Abstract: Capsicum oleoresin was used as the raw material to explore the effect of resin separation and crystallization on the purity of capsaicinoids. The results showed that NKA-Ⅱ macroporous resin was feasible for the purification. During the resin adsorption process, the optimum adsorption conditions were as follows:4.0mg/mL of the sample concentration, 2.5mg/mL of the sample flow rate with pH7. And the optimal desorption conditions were 90% of alcohol, 2.0mL/min of the eluting rate with pH4. After capsicum oleoresin was separated by NKA-Ⅱresin and extracted by petroleum ether and ethyl ether, then it was recrystallized by petroleum ether for 3.0h with 20mg/mL of concentration and-5℃ of temperature, the purity of capsaicin was up to 92.46%.