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A poly(vinyl alcohol) (PVA) and Soluplus (SP)-based nanofiber (NF) mat was fabricated using an electrospinning method for the delivery of Angelica gigas Nakai (AGN) extract (ext) to oral cancers. AGN/SP NF (mean diameter: 75 ± 26 nm; entrapment efficiency: 84.6 ± 18.6%) and AGN/PVA/SP NF (mean diameter: 170 ± 35 nm; entrapment efficiency: 81.0 ± 10.1%) were fabricated using an electrospinning method. Amorphization of AGN EtOH ext was verified by X-ray diffractometry (XRD) analysis during the electrospinning process for the fabrication of NF structures. The AGN/PVA/SP NF group exhibited instant wetting (within 2 s) and rapid disintegration (within 3 min) properties compared with those in the AGN/PVA NF group, assuring the successful and conventional application of AGN/PVA/SP NF film in the oral cavity without the intake of beverages. After the spontaneous dispersion of NF in the aqueous media, it was converted to nanoparticles with a narrow size distribution. In YD-9 cells (oral squamous cell carcinoma from buccal cheek), the anti-proliferation activity was ordered as follows: AGN EtOH ext suspension < AGN/PVA NF < AGN/PVA/SP NF. All of these findings indicated that AGN/PVA/SP NF can be used as a fast-dissolving mat formulation for the therapy of oral cancers.