Corn (Zea mays L.) not only used as food by humans, however also used for animal feed and industrial materials but in part of corncobs still untapped, corncobs is a lignocellulosic material with 38,99% ﬁber which contain the highest xilan (12,4%) comparedwithotheragriculturalwaste.Theobjectiveofthisresearchwastogetxylan fromcorncobswithextractionmethod.Xylanextractionfromcorncobsweredoneintwo steps, ﬁrstly deligniﬁcation process in NaOCl with concentration 0,5 on temperature 28∘C, solids which resulting from immersion in NaOH solution with concentration 5%, 10%, 15%, and 20% for 24 hours with temperature 20, 40, and 70∘C.the resulting of ﬁltrate were neutralized with HCL 6N, futhermore centrifuge during 30 minute with 4000 rpm. Water soluble xylan can separated with ethanol 95% with ratio supernatan and ethanol 1:3, yielding 12.9% of xylan. The solubility of xylan produced with alkali (NaOH 1%), HCl 1N, ethanol, in cold and hot water was observed. Quantitative and qualitative analysis of xylan were done using HPLC by measuring retention time. The instrumen used with HPLC Shimadzu C-R3A, C18 column type, water mobile phase, Refractive index detector with ﬂow rate 0,8 ml/minute result showed with purity 96%.