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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 enantiomer concentration of flurbiprofen in plasma by high performance liquid chromatography. Methods: Flurbiprofen in plasma was extracted with cyclohexane in this experiment. The chromatographic column was Chirobiotic V (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of methanol-acetic acid-triethylamine (100: 0.01: 0.01) , Detection wavelength of 250 nm, the internal standard for S-ketoprofen. Results: No interference between the components, good resolution. The plasma R-flurbiprofen and S-flurbiprofen concentrations in the range of 30 to 1 000 ng.mL-1 within a good linear relationship. The relative recoveries of the two enantiomers were 98.6% -100.2% and 98.7% -101.2%, respectively, and the absolute recoveries were 76.1% -81.6% and 76.6% -80.5%, respectively. The RSDs were 3.9% -5.7% and 4.1% % ~ 6.2%, daytime RSD were 5.8% ~ 7.5% and 6.1% ~ 7.4% respectively. Conclusion: The method is rapid, simple, reproducible and sensitive. It can meet the need of determination of enantiomer concentration and pharmacokinetics of flurbiprofen in plasma.