摘要
目的建立测定比格犬血浆非布司他浓度的高效液相色谱紫外(HPLC-UV)检测法。方法采用冰醋酸和乙腈对500μL比格犬血浆进行蛋白沉淀,离心后取上清液20μL进样分析。采用反相C18液相色谱柱(250mm×4.6mm,5μm)进行检测;流动相为甲醇-水(90∶10,V/V),流速1.0 mL/min,紫外检测波长为314nm。结果非布司他色谱峰的保留时间为4.50min,标准曲线在0.27~16.32μg/mL浓度范围内线性关系良好,平均相关系数(r)=0.999 5±0.002 0。日内和日间的精密度均不超过7.0%;准确度分别为96.7%~104.2%、97.7%~105.4%。结论 HPLC-UV检测法简单、准确、可靠,可用于非布司他药代动力学研究。
Objective To establish a high performance liquid chromatography-ultraviolet(HPLC-UV) assay for detecting plasma concentration of febuxostat in Beagle. Methods 500 /xL Beagle plasma sample was subjected to protein precipitation using glacial acetic acid and acetonitrile, and analysis was performed on 20uL supernatant after centrifugation. Reversed-phase C18 HPLC column (250.0 mmX4.6 mm,5 um) was applied with mobile phase consisted of methanol-water (90 : 10V/V) at a flow rate of 1.0 mL/min,the UV detection wavelength was set at 314 nm. Results Retention time of febuxostat chromatographic peak was 4.50 min. The standard curve was linear over the concentration range of 0.27-- 16.32/xg/mL with average correlation coefficient of 0. 999 5~0. 002 0. The relative standard deviations of intra and inter-day assay variations were less than 7.0~/00, and the accuracy were 96.7% -- 104.2%, 97.7% -- 105.4 %, respectively. Conclusion HPLC UV assay is simple, accurate and reliable, which can be applied to investigate the pharmacokinetics of febuxostat.
出处
《重庆医学》
CAS
CSCD
北大核心
2013年第1期49-50,53,共3页
Chongqing medicine
基金
2010年重庆医药高等专科学校科研课题基金资助项目(2009106)
关键词
色谱法
液相
分光光度法
紫外线
药代动力学
非布司他
chromatography, liquid
spectrophotometry, ultraviolet
pharmacokinetics
febuxostat