solids content of 10% solids to water) have been explored in a Buchi B-290 mini spray dryer. The inlet and outlet temperatures of the spray drying process have a significant effect on the yield of the resulting hibiscus and fibre powder. The best yield found from this study was found at an inlet temperature of 130ºC with a 5% feed rate and an outlet temperature of 77 ºC giving a yield of 46% of total materials sprayed.