Cocaine in food is hard to detect. In order to evaluate the safety of sports nutritional food, the method of liquid-liquid extraction-gas chromatography was used to detect cocaine in urine and blood. The human urine and blood biological samples to be detected were pretreated. After optimizing the conditions of liquid-liquid extraction, the chromatograms of urine and blood under different conditions were obtained by GC-FID. The results showed that the separation effect of COC in urine and COC, EME and matrix interference in blood were obvious. With the increase of the concentration of standard solution of cocaine, the average recovery rate of cocaine in urine and blood increased. The highest average recovery rate was 96.73% and 98.43%, respectively. The average minimum relative standard deviation was 1.39%. The average relative standard deviation of EME and COD in the blood of daytime and daytime after eating sports nutritional food was less than 2.3%. It shows that this method could accurately detect the cocaine in human urine and blood after eating sports nutritional food. It could evaluate the safety of sports nutritional food.