In this work, the optimization of the synthesis of PAN/Ag nanofiber composites via electrospinning was investigated via Taguchi experimental design approach. The adsorption capacity of sulfur compounds from natural gas condensate was considered as an objective function. The PAN/Ag nanofiber with 11 wt% PAN, 45 wt% AgNO3, 15 kV applied voltage, and 15 cm for distance of needle to a collector showed the highest adsorption capacity. The SEM, EDX, TEM, XRD, and FT-IR techniques were employed to elucidate the optimized PAN/Ag nanofiber structure. The results showed the successful synthesis of PAN/Ag nanofibers with diameters in 100-300 nm range and well distribution of Ag nanoparticles in the polymeric matrix. In addition, optimization of the adsorption capacity of PAN/Ag nanofiber in desulfurization of natural gas condensate in batch mode was performed via central composite design. Four factors including adsorbent weight, sulfur concentration in the natural gas condensate, the volume of sample, and the adsorption time were considered as effective factors each in three levels. The ANOVA analysis showed the more important factors on adsorbent performance are the concentration of sulfur in gas condensate and the weight of the adsorbent. The interaction terms between time and concentration and between volume and concentration are also important in response. Moreover, the response surface analysis of interaction terms showed the adsorptive nature of desulfurization.