Water samples of River Gwagwarwa and River Rafin Malam were subjected to liquid-liquid extraction and analyzed for organic pollutants. The organic parameters were determined using the standard methods of America Public health Agency (APHA) and was extracted and analyzed using Gas chromatography-mass spectrometer (GC-MS). Ten different organic compounds were detected at different percentage values at River Gwagwarwa while only seven different compounds were detected in River Rafin Malam. The compounds fall within five classes of organic compounds, which include carboxylic acid, acid chloride, ester, aldehyde and acid anhydride. The distribution pattern of the organic pollutants at the two sampling stations depict the pattern; River Gwagwarwa > River Rafin Malam. The study shows that organochlorine was the predominant organic pollutant present in River Gwagwarwa sample which is a hazardous pollutant while River Rafin Malam has no toxic pollutant which is attributed to lack of activity of the River.