摘要
目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定人血浆中5-氟尿嘧啶的浓度。方法:以5-溴尿嘧啶为内标,用Agilent-C18反相色谱柱(2.1 mm×150 mm,3.5μm)进行分离,甲醇-去离子水(0.1%甲酸)(80∶20)为流动相,柱温20℃,流速0.2 mL.min-1。采用电喷雾负离子化,多反应监测(MRM)进行定量分析。结果:5-氟尿嘧啶在5-1000μg.L-1浓度范围线性关系良好,最低检测浓度为5μg.L-1。日内与日间精密度均小于10%,方法回收率在96.0%-106.8%之间。结论:本方法简便快速、灵敏准确,适用于5-氟尿嘧啶在人体内的药代动力学研究。
Objective： To establish a method of high performance liquid chromatography tandem mass spectrometry （ HPLC - MS/MS） for concentration determination of 5 - fluorouracil in human plasma. Methods： Tile samples were separated by Agilent - Cls column with 5 - bromouracil as the internal standard. The mobile phase consisted of methanol -deionized water（0. 1% formic acid） （80： 20）. The column temperature was 20 ℃, and the flow rate was 0.2 mL · min^-1. 5 -fluorouracil was quantitated by multiple reaction monitoring（MRM） mode with negative elec- trospray ionization（ESI）. Results： The calibration curve of 5 -fluorouracil was linear in the range of 5 -1000 μg · L^-1. The minimal detectable plasma drug concentration was 5 μg · L^-1. Intra -day and inter -day RSD were both less than 10% and the average recovery was between 96.0% and 106. 8%. Conclusion： The method is sim- ple, sensitive and accurate. It is suitable for the pharmacokinetics study of 5 - fluorouracil in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第2期259-262,共4页
Chinese Journal of Pharmaceutical Analysis
