摘要
目的:建立固相萃取-亲水作用色谱法(SPE—HILIC)测定人体血浆中的表阿霉素。方法:血浆样品中加入表柔红霉素作为内标,经 Oasis HLB 固相萃取(SPE)小柱萃取后进样测定,色谱柱为 Kromasil KR100—5SIL 硅胶色谱柱(250 mm×4.6mm,5μm),乙腈-甲酸铵缓冲液(40 mmol·mL^(-1),pH 2.9)(90:10)为流动相,检测波长为254 nm。结果:血浆中表阿霉素的线性范围为0.05~2.5μg·mL^(-1)(r^2=0.9991);最低检测限为0.05μg·mL^(-1);样品的回收率高于89.4%;日内及日间精密度RSD 小于7.0%。结论:方法简便,准确可靠,流动相与质谱检测器兼容,适用于血浆表阿霉素浓度测定及药代动力学研究。
Objective : To develop a solid phase extraction and hydrophilic interaction chromatography (SPE-HIL-IC) method for the determination of epirubicin in human plasma. Methods:Plasma samples were prepared with Oasis HLB solid phase extraction column. The chromatographic separation was performed on a Kromasil KR100 -5SIL column (250 mm×4.6 mm,5μm) with mobile phase of acetonitrile- 40 mmol·mL^-1 ammonium formate buffer solution (pH 2.9 ) (90: 10). The detection wavelength was 254 nm. Results:The calibration curve was linear over the range of 0.05-2.5 μg·mL^-1 (r^2=0.9991). The determination limit of epirubicin was 0.05 μg·mL^-1. The recovery was over 89.4%. The intra-day and inter-day RSDs were less than 7.0%. Conclusion : The method is simple, accurate and the mobile phase has the potential to be coupled with mass spectroscopy. It can be used to determine the epirubicin concentration in plasma and for the study of its pharmacokinetics.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第4期595-598,共4页
Chinese Journal of Pharmaceutical Analysis
基金
三峡大学博士启动基金资助项目
关键词
亲水作用色谱
固相萃取
表阿霉素
人体血浆
hydrophilic interaction chromatography
solid phase extraction
epirubicin
human plasma