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By means of electrospinning, composite fibers mat built from PVP (polyvinylpyrrolidone) and CA (Cellulose Acetate) with garlic extract as active agent and glycerin as additive has been successfully produced. The electrospun nanofiber mats for all variations show some cluster with branches of fibers as the effect of glycerin. The average fiber diameter of composite fiber decreased along with the increasing applied voltage from 12 to 15 kV. However, the average diameter reduced when the applied voltage increased afterwards. In the FTIR study, a sharp peak at 1014 cm-1 as the characteristic peak of garlic extract, which attributes to the existence of S=O group and proving the presence of organosulfur compounds such as alliin, allicin dan diallyl disulfide, was found. In the composite fibers of PVP/CA/Glycerin/Garlic, the characteristic peak of garlic shifted to a higher wavenumber 1036 cm-1.