目的 建立高效液相色谱同时测定人血浆中化疗药物5-氟脲嘧啶（5-FU）和丝裂霉素（MMC）浓度的方法。方法 以5-氯脲嘧啶（5-CU）和对氨基苯乙酮为内标，采用惠普1100型高效液相色谱仪，以HP Hypersil ODS column(125 mm×4 mm, 5 μm)为分析柱，前加HP Licrosphere C₁₈保护柱，以乙腈和水为流动相低压梯度洗脱，紫外可变波长检测器在254 nm波长检测5-FU和5-CU，310nm检测对氨基苯乙酮，365 nm检测MMC，同时测定5-FU和MMC的浓度。血浆样本用醋酸乙酯分二步直接萃取两种药物及其内标，40℃氮气吹干，残留物100 μL水溶解后，20 μL进样。结果 样品中各成分分离良好，无干扰。线性方程为：5-FU：Y=1 162X-3.162，r=1.000 0；MMC：Y=339.4X-1.062，r=0.998 9。线性范围：5-FU：50～2 500 ng·mL^-1；MMC：10～500 ng·mL^-1。检测限：5-FU：10 ng·mL^-1；MMC：10 ng·mL^-1。提取回收率：5-FU，5-CU，MMC约70%；对氨基苯乙酮为99%。结论 本法适用于包含5-FU和MMC的化疗方案的监测及药动学的研究。

OBJECTIVE To develop a high-performance liquid chromatography method for simultaneously determining the concentrations of fluorouracil (5-FU) and mitomycin C(MMC),the chemotherapeutic drugs in human plasma.METHODS The HP 1100 HPLC system was used, including a quaternary pump, a manual injector, a variable wavelength detector and a LC 2D ChemStation. The analytical column was a HP Hypersil ODS column(125 mm×4 mm, 5 μm) with a HP Licrosphere C₁₈ guard column. The gradient mobile phase, consisted of acetonitrile and water was flowed through the system with the speed of 0.8～1.2 mL·min^-1.The gradient rate of acetonitrile and water was became from 0% to 28%.The detective UV wavelength was 254 nm for 5-FU and 5-CU(IS), 310 nm for 4-aminoacetophenone(IS) and 365 nm for MMC. The plasma samples, added 5-chlorouracil (5-CU) and 4-aminoacetophenone as the internal standards,were extracted two times with ethylacetate. The organic phase was evaporated by N₂ at 40℃.The residue was with 100 μL water. 20 μL was injected.RESULTS The chromatography was good and not interfered by the components of the plasma.The liner equations were Y=1 162 x-3.162，r=1.0000（50～2 500 ng·mL^-1）for 5FU and Y=339.4x-1.062，r=0.998 9(10～500 ng·mL^-1) for MMC,respectively.The RSD of intraday was less than 5%, and the RSD of interday was less than 10%.The extracted recovery of 5-FU, 5-CU and MMC was about 70%.CONCLUSION It appeared to be an accurate, convenient and effective method which can simultaneously determine the concentrations of 5-FU and MMC in plasma.