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目的:建立替加氟静脉输注后血浆中活性代谢物5-FU浓度的HPLC-UV检测方法。方法:5名肿瘤病人静脉滴注替加氟4 h后采集静脉血。以阿昔洛韦为内标,采用硝酸银沉淀蛋白,上清液吹干后用流动相复溶。采用Kromasil 100-5 C18柱(4.6 mm×250 mm)色谱柱,检测波长265 nm,柱温45℃,流速1.0 mL.min-1,流动相为三乙胺(0.5%,冰醋酸调pH至6.98)-甲醇(97∶3,V/V)。结果:在线性范围62.5～750 ng.mL-1内低、中、高浓度5-FU的回收率分别为:88.3%、82.4%和91.6%;低、中、高浓度的批内RSD分别为:1.6%、1.8%和3.2%;批间样品RSD分别为:13.8%、13.8%和5.7%。最低检测限为31.25 ng.mL-1。结论:方法灵敏度高、稳定性好、特异性强、干扰少,可以为5-FU药代动力学和生物等效性研究提供方法。
OBJECTIVE: To establish a HPLC-UV method for the determination of 5-FU in plasma after intravenous administration of tegafur. Methods: Five tumor patients were treated with intravenous drip of tegafur for 4 h after venous blood was collected. Acyclovir as an internal standard, silver nitrate precipitation protein, the supernatant was dried with a mobile phase reconstituted. A Kromasil 100-5 C18 column (4.6 mm × 250 mm) was used. The detection wavelength was 265 nm, the column temperature was 45 ℃, the flow rate was 1.0 mL.min-1. The mobile phase consisted of triethylamine (0.5% 6.98) -methanol (97: 3, V / V). Results: The recoveries of low, medium and high concentrations of 5-FU in the linear range of 62.5-750 ng · mL-1 were 88.3%, 82.4% and 91.6%, respectively. The intra-assay RSD of low, medium and high concentrations were : 1.6%, 1.8% and 3.2%, respectively; RSD of inter-sample was 13.8%, 13.8% and 5.7% respectively. The minimum detection limit is 31.25 ng.mL-1. Conclusion: The method has high sensitivity, good stability, strong specificity and less interference and can provide a method for the study of pharmacokinetics and bioequivalence of 5-FU.