High-performance liquid chromatography–mass spectrometry (HPLC–MS) was performed on insulin alone and insulin released from QD-INS and QD-INS–CS/GS. Release was promoted by hydrolysis for 28 days at 23 °C. Analysis shows insulin released from QD-INS and QD-INS–CS/GS has similar spectra to insulin alone, with 87.5% of the insulin released as a monomer.