Azodicarbonamide (ADC) has been used as a flour bleaching agent or dough conditioner. A high‐performance liquid chromatography method was developed for simple and simultaneous analysis of ADC, semicarbazide (SEM), and hydrazine (HZ) using 4‐ethylbenzaldehyde (4‐EBA). Samples were extracted with methanol at neutral pH, and the extracts were concentrated at pH 1.0 and derivatized with 4‐EBA at pH 3. It was identified that ADC was decomposed to SEM, which was continually decomposed to HZ in an aqueous solution. This method was applied to the analysis of wheat flour products, and the results showed that SEM was detected up to a concentration of 0.42 mg/kg, but HZ was not detected in wheat flour products. The developed method enabled simple, less time‐consuming, and simultaneous analysis, and can be utilized to effectively evaluate ADC, SEM, and HZ concentrations in wheat flour products.