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The effect of the drying temperature on the volatile components and sensory acceptance of the Roselle (Hibiscus sabdariffa) extract in powder was investigated. The Roselle extraction was carried out by maceration with 7 L of 30% ethanol (v/v), 560 g of fresh Roselle calyces for 168 h. The Roselle extracts were spray dried at different temperatures 150, 160, 170, 180, 190, 200 and 210 degrees C, giving different outlet values about yield and final moisture. The volatile compounds in Roselle extract and dried samples were performed using needles of solid phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS HP-5890). Twenty volatile compounds were identified in the extracts among them terpenoids, esters, hydrocarbons and aldehydes. Fourteen volatile compounds were identified in the powder sample, but only ten were present in the Roselle extract. This indicates that some compounds were lost and some others were generated due to a degradation process. An acceptability sensory analysis showed that the best powder sample was the Roselle extract dehydrated using temperature between 190 degrees C and 200 degrees C (p<0.05). There was not statistically significant difference in the pH of Roselle extracts ranging from 3.4 to 3.9. It was concluded that the spray drying temperature of the Roselle extracts has an effect on the volatile compounds losses.