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High-performance liquid chromatographic method for separating [Separate sth. from sth.]tripdiolide from 2-epitripdiolide

A high-performance liquid chromatography and triptolide technology, applied in the chemical field, can solve problems such as poor reproducibility, solvent consumption, and difficult separation, and achieve the effect of high repeatability and low cost

Active Publication Date: 2018-07-24
绍兴市逸晨医疗科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This makes the separation of these four compounds very difficult
The prior art relies on repeated silica gel column chromatography when separating these four compounds. However, repeated silica gel column chromatography consumes solvent and has poor reproducibility. It is only suitable for a small amount of separation in the laboratory and is difficult to promote in industrial production.

Method used

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  • High-performance liquid chromatographic method for separating [Separate sth. from sth.]tripdiolide from 2-epitripdiolide
  • High-performance liquid chromatographic method for separating [Separate sth. from sth.]tripdiolide from 2-epitripdiolide
  • High-performance liquid chromatographic method for separating [Separate sth. from sth.]tripdiolide from 2-epitripdiolide

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Embodiment Construction

[0074] The following describes the substantive content of the present invention in detail in conjunction with the drawings and embodiments, but does not limit the protection scope of the present invention.

[0075] 1. Experimental materials

[0076] The dried roots of Tripterygium wilfordii were purchased from the Bozhou Chinese medicinal materials market, and were identified as the dried roots of Tripterygium wilfordii of the Euonymus family;

[0077] XDA-1B macroporous adsorption resin was purchased from Zhengzhou Qinshi Technology Co., Ltd.;

[0078] DM130 macroporous adsorption resin was purchased from Anhui Sanxing Resin Technology Co., Ltd.;

[0079] 95% ethanol, triethylamine, ethyl acetate, n-butanol, ammonia water and hydrochloric acid were purchased from Nanjing Chemical Reagent Co., Ltd.;

[0080] TBE-300C high-speed countercurrent chromatograph, Shanghai Tongtian Biotechnology Co., Ltd.

[0081] 2. Experimental method

[0082] A method for preparing triptolide ...

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Abstract

The invention discloses a high-performance liquid chromatographic method for separating tripdiolide from 2-epitripdiolide. Triptonide, triptolide, tripdiolide and 2-epitripdiolide in tripterygium wilfordii are very close in structure, wherein the tripdiolide and the 2-epitripdiolide are a pair of chiral isomers, and are large in separation difficulty. The prior arts are all dependent on repeated silica-gel column chromatography when the four compounds are separated, but the repeated silica-gel column chromatography consumes a solvent, is poor in reproducibility and is difficult to be promotedin industrial production. In the prior industrial production, the only column chromatography which is being used is macroporous resin. The method provided by the invention can realize separated preparation of the triptonide, the triptolide, the tripdiolide and the 2-epitripdiolide in tripterygium wilfordii without dependence on the repeated silica-gel column chromatography. The HPLC method disclosed by the invention has the beneficial effects that on the basis of the conventional C18 chromatographic column, the chiral isomers (the tripdiolide and the 2-epitripdiolide) can be effectively separated, so that the cost is low and the repeatability is high.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a preparation method and a separation and analysis method of known compounds, in particular to a method for preparing triptolide ketone, triptolide, triptolide and 2-epitriptolide and triptolide The HPLC separation and analysis method of B and 2-epitriptolide. Background technique [0002] Studies have found that four chemical components with very similar structures in Triptolide have excellent anti-tumor activity, namely: triptolide ketone, triptolide, triptolide and 2-epitriptolide. The structural formula is as follows: [0003] [0004] From the chemical structure, it can be found that the structures of these four compounds are very close, wherein triptolide and 2-epitriptolide are a pair of chiral isomers. This makes the separation of these four compounds very difficult. The prior art relies on repeated silica gel column chromatography when separating these four compounds. Howeve...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 赖旭宇
Owner 绍兴市逸晨医疗科技有限公司
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