柱前衍生化毛细管区带电泳法测定六味地黄丸中蜜二糖的含量Determination of melibiose as 1-phenyl-3-methyl-5-pyrazolone derivatives in Liuweidihuang pills by capillary zone electrophoresis
张佳蕊,刘永利,赵莉,木其尔,刘有平,邸欣
ZHANG Jia-rui,LIU Yong-li,ZHAO Li,MU Qi-er,LIU You-ping,DI Xin(School of Pharmacy
摘要(Abstract):
目的建立1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化毛细管区带电泳法测定六味地黄丸中蜜二糖的含量。方法采用熔融石英毛细管(45 cm×50μm,有效长度为36.7 cm),运行缓冲液为110 mmol.L-1硼酸(pH 10.0)溶液、分离电压为12 kV,检测波长为245 nm,温度为30℃,压力自动进样(50 mbar×6 s)。结果蜜二糖质量浓度在30.7~614.4 mg.L-1内线性关系良好(r=0.999 5),平均加样回收率为98.9%,RSD为2.6%(n=9)。结论该方法可作为六味地黄丸的质量控制方法之一。
Objective To develop a pre-column derivative capillary zone electrophoretic method for the determination of melibiose as 1-phenyl-3-methyl5-pyrazolone derivatives in Liuweidihuang pills.Methods An untreated fused silica capillary(45 cm × 50 μm,effective length is 36.7 cm) was used.The separation was carried out at 12 kV in a 110 mmol·L-1 boric acid buffer at pH 10.0.The capillary was kept at 30℃.The detection wavelength was set at 245 nm.Pressure injection of(50 mbar × 6 s) was employed.Results The linear range of melibiose was 30.7-614.4 mg·L1(r=0.999 5).The average recovery of melibiose was 98.9% with RSD of 2.6%(n=9).Conclusions The method is sensitive and well reproducible and can be applied in the determination of melibiose in Liuweidihuang pills.
关键词(KeyWords):
六味地黄丸;蜜二糖;毛细管区带电泳法;衍生化;1-苯基-5-吡唑啉酮
Liuweidihuang pills;melibiose;capillary zone electrophoresis;derivatization;PMP
基金项目(Foundation): 国家自然科学基金资助项目(20445003)
作者(Author):
张佳蕊,刘永利,赵莉,木其尔,刘有平,邸欣
ZHANG Jia-rui,LIU Yong-li,ZHAO Li,MU Qi-er,LIU You-ping,DI Xin(School of Pharmacy
参考文献(References):
- [1]谢鸣.方剂学[M].北京:人民卫生出版社,2002:208.
- [2]国家药典委员会.中华人民国和国药典:一部[M].北京:人民卫生出版社,2005:401-402.
- [3]武卫红,温学森,赵宇.地黄寡糖及其药理活性研究进展[J].中药材,2006,29(5):507-510.
- [4]HONDA S,SUZUKI S,TAGA A.Analysis of carbohy-drates as 1-phenyl-3-methyl-5-pyrazolone derivatives bycapillary/microchip electrophoresis and capillary elec-trochromatography[J].Journal of Pharmaceutical andBiomedical analysis,2003,30:1689-1714.
- 六味地黄丸
- 蜜二糖
- 毛细管区带电泳法
- 衍生化
- 1-苯基-5-吡唑啉酮
Liuweidihuang pills - melibiose
- capillary zone electrophoresis
- derivatization
- PMP