反相高效液相色谱荧光法测定人血浆中酒石酸罗格列酮含量

Reverse phase-high performance liquid chromatograpgy determination of rosiglitazone tartrate in human plasma by fluorescence detector

目的:建立快速灵敏的高效液相-荧光检测法测定罗格列酮的血浆浓度。方法:血浆样品加入内标(苯丙哌林)后用乙醚提取,乙醚层经空气流吹干后用流动相定容,20μl进样。色谱柱为KromasilC18(250×4.6mm,5μm),流动相采用0.025mol/L,pH=4.85的磷酸二氢钠缓冲液-乙腈(50:50),流速为0.5ml/min,荧光激发波长为250nm,发射波长370nm,内标法定量。结果:本法的最低定量浓度为4.87ng/ml,在14.6￣608.3ng/ml浓度范围内线性良好,r2=0.999。日内精密度为2.65%￣8.25%,日间精密度为5.0%￣8.6%,萃取回收率为68.04%以上,准确度为85.11%￣103.50%,整个分析过程在15min内完成。结论:该法准确、精密度高、重现性好,适用于人血浆中罗格列酮的动力学研究和生物等效性研究。

Objective：To develop a method for the quantitative determination of rosiglitazone in human plasma by means of reverse phase-high performance liquid chromatograpgy with a fluorescence detector.Methods：The rosiglitazone and benproperine （internal standard） in plasma was extracted with ether.Separation was accomplished on an reversed phase column （5μm,4.6×250mm）with a mobile phase of 0.025mo1/L sodium dihydrogen phosphate-acetonitrile（50：50;adjusted pH to 4.85 with phosphorous acid and triethylamine）.The flow rate was 0.5ml/min.Results：The calibration curve was linear within the range of 14.6-608.3ng/ml （r^2=0.999） plasma with acceptable accuracy and precision,The recovery of Rosiglitazone -in plasma were above 86%.The RSD of the within-day precision and the between-day precision were both lower than 8.6%.Conclusion：This method can be successfully used for the detection of plasma drug concentration in clinical pharmaeokinetic and bioequivalence studies of Rosiglitazone.