黑种草子中黑种草皂苷A的结构鉴定及含量测定

目的对从黑种草子中分离得到的黑种草皂苷A进行结构鉴定,并建立其含量测定方法。方法采用大孔吸附树脂、硅胶柱等方法分离纯化得到黑种草皂苷A,综合理化性质和波谱学数据进行结构鉴定。用HPLC法测定其在药材中的含量,用Agilent Eclipse XDB-C 18色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-水(28∶72);柱温:35℃;流速:1.0 mL·min-1;检测波长:210 nm。结果黑种草皂苷A在0.02012~1.00600 mg·mL^-1范围内,峰面积与质量浓度呈良好的线性关系(r=0.9999);平均回收率为104.51%,RSD值为1.46%(n=6)。结论该含量测定方法操作简便、准确度高、重复性好,可控制黑种草子药材的质量。

Structural identification and determination of nigella A in seeds of Nigella glandulifera

Objective To separate and characterize nigella A in seeds of Nigella glandulifera and to establish a method for its content determination.Methods The compound was isolated by chromatography on macroporous adsorption resin and silica gel,and the structure was elucidated by spectroscopic analysis.The content of nigella A was determined by HPLC.The separation was performed on an Agilent Eclipse XDB-C 18 column(250 mm×4.6 mm,5μm)using isocratic elution with acetonitrile-water(28∶72)at the flow rate of 1.0 mL·min^-1.The detection wavelength was set at 210 nm,and column temperature was 35℃.Results The linear range of nigella A was 0.02012-1.00600 mg·mL-1(r=0.9999).The average recovery was 104.51%(RSD=1.46%,n=6).Conclusion The method is simple,accurate and reproducible.It is effective in controlling the quality of seeds of Nigella glandulifera.