蟾酥中3种脂溶性有效成分提取工艺及含量测定方法

刘冬; 杜守颖; 何秀峰; 乐大勇; 李娜

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蟾酥中3种脂溶性有效成分提取工艺及含量测定方法

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- 蟾酥中3种脂溶性有效成分提取工艺及含量测定方法
- Study on Extraction and Determination Method of Three Liposoluble Effective Constituents in Bufons Venenum
- 中国实验方剂学杂志 2011年17卷第3期页码：69-72
- 作者机构：
- 作者简介：
- 基金信息：
  
  "重大新药创制"科技重大专项(2009ZX09502-008);"中药生产技术及过程控制技术标准平台"(2009ZX09308-003);教育部博士点基金(20090013110007)
- DOI：
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- 纸质出版日期：2011
- 稿件说明：
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刘冬, 杜守颖, 何秀峰, 等. 蟾酥中3种脂溶性有效成分提取工艺及含量测定方法[J]. 中国实验方剂学杂志, 2011,17(3):69-72.

LIU Dong, DU Shou-ying, HE Xiu-feng, et al. Study on Extraction and Determination Method of Three Liposoluble Effective Constituents in Bufons Venenum[J]. Chinese journal of experimental traditional medical formulae, 2011, 17(3): 69-72.
刘冬, 杜守颖, 何秀峰, 等. 蟾酥中3种脂溶性有效成分提取工艺及含量测定方法[J]. 中国实验方剂学杂志, 2011,17(3):69-72. DOI：

LIU Dong, DU Shou-ying, HE Xiu-feng, et al. Study on Extraction and Determination Method of Three Liposoluble Effective Constituents in Bufons Venenum[J]. Chinese journal of experimental traditional medical formulae, 2011, 17(3): 69-72. DOI：

摘要

目的 :优化蟾酥中脂溶性成分蟾毒灵、华蟾酥毒基及酯蟾毒配基的提取工艺

并建立了测定蟾酥提取物中上述3种成分含量的HPLC方法。方法 :以蟾酥中脂溶性成分蟾毒灵、华蟾酥毒基及酯蟾毒配基含量为指标

采用L9(34)正交试验对蟾酥提取工艺进行了优化;建立的HPLC法

Diamonsil-C18色谱柱(4.6 mm×250 mm

5 μm)

流动相乙腈-水(55:45)

流速1.0 mL ·min-1

检测波长296 nm。结果 :最佳提取工艺条件为A2B3C3D2

即75倍量95%乙醇80℃提取120 min;所建立的HPLC方法蟾毒灵、华蟾酥毒基及酯蟾毒配基均得到很好的分离

且重现性、精密度、线性关系良好

最小检测限分别为14.6

9.0

11.8 ng ·mL-1。结论 :确定了蟾酥最佳提取条件

HPLC能准确测定蟾酥提取物中蟾毒灵、华蟾酥毒基及酯蟾毒配基的含量

方法简便

结果准确。

Abstract

Objective: Study on extract method of liposoluble constituent bufalin

cinobufagin and resibufogenin in Bufons Venenum by orthogonal experiment design and established HPLC method for determination the assay of three effective constituents above. Method: An orthogonal test was adopted in this study. The content of bufalin

cinobufagin and resibufogenin was used as index for optimizing the extraction condition. In established HPLC method

the column:Diamonsil-C\-18 column(4.6 mm×250 mm

5 μm)

mobile phase:acetonitrile-water (55 ∶45)

the flow rate :1.0 mL·min-1

the detection wavelength 296 nm. Result: The best extraction technology was to extract for 120 min with 75 times 95% ethanol in 80 ℃. The calibration curves of bufalin

cinobufagin

resibufogenin were linear and LOD were 14.6

9.0

11.8 ng ·mL-1 respectively. The repeatability and precision of the HPLC method was good. Conclusion: Confirmed the best extract method and established HPLC method to determine the assay of three constituents in Bufons Venenum extraction was simple and accurate.

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