本文利用环糊精修饰毛细管胶束电动色谱法(CD-MEKC)同时分离检测橙皮苷和柚皮苷对映体。实验优化的条件为:以60mmol/L胆酸钠(SC)+30mmol/L羟丙基-β-环糊精(HP-β-CD)+20 mmol/L NaH2PO4-100 mmol/L NaOH(pH=9.0,97%(V/V))+3%(V/V)甲醇为运行缓冲液,分离电压25kV,紫外检测波长214nm。在上述最佳条件下,橙皮苷和柚皮苷对映体在9min内得到完全分离,橙皮苷对映体的检测限(S/N=3)分别为0.13μg/mL和0.25μg/mL;柚皮苷对映体的检测限(S/N=3)分别为0.14μg/mL和0.07μg/mL。将所建立的方法用于胃苏颗粒制剂中橙皮苷和柚皮苷的对映体测定,回收率在86.0%~113.2%之间。
In this study,an effective method of cyclodextrin modified chiral micelle electrokinetic capillary chromatography (CD-MEKC) was established to enantioseparate and detect hesperidin and naringin simultaneously. Under the following conditions:running buffer of 60 mmol/L SC+30 mmol/L HP-β-CD +20 mmol/L Nail2 PO4-100 mmol/L NaOH(pH = 9. 0, 97G (V/V)) +3% (V/V) methanol, and separation voltage of 18 kV, the enantiomers were baselinly separated in 9 min. The detection limit (defined as S/N=3) of hesperidin and naringin enantiomers was ranged from 0.07 μg/mL to 0.25 μg/mL. The method can be successfully applied to the determination of hesperidin and naringin enantiomers in Weisu granules with satisfactory results.