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目的应用反相高效液相色谱法测定兔血清中5-氟尿嘧啶的浓度。方法兔血清样品经乙酸乙酯/异丙醇(84/16)萃取后,水浴氮气吹干,流动相定容后进样。色谱柱为kromasil-C18柱(250mm×4.6mm,5μm),流动相为20mM醋酸铵/乙腈(体积比98.2∶1.8,pH8.05),流速0.8mL/min,紫外检测波长为270nm。结果5-氟尿嘧啶在5～80μg/L浓度范围内呈良好的线性关系。10、20、40μg/L三个浓度的批内RSD分别为11.6%、5.6%、5.4%;批间RSD分别为12.8%、2.7%、6.2%;平均回收率分别为106.7±11.7%、98.0±5.3%、99.3±5.3%。结论本方法可靠、重复性好,具有特异性强、灵敏、精密度与准确度高等特点,满足5-氟尿嘧啶药代动力学研究的要求。
Objective To determine the concentration of 5-Fluorouracil in rabbit serum by reversed-phase high performance liquid chromatography. Methods Rabbit serum samples were extracted with ethyl acetate / isopropanol (84/16), dried in water bath, and the mobile phase was fixed for injection. The chromatographic column was a kromasil-C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of 20 mM ammonium acetate / acetonitrile (volume ratio 98.2:1.8, pH 8.05) at a flow rate of 0.8 mL / min and a UV detection wavelength of 270 nm. Results 5-Fluorouracil showed good linearity in the concentration range of 5 ~ 80μg / L. The intra-assay RSD of 10, 20 and 40 μg / L were 11.6%, 5.6% and 5.4% respectively. The inter-assay RSD were 12.8%, 2.7% and 6.2% respectively. The average recoveries were 106.7 ± 11.7% and 98.0% ± 5.3%, 99.3 ± 5.3%. Conclusion The method is reliable, reproducible and has the characteristics of specificity, sensitivity, precision and accuracy, and meets the requirements of 5-fluorouracil pharmacokinetic study.