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• Ultrasound and ultraviolet had synergistic effect on the degradation of chlorpyrifos. • The degradation mechanism mainly involves oxidation, hydrolysis and de-chlorination. • The toxicities of degradation products were lower than that of chlorpyrifos. • The combined treatment had little effect on the quality of the treated milk. The aim of this study was to compare the degradation kinetics of chlorpyrifos by treatment with ultrasound (US), ultraviolet radiation (UV) and a combination of both (US/UV), to evaluate the toxicity of the degradation products and the effect of the treatments on milk quality. US/UV markedly accelerated the degradation of chlorpyrifos. The half-life of chlorpyrifos by US/UV was 6.4 min, which was greatly shortened compared to the treatment with US or UV alone. Five degradation products were identified by GC–MS, and a degradation pathway for chlorpyrifos was proposed, based on density functional theory calculations. According to the luminescent bacteria test and predictions from a structure/activity relationship model, the toxicity of the degradation products was lower than that of chlorpyrifos. In addition, US/UV treatment had little effect on the quality of the treated milk. Therefore, US/UV can be used as a potential non-thermal processing method to degrade pesticide residues in milk. [ABSTRACT FROM AUTHOR]