In this chapter, fundamental aspects of regenerative medicine are explained with special emphasis on application of polymeric materials for tissue engineering. In that regard, current chapter describes synthesis and processing of a biodegradable polymeric system in different compositions that can be applicable in tissue engineering. Copolymers of polyoctanediol citrate acid-sebacate acid P(OCS) were polymerized via polyesterification reaction in different molar ratios of the monomers in order to have a range of properties in developed materials. Different compositions have further been processed into the scaffolds for tissue engineering application. Developed scaffolds, were carefully analyzed by MALDI-ToF-MS and resultant spectra are interpreted in a great detail. Data obtained from MALDI analysis confirm that copolymer compositions match the expected structures, which were pre-determined in polymerization reaction. Furthermore, MALDI spectra provides a clear picture of the molecular structure that, in turn, plays a crucial role in understanding of the material properties. In a separate section, a detailed analysis is extracted from MALDI results regarding the suitability of the proposed materials for their application in tissue engineering. This chapter is dedicated to the MALDI analysis of a linear polymer system with 3 monomers involved in synthesis of P(OCS) materials.