目的：探讨复方乙酰水杨酸片中非那西丁和咖啡因的含量测定方法。方法：在乙醇中溶解样品，用０２ｍｏｌ／ＬＮａＯＨ水解乙酰水杨酸后，以ｐＨ６５磷酸盐缓冲液为溶剂进行定量，采用多元回归分光光度法。结果：非那西丁和咖啡因的平均回收率分别为９９８％和９９９％，ＲＳＤ为０７２％和０５２％。结论：样品的测定结果同部颁标准法比较在准确度上无显著差异。 Objective: To investigate the method for the determination of phenacetin and caffeine in compound acetylsalicylic acid tablets. Methods: The samples were dissolved in ethanol, hydrolyzed acetylsalicylic acid with 02 mol / L NaOH, and quantified with pH65 phosphate buffer as solvent. Multiple regression spectrophotometry was used. Results: The average recoveries of phenacetin and caffeine were 99.8% and 99.9%, respectively, with RSDs of 072% and 052%. Conclusion: There is no significant difference in accuracy between the results of the sample determination and the ministry standard method.