Produksi jagung di Madura memberikan andil besar terhadap total produksi jagung di Jawa Timur. Di tingkat nasional, BPS menunjukkan bahwa produksi jagung di Jawa Timur mencapai 6 juta ton, berkontribusi sebesar 31.3%, atau hampir sepertiga dari total produksi jagung nasional. Produksi jagung yang besar seharusnya didukung dengan kesiapan teknologi produksi untuk mengolahnya menjadi aneka produk turunan, seperti pati. Pati jagung adalah bahan strategis karena digunakan di berbagai sektor, khususnya pangan. Studi ini dilakukan untuk optimasi proses ekstraksi pati jagung Madura-3. Teknik optimasi dilakukan menggunakan desain rancangan d-optimal pada Response Surface Methodology (RSM). Kondisi optimasi meliputi lama perendaman (X1) dan konsentrasi NaOH (X2), dengan rentang sebagai berikut: X1 (12 jam – 36 jam) dan X2 (0.05 – 0.5%). Hasil uji statistik memperlihatkan bahwa model yang berhasil dikonstruksi dinyatakan signifikan, ditunjukkan dengan F value sebesar 7.30, dan Prob lebih dari F sebesar 0.0075 (P kurang dari 0.05). Selain itu, lack of fit adalah 0.45, memperlihatkan bahwa parameter ini tidak signifikan. Lack of fit yang tidak signifikan memang diinginkan. Selain itu, nilai adequate precision dari model mencapai 7.469 (diinginkan lebih dari 4.0) Hasil optimasi menunjukkan bahwa kondisi optimum dapat dicapai pada kondisi X1 = 36 jam dan X2 = 0.05%. Kondisi optimum ini diprediksi mampu menghasilkan nilai rendemen 5.29%, dengan nilai desirability 0.719. Extraction of Madura-3 corn starch by optimizing soaking time and NaOH concentrationCorn production in Madura showed a tremendous contribution to total production in the Province of East Java. Noticeably, the province was recorded to yield 6 million tons of corn, responsible for approximately 31.3% of domestic production in 2018, as reported by BPS-Statistics. For this reason, there is a need for developing technology that enables to convert the corn into other valuable products, such as starch. Corn starch is essential material since it is applied in copious sectors mainly including food and pharmacy. This present work aimed at optimizing conditions for isolating starch of Madura-3 corn carried out using d-optimal design in Response Surface Methodology (RSM). The variables included soaking time (X1) and concentration of NaOH (X2), arranged as follows: X1 (12 – 36 h) and X2 (0.05 – 0.5%) according to preliminary research. The results demonstrated that the model constructed from data was significant, resulting in an F value of 7.30 and Prob more than F of 0.0075 (P less than 0.05). Furthermore, the statistical analysis showed a lack of fit at 0.45, which means that it was insignificance, which is favorable for this experiment. In addition, adequate precision of the constructed model was achieved at 7.469 (more than 4.0). Based on the statistical evaluation, the optimum condition for starch isolation was found at X1 = 36 h and X2 = 0.05%, which was predicted to yield starch at 5.29% with the desirability value of 0.719.