In this paper, HPLC-DAD and HPLC-FLD methods have been developed to monitor the hydroxylchloroquine pharmaceuticals in water samples. Within the validation of the methods developed, linearity, sensitivity and accuracy were examined, and the limits of detection and quantification and the working range of the method were determined. By comparing the performance characteristics of both methods, it was concluded that the HPLC-FLD method is more acceptable for the analysis of hydroxychloroquine because it allows the determination of lower concentrations of the investigated drug. Both methods were used to monitor photolytic and photocatalytic degradation of hydroxychloroquines. In the second part, photolytic and photocatalytic degradation of hydroxychloroquine was investigated using TiO2 as photocatalysts in the form of thin film and suspensions and various sources of radiation: LED lamps at wavelengths of 365 and 405 nm, solar - like lamp and halogen lamp. The results of photolytic and photocatalytic degradation of hydroxychloroquines have shown that they are not subject to photolytic degradation, and photocatalytic degradation is faster with the photocatalyst present in the form of suspension. Photocatalytic degradation kinetics follows the kinetics of the first order. Using the validated HPLC-FLD method, four degradation products were detected during photocatalytic degradation by a 365 nm LED lamp, whilst during photocatalytic degradation with 405 nm LED lamp, there were three degradation products. Using the validated HPLC-DAD method, two degradation products were detected during photocatalytic degradation by a 405 nm LED lamp, whilst during photocatalytic degradation with 365 nm LED lamp did not detect any degradant products.