Pectin is a type of anionic polysaccharide naturally found in a number of fruits and vegetables. Although pectin is widely used for food industry, its biomedical applications such as wound dressing, drug delivery and cancer targeting have also been investigated. In our study, we combined extracted pectin (from albedo of lemon peels) with chitosan (as a natural polymer) to synthesize chitosan/pectin cryogels. The extracted pectin was subjected to qualitative and quantitative analyses. Chitosan/pectin spongy supermacroporous cryogels were produced by cryogelation method at different combinations (100:0, 80:20, 60:40 and 40:60, w/w). Polyelectrolyte interactions between pectin and chitosan and crosslinking of chitosan with glutaraldehyde were verified by using FTIR. The porosity, swelling ratio, degradation behaviors and mechanical properties of cryogels were determined. SEM analysis demonstrated the pore morphology and average pore diameters of cryogels. After all analysis, 40:60 chitosan/pectin cryogel was selected for cytotoxicity studies. Glioblastoma (U-87 MG) cell line was used to evaluate the in vitro cytotoxicity of scaffolds. MTT assay and SEM analyses demonstrated the scaffolds were nontoxic, and supported cell attachment and viability.