Method for separating and preparing natural naphthoquinone compounds

A compound and separation method technology, applied in the field of medicine, can solve the problems of difficulty in simultaneous separation and time-consuming, and achieve the effects of simple operation and high compound purity.

Inactive Publication Date: 2017-09-12
FUDAN UNIV
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Problems solved by technology

Although it has been reported that naphthoquinone compounds, such as shikonin, β-hydroxyisovalerylshikonin, acetylshikonin, and isobutyrylshikonin, were isolated and purified from Sclerophylla sclerae by conventional HSCCC (Lu, et al, Journal of

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  • Method for separating and preparing natural naphthoquinone compounds
  • Method for separating and preparing natural naphthoquinone compounds
  • Method for separating and preparing natural naphthoquinone compounds

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Embodiment 1

[0042] (1) In this embodiment, the OptiChrome-300PLUS high-speed countercurrent chromatograph produced by Jiangyin Countercurrent Technology Co., Ltd. is improved, and the Agilent 1200HPLC high-performance liquid chromatograph produced by Agilent Co., Ltd. of the United States is used for purity analysis;

[0043] Set up a high-speed countercurrent chromatograph, in which, after the detector of the high-speed countercurrent chromatograph, flow valves a and b are connected, six-way valves a and b are respectively connected to storage rings I and II, and six-way valve c is connected in front of the constant flow pump, which is responsible for switching the normal washing Detachment mode and circulation elution mode, (the structure diagram of the high-speed countercurrent chromatograph of setting is as follows figure 1 shown);

[0044] (2) Preparation of extract samples

[0045] 54.8g of dried whole herb of Xinjiang comfrey was ultrasonically extracted three times with 500mL of ...

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Abstract

The present invention belongs to the technical field of medicine, and relates to a high-speed countercurrent chromatography continuous circulation method for separating and preparing naphthoquinone compounds from Arnebia euchroma (Royle) Johnst. According to the method, the natural naphthoquinone compounds represented by a formula (I) are separated and prepared by using a high-speed countercurrent chromatography continuous circulation separation method, n-hexane, ethyl acetate, acetonitrile and water are used as a two-phase solvent system for high-speed countercurrent chromatography separation, an online storage technology and a circulation elution mode are combined, the fractions containing the target compound are subjected to continuous circulation elution, and the fractions are collected to obtain shikonin with a purity of more than 95%, propionylshikonin with a purity of more than 95%, deoxyshikonin with a purity of more than 95%, (beta,beta-dimethylacryl)shikonin with a purity of more than 95% and isovalerylshikonin with a purity of more than 95%. With the method of the present invention, the high purity naphthoquinone compounds can be obtained through the one separation purification, such that the method has advantages of simple operation, rapidness and high efficiency, and is suitable for the separation and preparation of naphthoquinone and a variety of natural compounds. The formula (I) is defined in the specification.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for separating and preparing natural naphthoquinone compounds, in particular to preparing naphthoquinone compounds by adopting a high-speed countercurrent chromatography continuous circulation separation method. Background technique [0002] Arnebia euchroma (Royle) Johnst is a plant of the genus Arnebia euchroma (Royle) Johnst. Its dried roots are used as medicine and recorded in "Chinese Pharmacopoeia". ", listed as medium grade, sweet in the mouth, salty, cold in nature, GUIXIN, Liver Meridian. The traditional effects include clearing heat and cooling blood, promoting blood circulation, detoxifying and clearing rash. Chemical composition studies and modern pharmacological studies have shown that comfrey contains a variety of physiologically active components, which have been isolated from comfrey plants to naphthoquinones, benzoquinones, monoterpene phenol alkaloids, ...

Claims

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Application Information

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IPC IPC(8): C07C50/32C07C46/10C07C69/30C07C67/58
CPCC07C46/10C07C67/58C07C50/32C07C69/30
Inventor 何建明穆青张诗悦
Owner FUDAN UNIV
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