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目的:建立酮洛芬对映异构体的拆分方法。方法:采用柱前衍生化RP-HPLC法,以L-丙氨酸-β-萘胺(L-Ala-β-NA)为手性衍生化试剂,色谱柱:Hypersil ODS-2柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.025 mol·L~(-1)磷酸二氢钾溶液(40∶60,v/v),流速:1.0 ml·min~(-1),检测波长:245 nm,柱温:25℃,进样量:10μl。结果:酮洛芬对映体衍生物获得较好的基线分离,S-(+)-对映体和R-(-)-对映体衍生物的色谱峰保留时间分别在24.2 min和26.0 min处。右旋酮洛芬在0.025~0.125 mg质量范围内线性关系良好(r=0.998 1),平均回收率为90.93%(RSD=4.10%,n=9)。结论:该方法简便、准确、快速,为酮洛芬的光学异构体的测定提供了参考依据。
Objective: To establish the resolution method of enantiomers of ketoprofen. Methods: The pre-column derivatization RP-HPLC method was used with chiral derivatization reagent L-alan-β-naphthylamine (Hypersil ODS-2 column × 4.6 mm, 5μm). The mobile phase was acetonitrile-0.025 mol·L -1 potassium dihydrogen phosphate solution (40:60, v / v), the flow rate was 1.0 ml · min -1 : 245 nm, column temperature: 25 ℃, injection volume: 10μl. Results: The baseline separation of ketoprofen enantiomers was achieved. The retention time of the chromatographic peaks of S - (+) - enantiomer and R - (-) - enantiomer was 24.2 min and 26.0 min Department. Dexketoprofen had a good linearity (r = 0.998 1) within the range of 0.025-0.1125 mg with an average recovery of 90.93% (RSD = 4.10%, n = 9). Conclusion: The method is simple, accurate and rapid and provides a reference for the determination of ketoprofen optical isomers.