Acetalated Dextran (Ac-Dex) is a promising pH-sensitive biocompatible and biodegradable polymer for nanomedicine applications. In this work, Ac-Dex nanoparticles were synthesized by two different solvent evaporation methods, the single nanoemulsion and the double nanoemulsion. The Ac-Dex particles were characterized by Scanning Electron Microscopy and the synthesis of highly homogeneous spherical particles was verified. Then, an optical fiber sensor based on quasi-elastic light scattering and comprised of only single-mode optical fibers and standard telecommunication devices showed sensitivity regarding the nanoparticles concentrations and was used for monitoring their degradation over 12 hours under pH and temperature conditions of cancerous tissues. The results revealed a well-controlled degradation pattern, corroborating the suitability of the modified polymer to the release of active compounds in a sustainable manner and also demonstrating the applicability of the sensor for the in-situ evaluation of the degradation.