This study aims to produce drug delivery systems using ultrasonic spray pyrolysis (USP) and electrospinning methods. For this purpose, the study was carried out in two steps. In the first step, polyvinylpyrrolidone (PVP)/gelatin (GEL) based nanofibers were produced by the electrospinning method. The nanofibers were coated with azithromycin (AZI) in the second step using the USP method. Finally, characterization studies such as morphological, chemical, and thermal were carried out, and drug release behaviors were analyzed. The findings show that nanofibers are noticeably fine, smooth, and uni-form. Although burst release was observed for the first time because the drug molecules were located on the nanofibrous surface, the release time was increased from 30 min to 48 h by obtaining sandwich structures. The results showed that the USP method could be used to produce new drug delivery systems with the electrospinning method.