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This study was conducted in Maiduguri Metropolis of Borno State, Nigeria. The levels of fluoride, cadmium, arsenic, lead and nickel were determined in sachet, tap and ground water. The levels of fluoride and some heavy metals were also determined in blood and urine samples with respect to age groups. The sample collection and preparation were carried out using standard procedures. The concentrations of the heavy metals were determined by using Inductively Coupled Plasma Atomic Emission Spectrophotometer (ICPAES), while fluoride was determined Potentiometrically Using Ion-Selective Electrode. The results of this study showed that the concentration of fluoride was highest in male subject with a value of 1.65 mg/l within the age group of 51-60, while the lowest concentration of 0.02 mg/l was observed in female subject within the age group of 1-10. The concentrations of the metals studied in blood samples from male subject were significantly higher than in the female subject.