Background: Simple, chip and rapid analytical methods are required in biomedical analysis laboratories to support therapeutic drug monitoring units in hospitals. The present work aimed to provide such a method for quantitative determination of carvedilol in plasma samples. Results: A new, simple, precise and efficient method was developed for the determination of carvedilol in human plasma using a dispersive liquid–liquid microextraction based on solidification of floating organic droplet, followed by spectrofluorimetry method. Some important parameters such as types and volumes of extraction and disperser solvents, pH, salt effect and sample volume were optimized. Under the optimized experimental conditions, the method provided a linear range of 40 to 300 ng ml^-1, with a correlation coefficient of 0.996. The limit of detection, lower limit of quantification and upper limit of quantification were 18, 40 and 300 ng ml^-1, respectively. The found recovery was from 98.2 to 102.2%, the mean intra- and inter-day precisions were 8.3 and 6.4%, respectively. The relative error for accuracy varied from 0.4 to 2.2%. The short-term temperature and freeze–thaw stability studies showed that carvedilol in human plasma was stable for sample preparation and analysis after storage. Conclusion: The proposed method provided reasonable acceptable results and could be used for therapeutic monitoring of carvedilol.