目的：建立一套测定咖啡因的２种主要代谢物ＡＦＭＵ和１Ｘ的高效液相色谱（ＨＰＬＣ）方法。方法：选用岛津ＳｈｉｍＰａｃｋＣＬＣＯＤＳ柱，流动相为甲醇乙腈水醋酸（１２∶１．５∶８６．４５∶０．０５）。对１２０名健康志愿者服用咖啡５ｇ后４ｈ～５ｈ尿样进行测定，以ＡＦＭＵ与１Ｘ摩尔比作为代谢指标，并作频谱显示。结果：受试者可明显划分为快乙酰化者和慢乙酰化者，快、慢乙酰化表型之比１０１∶１９。结论：咖啡因ＨＰＬＣ方法的建立及在Ｎ乙酰化分型中的成功应用，为国内进行Ｎ乙酰化分型提供了一种值得推广的新方法 Objective: To establish a high performance liquid chromatography (HPLC) method for the determination of two major metabolites of caffeine, AFMU and 1X. Methods: The Shima  PackCLC  ODS column Shimadzu, mobile phase methanol  acetonitrile  water  acetic acid (12: 1.5: 86.45: 0.05). 120 healthy volunteers taking 5g of coffee after 4h ~ 5h urine samples were measured to AFMU and 1X molar ratio as a metabolic index, and the spectrum showed. Results: Subjects were clearly divided into fast acetylator and slow acetylator, fast, slow acetylated phenotype ratio 101:19. Conclusion: The establishment of caffeine HPLC method and its successful application in N-acetylation typing provide a promising new method for N-acetylation typing in China