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Method for separating and purifying m-trihydroxybenzene compounds in Agrimonia polosa Ledeb

Active Publication Date: 2015-10-21
浙江赛默制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The difference between this patent and the present invention lies in: ① The polarity of the target compound is quite different
Crutchol has a single benzene ring structure and contains an unsaturated six-membered ring ketone, so it is more polar than other phloroglucinol compounds in Agrimony; The phloroglucinol compounds extracted from petroleum ether in Agrimony, which are weaker in polarity than craneol, could not be separated by aqueous system
[0007] We know that the phloroglucinol compounds in Agrimony are mostly phloroglucinol dicondensates and phloroglucinol tricondensates, and there are many homologues and isomers, and the polarity of these compounds is very weak (except craneol), the purpose of separation cannot be achieved by using the HSCCC conventional solvent system, which is a major technical problem in the separation of natural products

Method used

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  • Method for separating and purifying m-trihydroxybenzene compounds in Agrimonia polosa Ledeb
  • Method for separating and purifying m-trihydroxybenzene compounds in Agrimonia polosa Ledeb
  • Method for separating and purifying m-trihydroxybenzene compounds in Agrimonia polosa Ledeb

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Preparation of the crude extract of Agrimony: take 150g of Agrimony and crush it into a coarse powder, add 1500ml of petroleum ether (60-90°C), heat and reflux for extraction twice, each time for 1h; filter, combine the filtrates, recover the solvent and residue Add 50ml of chloroform to dissolve, shake and extract with 50ml of 5% sodium hydroxide, discard the chloroform solution, adjust the pH value of the sodium hydroxide solution to 1-2 with dilute hydrochloric acid, shake and extract twice with chloroform, combine the chloroform solution, and wash with water , discarded the aqueous solution, and concentrated the chloroform solution to obtain 310 mg of Agrimony crude extract. High performance liquid chromatography as figure 1 shown.

[0041] 2. The first high-speed countercurrent chromatographic separation: make n-hexane, acetonitrile, dichloromethane, and methanol into a solvent system in a volume ratio of 6:6:0.5:0.5, mix evenly, let stand to separate layers, a...

Embodiment 2

[0053] 1. Preparation of Agrimony Crude Extract: Steps are the same as in Example 1.

[0054] 2. The first high-speed countercurrent chromatographic separation: the solvent system is composed of n-hexane, acetonitrile and dichloromethane with a volume ratio of 5:5:0.5, the column temperature is set at 10°C, the rotation speed is 700rpm, and the flow rate of the mobile phase is 2mL / min, the 140-170 min eluate was collected in separate tubes at 8 min gradient time intervals, and the remaining steps of high-speed countercurrent chromatographic separation were the same as in Example 1.

[0055] 3. The second high-speed countercurrent chromatographic separation: the solvent system is composed of n-hexane, dichloromethane and acetonitrile with a volume ratio of 10:7:3. min, the remaining steps of high-speed countercurrent chromatographic separation are the same as in Example 1.

Embodiment 3

[0057] 1. Preparation of Agrimony Crude Extract: Steps are the same as in Example 1.

[0058] 2. The first high-speed countercurrent chromatographic separation: The solvent system is composed of petroleum ether, acetonitrile, dichloromethane and methanol with a volume ratio of 6:6:0.5:0.5. The column temperature is set at 20°C and the speed is 1000rpm. The flow rate was 5mL / min, and the eluate was collected in separate tubes at 3min gradient time intervals for 65-90min. The remaining steps of high-speed countercurrent chromatographic separation were the same as in Example 1.

[0059] 3. The second high-speed countercurrent chromatography separation: the solvent system is composed of n-hexane, dichloromethane and acetonitrile with a volume ratio of 10:7:3, the column temperature is set at 20°C, the rotation speed is 700rpm, and the flow rate of the mobile phase is 5mL / min, the remaining steps of high-speed countercurrent chromatographic separation are the same as in Example 1....

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Abstract

The present invention provides a method for separating and purifying m-trihydroxybenzene compounds in Agrimonia polosa Ledeb. The method is characterized in that a Agrimonia polosa Ledeb crude extract is taken and is subjected to two high-speed countercurrent chromatography purification treatments to obtain m-trihydroxybenzene compounds, wherein the solvent systems used by the two high-speed countercurrent chromatography purification treatments are anhydrous systems, the second separation adopts closed circuit 7-time circulating eluting, and finally pseudoaspidin with a purity of 95.2% and alpha-Kosin with a purity of 93.2% are separated. According to the present invention, the HSCCC anhydrous solvent system and the closed circuit method are firstly used to separate the m-trihydroxybenzene compounds in Agrimonia polosa Ledeb, the purity and the recovery rate of the obtained monomer are high, and the multiple homologs are separated in one time, such that the technical disadvantags of low separation efficiency, low yield, no safety, no environmental protection and the like of the use of the traditional separation technology are solved.

Description

technical field [0001] The invention relates to the field of natural organic chemistry, in particular to a method for separating and purifying Agrimony phloroglucinol compounds. Background technique [0002] Agrimonia polosa Ledeb is the dry aboveground part of Rosaceae plant Agrimonia polosa Ledeb. It has the functions of astringent and hemostasis, cutting off malaria, stopping dysentery, detoxification, and tonifying deficiency. It is used to treat hemoptysis, hematemesis, metrorrhagia, and malaria , bloody dysentery, carbuncle sore, vaginal itching leukorrhea, fatigue and so on. Modern pharmacological research has found that Agrimony has various activities such as anti-tumor, lowering blood sugar, lowering blood pressure, and anti-oxidation. It is a natural medicinal material that has a significant health care effect on humans. [0003] The whole herb of Agrimony contains a variety of chemical components, such as agrimonin, tannic acid, volatile oil, sterols, organic aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/79C07C49/84
Inventor 唐岚单伟光傅璐璐卢程华李成平
Owner 浙江赛默制药有限公司
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