食品中的可卡因不易被察觉，为分析运动营养食品的安全性。本文采用液-液萃取-气相色谱法检测尿液和血液中的可卡因，将待检测的人体尿液和血液生物样本进行预处理，优化液-液萃取条件后，采用GC-FID方法获取检测尿液和血液在不同条件下的色谱图。实验结果表明，色谱图显示检测尿液中的COC和检测血液中的COC、EME与基体干扰的分离效果明显；随着加入可卡因标准溶液质量浓度的提升，检测尿液和血液中的可卡因平均回收率越高，最高平均回收率分别是96.73%和98.43%，且平均最小相对标准偏差是1.39%，人体食用运动营养食品后日内和日间血液中EME和COD的平均相对标准偏差均低于2.3%，说明该方法可准确检测出食用运动营养食品后人体尿液和血液中的可卡因，从而判定运动营养食品的安全性。

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.