萘普生对映体的手性分离和纯度检查

目的: 建立萘普生手性分离和光学纯度检查的高效液相色谱方法。 方法: 采用Chiralpak AD-H (4.6 mm×250 mm,5 μm,Daicel公司)手性色谱柱在正相条件下拆分萘普生对映体,考察了固定相种类、流动相组成、柱温及流速等对萘普生对映体分离的影响,流动相为正己烷-异丙醇(30∶ 70,v/v),检测波长272 nm,流速0.5 mL·min^-1,柱温20℃。 结果: 在此条件下,萘普生及其(R)-(-)-构型体达到基线分离,分离度为3.3。 结论: 该法简单快速,重现性好,能够用于萘普生对映体的分离和纯度考察。

Objective: To develop a high performance liquid chromatographic method for chiral separation of the undesired enantiomer from naproxen and quantitative determination of bulk drugs. Methods: Baseline chiral separation of naproxen was achieved under normal-phase chromatographic mode by the Chiralpak AD-H (4.6 mm×250 mm,5 μm,Daicel) chiral stationary phase. The influences of the kind of chiral stationary phase and form of the mobile phase, column temperature and flowrate on the enantiomeric separation were studied. The optimized chromatographic conditions were hexane-isopropyl alcohol ( 30∶ 70, v/v ) as the mobile phase with a flow rate of 0.5 mL·min^-1 and detection at the wavelength of 272nm. The column temperature was set at 20℃. Results: A baseline separation of naproxen enantiomers was achieved,and the resolution was 3.3 between the enantiomers under the above chromatographic conditions. Conclusion: The method is simple, rapid and with good reproducibility,and it can be used for sepration and purity of naproxen.