Advanced oxidation processes (AOPs) are widely applied to degrade persistent organic pollutants. In view of new stringent regulations on organic micropollutants, the real-time monitoring of AOPs became crucial to fulfil the high quality standards over time. A fluorescence sensor was employed to investigate the real-time monitoring of ozone and UV doses during AOPs designed to remove organic micropollutants from wastewater. Based on fluorescence data obtained in real-time with the sensor, accurate predictive models of UV and ozone doses were developed for two different tertiary wastewater effluents. This approach shows how fluorescence sensors can be used to optimize AOPs in real-time in terms of efficiency, chemicals and energy consumption.