目的：利用高效液相色谱法测定血清中的高三尖杉酯碱的含量。方法：以内标法为基础，取１ｍＬ血清标本加入内标三尖杉酯碱，经二氯甲烷２次重复提取，减压蒸干，残渣用流动相溶解，进样。色谱条件：以Ｃ１８反相柱为分析柱，流动相组成为０１ｍｏｌ·Ｌ－１甲酸铵－甲醇（２∶１），流速为１０ｍＬ·ｍｉｎ－１，在紫外检测器波长２９０ｎｍ处进行检测。结果：方法学检查：最低检测限２ｎｇ·ｍＬ－１，在４～１５００ｎｇ·ｍＬ－１范围内呈线性，回收率９１３％（ｎ＝８），批内和批间的相对标准偏差分别为１２％（ｎ＝８）和３６％（ｎ＝４）。结论：对临床化疗常与之配伍使用的３种药物，进行干扰实验，未发现干扰峰。 Objective: To determine the content of homoharringtonine in serum by high performance liquid chromatography. METHODS: Based on the internal standard method, 1 mL serum samples were added to the internal standard harringtonine, extracted twice with dichloromethane, evaporated to dryness under reduced pressure, and the residue was dissolved in the mobile phase and injected. Chromatographic conditions: A C18 reversed-phase column was used as an analytical column. The mobile phase consisted of 01 mol·L-1 ammonium formate-methanol (2∶1) at a flow rate of 10 mL·min-1 at a UV detector wavelength of 290 nm. Conduct the test. Results: Methodological examination: The minimum detection limit was 2ng·mL-1, linear in the range of 4～1500ng·mL-1. The recovery rate was 913% (n=8). The relative standard deviations within and between batches were respectively. It is 12% (n=8) and 36% (n=4). Conclusions: Interference experiments were conducted on the three drugs commonly used in clinical chemotherapy, and no interference peaks were found.