The rising pollution of surface water by endocrine disruptive chemicals (EDCS) could lead to the persistent harm of aquatic wildlife. Addressing this concern, advanced waste water treatment techniques should be established in addition to the present sewage treatment. Therefore, the promising advanced oxidation process of photocatalysis is discussed. With the aim of establishing a novel high throughput screening approach for photocatalysts, a workflow resting upon the use of a self-constructed 60-fold parallel stirring UV-A LED photoreactor, followed by parallel sample extraction by SPE and sequential automated analysis by GC-MS, was developed, and is presented in this article. With the described system, TiO 2 -based photocatalysts, doped with different amounts of zinc, and synthesised by a sol-gel-route, were tested regarding their activity in the photocatalytic degradation of the synthetic estrogen 17α-ethinylestradiol. Thereby, the functional behavior of the photoreactor system and its applicability in a high throughput process could be evaluated. As a result of the catalyst screening, TiO 2 catalysts with low amounts of zinc were found with a significantly higher activity, compared to undoped TiO 2 . In conclusion, the presented system provides an easily accessible high throughput method for a variety of photocatalytic experiments.Materials 2020, 13, 1365 2 of 17 active [11]. To maintain the conditions of fresh water, municipal sewage treatment plants are introduced to the hydrological cycle, but it has been reported in literature that it is not possible to sustainably remove a plurality of micropollutants, and therefore EDC, from our wastewaters with the widespread activated sludge process [12][13][14][15]. In addition to this common type of sewage treatment, advanced oxidation processes (AOPs) like ozonation [16][17][18][19][20][21], or physical removal techniques like nanofiltration [22][23][24][25] and adsorption to charcoal [26][27][28][29][30], have been discussed lately. While these additional treatments deliver satisfying results regarding the reduction of micropollutants, they are inseparably linked to certain disadvantages, such as the generation of hazardous products and the disposal of adsorbents. Another, and presumably the most promising treatment procedure, is the photocatalysis [31][32][33][34], which is another variant of an AOP. Concerning the semiconductor materials utilised in this process, titanium dioxide (TiO 2 ) is the most established and examined one [35][36][37][38][39][40][41][42][43]. Apart from the fact that it is already known that estrogens could be degraded satisfactorily with the help of photocatalysis making use of TiO 2 , only few information has been gathered respecting reaction kinetics, matrix effects, reaction products, doped TiO 2 catalysts, and other semiconductors completely differing in their composition from TiO 2 for the deployment in photocatalytic reactions. For targeting these research subjects in depth, it is essential to implement procedures which enable a con...