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Electrospinning was employed to produce composite fibers mat consisting of PVP (polyvinylpyrrolidone)/CA (Cellulose Acetate) and Garlic Extract. The electrospun nanofiber mats for all variations show uniform and beaded free fibers. The average fiber diameter of composite fiber decreased along with the increasing applied voltage. The broad FTIR peak representing the stretching vibrations of O-H in hydroxyl groups of phenols and the sharp peak at 1014 cm-1 is the characteristic peak of garlic extract, which indicates the existence of S=O group and proving the presence of organosulfur compounds such as alliin, allicin dan diallyl disulfide. The characteristic peak shifted to a higher wavenumber after being synthesized into fibers. During the electrospinning process, the condition of cone jet in the tip of the needle was recorded and it was confirmed that when the applied voltage was from 12 to 14 kV there is intermittent squirt of solution indicating that the removal rate of the solution due to the applied voltage is smaller than the feed rate of solution. The concentration of garlic extract in the fibers was also examined and it was found that fibers with larger diameter contained larger concentration of garlic extract.