Chlorpyrifos is one of the most toxic pollutants for aquatic ecosystem. The present study investigated the extraction of chlorpyrifos in water and liver tissue of zebrafish (Danio rerio). Water was collected at 0, 24, 48, 72 and 96hrs after the addition of toxicant and the amount of chlorpyrifos present in the water and liver tissue. In the concentration level range of 200 μg/L for the extraction of chlorpyrifos from water and liver tissue. Amount of chlorpyrifos in water and liver tissue analyzed by HPLC to know the amount of residue left out in the water and zebrafish liver after addition of 200 μg/L of chlorpyrifos initially. The recoveries were the decrease of concentration chlorpyrifos in water and increase in liver with increase in time of exposure is an indication of the accumulation of the toxicant in the organism through uptake. This could be hazardous as it could make its way into the food chain.