This study presents an analytical method (VA-D mu SPE-FAAS) for determining Mo(VI) in various food and water samples using flame atomic absorption spectrometry after separation via vortex-assisted dispersive solid-phase microextraction. A polypropylene imidazole amphiphilic derivative was synthesized and employed as an effective adsorbent for Mo(VI) extraction. Optimization of experimental variables-including pH, adsorbent mass, adsorption time, desorption solvent type and volume, and elution time-was performed using both a univariate approach and a Box-Behnken Design-based chemometric study. Under optimized conditions, the method demonstrated a wide linear range (0.3-280 mu g kg-1), high extraction recoveries (93.3 %-96.1 %), a substantial enrichment factor (103), and a low limit of detection (0.1 mu g kg-1). The method showed strong matrix tolerance and was successfully applied to certified reference materials (NIST-1568a Rice Flour and GBW 07605 Tea), yielding recovery values within acceptable ranges (91.8 %-97.4 %), thereby confirming the accuracy and applicability of the procedure for real sample analysis.