Having long been a victim of organic contamination, Houjing River (Kaohsiung City, Southern Taiwan) has been a subject of interest to both citizens and the city government. In fact, along with progressively negative concerns from local residents, the city government has tried to identify the contamination sources and mitigate adverse effects on human health and the well-being of local residents who have dwelled along the river for decades. In this study, related industrial plants that were specific contamination sourceshave been identified after a series of samplings and analyses. Water and sediment samples were analysed employing Gas Chromatography and Mass Spectrometry (GC-MS) techniques. The analytical results were then used to discuss the impact of riverside industrial plants in worsening the contaminationof the river. Comparisons between different river basins in terms of contamination have also beendiscussed for a more comprehensive studyof the Houjing River. Hopefully, the results of this study would be able to provide scientific andtangible evidence for the city government in order to take immediate and more forceful actions on the aggravating contaminationof the river as the well-being of more than 100,000 lives depend on it.