Abstract: | The development of an analytical probe to monitor highly mutagenic picric acid (PA) carries enormous significance for the environment and for health. A novel, simple and rapid fluorescence analytical assay using sulfur‐doped graphene quantum dots (SGQDs) was designed for the highly sensitive and selective detection of PA. SGQDs were synthesized via simple pyrolysis of 3‐mercaptopropionic acid and citric acid and characterized using advanced analytical techniques. Fluorescence intensity (FI) of SGQDs was markedly quenched by addition of PA, attributed to the inner filter effect and dominating static quenching mechanism between the two, in addition to a significant colour change. The calibration curve of the proposed assay exhibited a favourable linearity between quenched FI and PA concentration over the 0.1–100 μΜ range with a lowest detection limit of 0.093 μΜ and a correlation coefficient of 0.9967. The analytical assay was investigated for detection of trace amounts of PA in pond and rain water samples and showed great potential for practical applications with both acceptable recovery (98.0–100.8%) and relative standard deviation (1.24–4.67%). Analytical performance of the assay in terms of its detection limit, linearity range, and recovery exhibited reasonable superiority over previously reported methods, thereby holding enormous promise as a simple, sensitive, and selective method for detection of PA. |