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Method for separating chrysophanol and physcion by silica-gel column chromatography

A technology of emodin methyl ether and silica gel column chromatography, which is applied in the fields of quinone separation/purification, anti-toxins, blood diseases, etc., can solve the problems that cannot meet the requirements of pharmacological activity screening and clinical application, and achieve the benefits of labor protection and Environmental protection, simplified process route, easy operation, and good separation effect

Active Publication Date: 2012-06-06
雷允上药业集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for separating chrysophanol and emodin methyl ether by silica gel column chromatography, to overcome the shortcomings of the existing production process for separating chrysophanol and emodin methyl ether, and to be unable to meet the screening and clinical application of pharmacological activity The defect of demand is a production process with simple process and suitable for industrial mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation of embodiment 1 chrysophanol and emodin methyl ether mixture

[0018] Take 15 kg of rhubarb powder, add 10 times the amount of 20% sulfuric acid, heat on a water bath for 3 hours, filter, wash the filter cake with water until it is nearly neutral, and then dry it at 70°C. Take the dried powder and heat reflux with ethyl acetate for several times to extract the total free anthraquinones, recover the ethyl acetate liquid to obtain 580 g of total free anthraquinones, dissolve it with acetone, mix it with 600 grams of silica gel (100-200 mesh) as a sample, Evaporate the solvent to dryness on a rotary evaporator, take it out, dry it at 60°C, grind it finely, pass it through an 80-mesh sieve, put it on a short and thick silica gel column (1.2kg silica gel, 100-200 mesh, dry-packed column), and quickly elute with chloroform. Chloroform was reclaimed to obtain 230 grams of chrysophanol and emodin methyl ether mixture. Product analysis uses Shimadzu high perform...

Embodiment 2

[0019] The atmospheric pressure silica gel column chromatography separation of embodiment 2 chrysophanol and emodin methyl ether

[0020] Take 50 grams of the mixture of chrysophanol and emodin methyl ether prepared in Example 1, dissolve it in chloroform, mix it with 50 grams of silica gel (100-200 mesh), evaporate the solvent to dryness on a rotary evaporator, take it out, and dry it at 60°C , grind finely, pass 80 mesh, and set aside. Take another 2kg of 200-300 mesh silica gel, stir well with petroleum ether (60-90°), remove air bubbles, then wet-pack the column, elute with petroleum ether (60-90°) to balance, load the sample, and wash with petroleum ether first. Depolarize impurities less than chrysophanol, then use petroleum ether (60-90°) / butyl acetate, the ratio is 100 / 0.5-30 / 1 gradient elution, silica gel thin layer chromatography tracking detection, developing agent is petroleum ether (60~90°): butyl acetate (20:1), inspected under sunlight, the same fractions were ...

Embodiment 3

[0021] The low-pressure silica gel column chromatography separation of embodiment 3 chrysophanol and emodin methyl ether

[0022] Take 10 grams of the mixture of chrysophanol and emodin methyl ether prepared in Example 1, dissolve it in chloroform, mix the sample with 10 grams of silica gel (200-300 mesh), evaporate the solvent to dryness on a rotary evaporator, take it out, and dry it at 60°C , ground finely, passed through a 100-mesh sieve, and set aside. Take another 500g of silica gel H, stir with petroleum ether (60-90°) evenly, remove air bubbles and then wet-pack the column, elute with petroleum ether (60-90°) to balance, load the sample, add liquid ball to elute Liquid, pressurized with a nitrogen cylinder, the pressure is 2 ~ 3kPa, first use petroleum ether to elute impurities less polar than chrysophanol, and then use petroleum ether (60 ~ 90°) / butyl acetate, the ratio is 100 / 1 ~ 20 / 1 gradient elution, silica gel thin-layer chromatography tracking detection, devel...

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Abstract

The invention discloses a method for separating chrysophanol and physcion by silica-gel column chromatography, comprising the following steps of: filling a column with silica gel, or taking commodity,namely silica gel filled column, using a solvent to dissolve a sample of a mixture containing chrysophanol and physcion, stirring the sample with the silica gel, drying the solvent, then sampling, orusing a low-polarity solvent to dissolve and directly adding the sample, firstly using petroleum ether to elute impurities with the polarity of less than that of chrysophanol under proper pressure, using petroleum ether / butyl acetate with the proportion of 100 / 0.1 to 10 / 1 to elute chrysophanol and physcion, carrying out tracking and detection by thin-layer chromatography, combining same fractions, separating in sequence to obtain the chrysophanol and physcion, carrying out crystallization and recrystallization respectively and obtaining the pure product. The method has large sample-carrying amount and high separating efficiency; the adopted eluting agent is safe and environment-friendly, can be recycled and reused repeatedly, has low cost, not only is applicable to preparation with littleamount in a testing laboratory, but also can realize industrial production on large scale; and the obtained chrysophanol and physcion have the purity of more than 99 percent respectively, can be usedas chemical reference substances in traditional Chinese medicine or are applied as raw material of medicine and chemical industry.

Description

technical field [0001] The invention relates to the extraction and separation of Chinese herbal medicine components, more specifically to a separation method of high-purity chrysophanol and emodin methyl ether. Background technique [0002] Chrysophanol and emodin methyl ether belong to anthraquinone compounds, which are two active ingredients naturally present in many traditional Chinese medicines, such as rhubarb, knotweed, cassia seed, Polygonum multiflorum and other traditional Chinese medicines all contain these two free anthraquinone aglycones or sugar Conjugated anthraquinone glycosides. Chrysophanol has the effect of hemostasis and anti-aging, and also has anti-AlCl 3 The protective effect of memory impairment induced by acute aging mice, and the effect of resisting normal pressure hypoxia, acute cerebral hypoxia and improving body endurance. Chrysophanol can be oxidized to make rhein, and then acetylated to make diacerein, which is an important drug raw material f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/34C07C46/10A61P7/04A61P39/06A61P35/00
Inventor 周一君杨增石荣火卢扬陆荣
Owner 雷允上药业集团有限公司
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