高效液相色谱法测定人血浆氟比洛芬对映体浓度

Determination of enantiomers of flurbiprofen in plasma by HPLC

目的:建立用高效液相色谱法测定血浆氟比洛芬对映体浓度的方法。方法:本试验采用环己烷提取血浆样品中氟比洛芬,色谱柱为Chirobiotic V(250 mm×4.6 mm,5μm),流动相为甲醇-冰醋酸-三乙胺(100∶0.01∶0.01),检测波长为250 nm,内标为S-酮洛芬。结果:各组分之间没有干扰,分离度良好。血浆中R-氟比洛芬和S-氟比洛芬浓度在30～1 000 ng.mL-1范围内线性关系良好。两个对映体相对回收率分别为98.6%～100.2%和98.7%～101.2%,绝对回收率分别为76.1%～81.6%和76.6%～80.5%,日内RSD分别为3.9%～5.7%和4.1%～6.2%,日间RSD分别为5.8%～7.5%和6.1%～7.4%。结论:该方法操作快速简便,重现性好、灵敏度高,可满足血浆氟比洛芬对映体浓度测定及药代动力学研究的需要。

Objective：To establish a method for the determination of plasma levels of enantiomers of flurbiprofen.Methods：Flurbiprofen was extracted with cyclohexane.HPLC was performed on a Chirobiotic column with methanol-aceticacid-triethylamine（100∶0.01∶0.01）as mobile phase.Detection wavelength was 250 nm.S-Ketoprofen was used as the internal standard.Results：Under this chromatographic condition,R-flurbiprofen,S-flurbiprofen and S-Ketoprofen had no interference with each other.The calibration curve was linear in the range of 30-1 000 ng·mL^-1 for R-flurbiprofen and S-flurbiprofen.The relative recoveries of R-flurbiprofen and S-flurbiprofen were 98.6%-100.2% and 98.7%-101.2%,respectively.The absolute recoveries of R-flurbiprofen and S-flurbiprofen were 76.1%-81.6% and 76.6%-80.5%,respectively.The intraday RSDs were 3.9%-5.7% and 4.1%-6.2%,and interday RSDs were 5.8%-7.5% and 6.1%-7.4%,respectively.Conclusion：This method is rapid and simple,with high sensitivity and good repeatability,it can be used for the determination of flurbiprofen enantiomers in human plasma and their pharmacokinetic study.