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In this study, spray-dried alfuzosin hydrochloride (ALF)-loaded casein (CAS) nanoparticles were successfully used for the preparation of a swellable floating matrix via direct compression. The developed NIR calibration model was able to assess ALF and CAS levels in five different batches of drug-loaded nanoparticles. The calibration and prediction plots exhibited good linearity with correlation coefficients of more than 0.9. The standard error of calibration and cross-validation was less than 5% of the measured values, confirming the accuracy of the model. A linear relationship was obtained correlating the actual drug entrapped and the predicted values obtained from the NIR partial least squares regression model. The un-crosslinked tablet demonstrated a substantial weight gain (317% after 2 h) and completely disintegrated after 3–4 h whereas both 10 and 40% w/w genipin-crosslinked tablets showed lower weight gain (114 and 42% after 2 h, respectively). A rapid floating of the tablets within 5–15 min (compared to 45 min for the marketed tablet) was observed, with maintained floating for 24 h. Marketed and prepared tablets succeeded to prolong ALF release for 24 h. The development of drug-loaded CAS nanoparticles using spray-drying represents a new alternative for the preparation of swellable floating tablets for prolonged drug release.