广东药学院药科学院
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李艺, 易润青, 刘丹, 等. 二元环糊精体系对柴胡中柴胡皂苷a与柴胡皂苷d的毛细管电泳分离测定[J]. 分析测试学报, 2011,30(8):902-906.
Separation and Determination of Saikosaponin a and Saikosaponin d of Bupleuri Radix by Capillary Electrophoresis[J]. 2011,30(8):902-906.
以磺丁基-β-环糊精(SBE-β-CD)和β-环糊精(β-CD)组成二元手性选择体系,用毛细管电泳法对柴胡中的柴胡皂苷a及柴胡皂苷d进行分离测定。考察了缓冲液的组成和浓度、手性选择剂的组成和浓度、进样方式及样品介质等对灵敏度和分离度的影响。结果表明:采用熔融石英毛细管柱(60 cm×50 μm i.d,有效长度为 53 cm),以20 mmol/L三羟甲基氨基甲烷(Tris)-20 mmol/L SBE-β-CD-25 mmol/L β-CD(pH 9.9)为运行缓冲液,分离电压15 kV,检测波长210 nm,以对硝基苯甲酸为内标,样品重力进样10 s,柴胡皂苷a和柴胡皂苷d可实现基线分离。两者分别在60~300 mg/L(r=0.999 7)和20~100 mg/L(r=0.999 5)范围内呈良好线性,平均加标回收率分别为102%和100%,RSD分别为1.2%和2.3%。该方法专属性强,结果准确可靠,重复性好,可用于柴胡中柴胡皂苷a及柴胡皂苷d含量的测定。
A high performance capillary electrophoresis(HPCE) method was established for the separation and quatitative determination of saikosaponin a and saikosaponin d in Bupleuri Radix by using sulfobutyl ether-β-cyclodextrin(SBE-β-CD)and β-cyclodextrin(β-CD) as dual cyclodextrin(CD) system.Experimental conditions,such as the concentration of running buffer,the types and concentration of CDs,separation voltage and sample medium,were investigated.The results indicated that saikosaponin a and saikosaponin d could be baseline separated on an uncoated fused sillica capillary column(60 cm×50 μm i.d.,effective length:53 cm) using 20 mmol/L tris(hydroxymethyl)aminomethane-20 mmol/L SBE-β-CD-25 mmol/Lβ-CD(pH 9.9) as running buffer.The separation voltage was set at 15 kV and the detection wavelength was 210 nm.Samples were injected into capillary by gravity for 10 s and p-nitrobenzoic acid was used as the internal standard.Under the optimal conditions,the calibration curves of saikosaponin a and saikosaponin d were linear in the concentration ranges of 60-300 mg/L(r=0.999 7) and 20-100 mg/L (r=0.999 5),respectively.The average recoveries of saikosaponin a and saikosaponin d were 102% and 100%,respectively,with RSD of 1.2% and 2.3%.The HPCE method was convenient,rapid and well repeatable,and was suitable for the quantitative analysis of saikosaponin a and saikosaponin d in Bupleuri Radix.
高效毛细管电泳法(HPCE)柴胡柴胡皂苷a柴胡皂苷d
high performance capillary electrophoresis(HPCE)Bupleuri Radixsaikosaponin asaikosaponin d
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