Poly(vinyl pyrrolidone)(PVP)/(strontium/barium acetate)/titanium isopropoxide composite fibers were prepared by electrospinning technique via sol-gel process. Diameters of fibers prepared by calcinations of PVP composite fibers were 80–140 nm (solid) and 1.2-2.2 μm (hollow fibers prepared by core-shell method). These fibers were characterized using scanning electron microscope (SEM), X-ray diffraction (XRD), and transmission electron microscope (TEM) analytical techniques. XRD results showed better crystalline nature of the materials when calcined at higher temperatures. SEM and TEM results clearly showed the formation of hollow submicrometer tubes. The surface area of the samples determined by BET analysis indicated that hollow fibers have ~20% higher surface area than solid fibers. The UV studies indicate better detoxification properties of the hollow fibers compared to solid fibers.