The aim of this in vitro study was to examine the effect of fluoride treatment on pellicle-covered enamel exposed to an acidic challenge simulating gastric reflux. Sixteen bovine and 16 human teeth were sectioned into four pieces, divided into four groups: (1) control, (2) 2-hour pellicle, (3) TiF(4), and (4) 2-hour pellicle + TiF(4), and subsequently subjected to 3 ml 0.01 M HCl stepwise for 4 + 4 + 4 min. The acid was analysed for calcium by atomic absorption spectroscopy. TiF(4) reduced Ca release from enamel by 76, 57 and 56% following the 4 + 4 + 4-min acid exposures, respectively, in bovine and 44, 54 and 54% in human enamel. These results suggest that treatment of enamel with a TiF(4) solution, with or without pellicle removal, may provide protection for the enamel against acid attack.