To reduce ammonia-like odor in chondroitin sulfate, longnose skate (Rasa rhina) cartilage was processed by washing, autoclaving, and alkali pretreatments. Content of total volatile basic nitrogen (TVB-N), index of ammonia-like odor, of raw skate cartilage without pretreatment was 254 mg/100 g, whereas those of skate cartilage pretreated with washing and autoclaving increased to 630 and 636 mg/100 g, respectively. TVB-N of skate cartilage pretreated with sodium hydroxide sharply decreased to 15 mg/l00 g at optimal condition of 0.12 M and 3.6 volume of NaOH, as determined by surface response methodology of central composite design for optimization. Alkali pretreatment resulted in 97.6% deodorizing. Washing and autoclaving pretreatments had almost no effect on the yield of chondroitin sulfate (approximately 30%), whereas decreased to 16.0% after alkali pretreatment, showing chondroitin sulfate of skate cartilage as chondroitin sulfate C.