Alkyl-substituted insulin molecules are depository preparations used in the treatment of diabetes. The isolation and purification of these active compounds is performed on the hand of several complicated separation steps. In this work, nonmodified and new synthesized alpha,beta-unsaturated bovine insulins-(C12)(n) were selectively isolated from aqueous solution using tweezing adsorptive bubble separation (TABS) with BSA, which enabled reversible binding with the unpolar side chains of bovine insulin and its derivates. The bovine insulin/serum albumin complex could be efficiently transferred into the foam phase at pH 8 with an enrichment factor of 2.6 and a recovery of 89.7%. Experiments with alkylated alpha,beta-unsaturated bovine insulins-(C12)(n) performed at pH 9 enriched even quantitatively the complex under equal experimental conditions, accompanied with an enrichment factor of 3.3. Additionally performed radio immunoassay tests revealed that the immunological activity of alpha,beta-unsaturated bovine insulins-(C12)(n) remained unchanged after foaming.