The optimization of an analytical methodology for the determination of the 16-priority polycyclic aromatic hydrocarbons (PAHs) established by the American Environmental Protection Agency-EPA, in atmospheric particulate material was developed. The methodology consists of the combination of two analysis techniques: Vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) and extraction with pressurized hot water (PHWE) and subsequent quantification by gas chromatography coupled to mass spectrometry (CG / MS). Box-Behnken surface designs were applied which allowed to determine the best experimental conditions to maximize the response, defined as the area signal of the 16 PAHs under study. The optimal conditions established were; vortex time: 10s, centrifugation time: 10 min, centrifugation speed: 3000 rpm for the VA-DLLME technique and quantity of organic modifier 10%, extraction time: 10 min and extraction temperature: 150 <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">o</sup> C for the PHWE technique. The developed method showed adequate linearity (r2> 0.99) and the analysis of the SRM 1649b reference material showed the accuracy of the method, obtaining recovery percentages in the range of 81.45 to 99.8%.