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Extraction, separation and purification method of arctiin

A technique for separation and purification of arctiside, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of high equipment cost, unsuitability for industrialization, difficulty in large-scale production, etc., and achieves easy industrial production, The effect of low production cost and convenient operation

Inactive Publication Date: 2014-07-23
重庆化工职业学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for the extraction and separation and purification of arctiin, which solves the problems that the existing methods are difficult for large-scale production, and the cost of equipment is high and is not suitable for industrialization.

Method used

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  • Extraction, separation and purification method of arctiin

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Effect test

Embodiment 1

[0027] Take 10kg of crushed burdock fruit, put it into the extraction tank, add 60L of 70% ethanol and aqueous solution, reflux extraction 3 times for 3 hours each time, combine the extract, add 900g of activated carbon, stir and decolorize, filter, concentrate the filtrate to about 35L, add petroleum Ether: Ethyl acetate = 1:2 Stir about 4L to extract impurities, TLC monitoring (conditions: dichloromethane / methanol = 5:1, UV observation, product Rf value = 0.4), repeat extraction 6 times, discard the layer containing impurities . The remaining mother liquor was extracted arctiin with dichloromethane for 5 times, the extracts were combined, concentrated, dissolved in 3L of methanol, and 600ml of isopropyl ether was added for crystallization. About 300g of white crystals were obtained by suction filtration, and the arctiin content was tested to be >98%.

Embodiment 2

[0029] Take 5 kg of crushed burdock seeds, put them into an extraction tank, add 30 L of 95% ethanol and aqueous solution, reflux extraction 3 times for 3 hours each time, combine the extracts, add 450 g of activated carbon, stir to decolorize, filter, concentrate the filtrate to about 18 L, add petroleum Ether: Ethyl acetate = 1:3 Stir about 3L to extract impurities, TLC monitoring (conditions: dichloromethane / methanol = 5:1, UV observation, product Rf value = 0.4), repeat extraction 4 times, discard the layer containing impurities . The remaining mother liquor was extracted with dichloromethane to extract arctiin 8 times, the extracts were combined, concentrated, dissolved in 1.5L of methanol, and 300ml of isopropyl ether was added for crystallization. About 180g of white crystals were obtained by suction filtration, and the arctiin content was tested to be >98%.

Embodiment 3

[0031] Get 10kg of crushed burdock seeds, put it into an extraction tank, add 60L of 75% ethanol and aqueous solution by weight, reflux extraction 3 times for 3 hours each time, combine the extracts, add 900g of activated carbon (stir to decolorize, filter, concentrate the filtrate to about 30L, add petroleum Ether: Ethyl acetate = 1:1 Stir about 4L to extract impurities, TLC monitoring (conditions: dichloromethane / methanol = 5:1, UV observation, product Rf value = 0.4), repeat extraction 5 times, discard the layer containing impurities The remaining mother liquor is extracted with dichloromethane to extract arctiin, extract 8 times, combine the extracts, concentrate, dissolve with 3L of methanol, add 600ml of isopropyl ether to crystallize. Suction filtration obtains about 310g of white crystals, and the content of arctiin after testing > 98%.

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Abstract

The invention discloses an extraction, separation and purification method of arctiin. The method comprises the following steps: a) ethanol extraction, namely grinding arctium lappa, adding an ethanol solution which is preferably 5-10 times by weight, carrying out reflux extraction for three hours for two to three times and mixing the extracting solutions; b) activated carbon decoloration, namely adding activated carbon which accounts for 0.5% of the extracting solution by volume, carrying out reflux decoloration and carrying out filtration, thus obtaining a decoloration solution; c) concentration, namely recycling the decoloration solution at reduced pressure and enabling about 20% by volume of ethanol solution to be remained; d) impurity removal, namely adding a mixed solution of petroleum ether and ethyl acetate, stirring the solution and extracting the impurities and repeating the step four-six times; e) arctiin extraction, namely adding a dichloromethane to extract product and repeating the step five-eight times; f) concentration and crystallization, namely mixing dichloromethane extracting solutions containing products, concentrating the extracting solution, adding methanol to dissolve the concentrate and adding 20% by volume of isopropyl ether for crystallization, wherein the concentration of the ratio of ethanol to water is 70-95%; the ratio of petroleum ether to ethyl acetate is (1:1)-(1:3). The method has the beneficial effects that the method is convenient to operate, is low in production cost and easily achieves industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical product production, and relates to a method for extracting, separating and purifying arctiin. Background technique [0002] Arctiin belongs to lignans, and its structural formula is as follows figure 1 As shown, molecular formula: C27H34O11, molecular weight: 534.55226, CAS number: 20362-31-6, arctiin has anti-pancreatic cancer activity, and one of its mechanisms is to induce apoptosis. This product can cause blood vessels to dilate and blood pressure to drop; cause convulsions in cold-blooded and warm-blooded animals, cause respiratory failure in large doses, and cause skin redness and diarrhea in mice, and inhibit the isolated rabbit intestine and uterus. It has a paralyzing effect on motor nerves and bones, and can cause mild tail-raising reactions in mice. At the same time, it has anti-nephropathy effect, enhances the immune function of the body, has anti-complement activity, calcium antago...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 揭芳芳龚立覃仁辉贺小兰刘筱琴廖明佳马健
Owner 重庆化工职业学院
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