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• A new fluorescence method was developed for the MPD determination. • The proposed method had a wide linear range of 10–600 μg L−1. • A low detection limit of 4 μg L−1 was obtained. • The method was successfully applied for detecting MPD in real samples. This work presented a new fluorescence method for the determination of m-phenylenediamine (MPD) based on the reaction between MPD and acetylacetone. The formed compound Hacac-MPD exhibited strong blue fluorescence emission under 365 nm excitation. Its fluorescence intensity had an excellent correlation with the MPD concentration Under the optimal conditions, the developed method gave a linear range of 10–600 μg L−1 with a low detection limit of 4 μg L−1. Furthermore, the coexistence of common inorganic ions and other aromatic amines had hardly influence on the determination of MPD, demonstrating high selectivity. Additionally, the MPD in spiked water samples and hair dye samples was successfully detected by the developed method, and the recoveries were 97.5%-101.6% and 98.3%-98.9%, respectively. The established method exhibited a good application prospect for the determination of MPD in environment and daily necessities. [ABSTRACT FROM AUTHOR]