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延胡索中紫堇碱标准品的制备及含量测定

【摘要】    目的研究延胡索中紫堇碱标准品的制备及含量测定方法。方法运用半制备高效液相色谱法分离纯化紫堇碱,采用薄层色谱法和高效液相色谱面积归一化法检测纯度,波谱法鉴定其结构,反相高效液相色谱法测定延胡索药材中紫堇碱的含量。结果制备的化合物鉴定为紫堇碱,纯度为99.5%;含量测定在0.131 2 ~1.131 2 μg范围内呈良好线性关系,r = 0.999 997,平均回收率为97.19%,RSD为2.25%(n = 9)。结论该制备方法效率高,所得化合物纯度高,可用于大量制备;含量测定方法准确,简便,可靠,重复性好。

【关键词】  紫堇碱; 半制备高效液相色谱法; 反相高效液相色谱

  husuo  W. T. Wang

  BAI Xue, XIAO Haitao, YANG Jie, ZHU Jie, HAO Xiaoyan*

  (Guiyang Medical University, Guiyang 550004, China)

  Abstract:ObjectiveTo study a preparation and determination method of corydaline in Corydalis yanhusuo  W. T. Wang.  MethodsThe corydaline was separated and purified by semi-preparative high performance liquid chromatograph. Its purity was determined by TLC and HPLC analysis and normalization of peak areas. The structure of corydaline was identified by spectrum, and the quantification was determined by RP-HPLC.  ResultsThe compound was identified as corydaline .The purity of the corydalis was 99.5%. There was a good linearity within the range of 0.131 2~1.131 2 μg (r= 0.999 997).The average recovery was 97.19%(RSD=2.25%,n=9) .  ConclusionThis preparation method is quick and convenient for producing the pure compounds from herbs with large capacity. The method is accurate and simple with good reproducibility, and it can control the quality of this herb and preparation effectively.

  Key words:Corydaline;   Semi-preparative high performance liquid chromatograph;  RP-HPLC
   
  延胡索Corydalis yanhusuo  W. T. Wang.为罂粟科植物延胡索的干燥块茎,具有活血化淤、理气止痛的功效,是我国传统常用中药。延胡索中主要含生物碱,其中延胡索乙素和丑素是延胡索镇痛的主要活性成分[1],2005年版《中国药典》及成方制剂中均采用延胡索乙素为对照品进行评价[2~4]。本课题组研究发现,延胡索生物总碱具有较好的抑制乙酰胆碱酯酶的作用,其中紫堇碱是主要活性成分之一,因此,有必要对延胡索中紫堇碱进行定性鉴别和含量测定。但是,目前市场上还没有紫堇碱对照品的销售,并且也未见采用紫堇碱为对照品来评价延胡索质量的报道。本文报道延胡索中紫堇碱对照品的制备方法和含量测定方法。

  1  仪器与材料
   
  X-4型显微熔点仪(国产,温度计未

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