To investigate the effects of vitamin C and E on electrolyte profile and the activity of acetylcholinesterase (AChE) in Aluminium (Al) chloride exposed rats, thirty-six male rats were used for this study. The animals were randomly grouped into six (n=6); group I (Control) was given normal saline. Group II (Al only) was exposed to 20mg/kg body weight (BW) of Al. Groups III (Vitamin C only) and IV (Vitamin E only) were administered 200mg/kg BW of vitamin C and vitamin E respectively. Groups V (Al + Vit C) and VI (Al + Vit E) were exposed to 20mg/kg Al and were treated with 200mg/kg vitamin C and vitamin E respectively. Al exposure resulted in a significant (P<0.05) increase in plasma calcium and erythrocyte magnesium concentrations compared with control. The erythrocyte sodium concentration of group treated with Al alone was significantly (P<0.05) higher by 2.01folds than the control group. While the two vitamins were unable to correct the disruption in calcium homeostasis, they ameliorated the intracellular levels of sodium and magnesium ions. A reduction in the activity of AChE (1378.90±130.02U/L)was observed in erythrocyte of the group exposed to Al when compared to the control (1968.80±283.72U/L). Treatment with vitamins C and E further inhibited erythrocyte AChE activity by 34% and 39% respectively compared to a 30% inhibition by Al only. Positive associations were observed between erythrocyte magnesium and blood sodium, and plasma calcium and erythrocyte sodium levels. Negative associations were however observed between plasma AChE activity and erythrocyte sodium and magnesium levels. In conclusion, vitamins C and E ameliorated ionoregulatory disruptions caused by sub-acute aluminium on only erythrocyte sodium and magnesium levels but not on plasma calcium level and erythrocyte acetylcholinesterase activity.