In this study, we introduced a novel method that utilizes derivatization treatments in conjunction with ultra-high performance liquid chromatography coupled with high-resolution mass spectrometry (UPLC-HRMS) for the simultaneous quantification of 23 aldehydes and ketones (AKs) in food samples. Several key factors including the extraction procedure, the type and composition of acid solutions, and derivatizing agent concentration were optimized which influenced the extraction and derivatization efficiencies. Under optimal conditions, ultrasound-assisted extraction (50 W, 10 min, and 30 ℃) was selected as the most suitable method for extracting AKs from solid samples, with phosphoric acid (1%, V/V) as the preferred acid and 2,4-dinitrophenylhydrazine (DNPH) at a concentration of 50 μg/mL as the derivatizing agent. The proposed method exhibited good linearity over a wide concentration range (R² ≥ 0.995), high sensitivity with limits of quantification (LOQs) of 0.0020–0.1324 µg/mL, and high accuracy. Using the developed method, 23 AKs were successfully determined in tea and coffee samples. Compared with existing methods, this method achieves higher throughput while significantly reducing analysis time.