C-phycocyanin (C-PC), a high-value phycobiliprotein derived from Spirulina platensis, is widely recognized for its applications in the cosmetic, food, and pharmaceutical sectors due to its anti-inflammatory, antioxidant, and natural colorant properties. Conventional extraction techniques are often limited by poor yield, significant energy requirement, and thermal degradation of the target protein. Pulsed electric field (PEF)-assisted extraction has developed into a sustainable, nonthermal approach that enhances cell membrane permeabilization, thereby improving the recovery of intracellular bioactive compounds. This chapter presents a comprehensive protocol for optimizing PEF parameters, including electric field strength, pulse number, pulse duration, and specific energy input for the efficient recovery of C-PC from Spirulina platensis dry biomass. The protocol integrates systematic experimental design and response surface methodology to identify optimal conditions that maximize yield, purity, and stability of the extracted pigment while minimizing processing costs. By providing optimization strategies and highlighting the critical process variables, this chapter provides a practical framework for researchers and industry practitioners aiming to scale up PEF-assisted extraction of C-PC in a sustainable and economically viable manner.