CN102311330A - Method for extracting agrimophol from hairyvein agrimony - Google Patents

Abstract

The invention provides a method for extracting agrimophol from hairyvein agrimony, which comprises the following steps: 1) crushing hairyvein agrimony medicinal materials, adding a 60-90% ethanol solution with an amount being 5-10 times of the material amount, performing refluxing and extraction for 2-3 times, decoloring the extract by active carbon, filtering, performing reduced pressure concentration to obtain an alcohol concentration of 20-40% so as to obtain a concentrate; 2) adding the concentrate into a macroporous resin column for adsorption, washing with water to obtain a sugar-free color, performing elution with 4-5BV70-80% ethanol, collecting the eluate, performing reduced pressure concentration, extracting the concentrate by chloroform, recovering the solvent of the extract to obtain a crude extract; 3) performing crystallization of the crude extract by petroleum ether and ethanol orderly, and drying the crystalline material. The method has simple process steps and operations, and low production cost, and is applicable to industrial production.

Description

A kind of method of from Herba Agrimoniae, extracting Agrimopholum

Technical field

The present invention relates to from a kind of Herba Agrimoniae, extract the method for Agrimopholum, especially relate to a kind of method that adopts the macroporous resin purification Agrimopholum.

Background technology

Agrimopholum (Agrimophol) be Agrimophol again, is a kind of Phloroglucinol compounds, CAS 65792-05-4 molecular formula C ₂₆H ₃₄O ₈, molecular weight 474.55, molecular structural formula:

Agrimopholum, faint yellow crystallization, fusing point 138.5-139.5 ℃.Be soluble in chloroform, benzene, be slightly soluble in methyl alcohol, ethanol, meet iron trichloride and be brown, meet the vitriol oil and be orange red.Agrimopholum all has definite insecticidal action to taeniasis suis, cysticercus, larva, Mohs tapeworm and Diplacanthus nanus.

Herba Agrimoniae is that Rosaceae Rosaceae Agrimony belongs to the Agrimonia plant; Cry Bud of hairyvein agrimony, Radix Agrimoniae again, execute the state Radix Agrimoniae, melon vanilla, Huanglong's tail etc.; Herb contains agrimonine, agrimonolide, tannin (for Jiao's property catechol tannin, gallotannin etc.), sterol, organic acid, phenolic constituent, saponin etc., has hemostasis, desinsection, antitumor action.

From Herba Agrimoniae, extract the method for Agrimopholum, milk of lime process and sherwood oil method are arranged, also adopt supercritical CO ₂Extraction process obtains crude extract silicagel column separation again.Because Agrimopholum content is lower in the medicinal material, volatile organic large usage quantity causes very big potential safety hazard, and cost is higher.

Summary of the invention:

The object of the invention overcomes the deficiency of prior art, and the method for extracting Agrimopholum in a kind of Herba Agrimoniae is provided, and this method is simple to operate, and production cost is lower.

The objective of the invention is to realize through following technical scheme:

A kind of method of from Herba Agrimoniae, extracting Agrimopholum is characterized in that comprising following steps:

1) get the Herba Agrimoniae pulverizing medicinal materials, add 5-10 and doubly measure 60-90% ethanolic soln refluxing extraction 2-3 time, extracting solution adds activated carbon decolorizing, filters, and is decompressed to determining alcohol 20-40%, gets liquid concentrator;

2) with the absorption of above-mentioned liquid concentrator adding macroporous resin column, washing is got the 4-5BV70-80% ethanol elution to there not being fried sugar, collects the elutriant concentrating under reduced pressure, and liquid concentrator is used chloroform extraction, and extraction liquid reclaims reagent, gets crude extract;

3) above-mentioned crude extract is used sherwood oil, alcohol crystal successively, crystallisate is drying to obtain.

Said step 2) a kind of among the optional AB-8 of macroporous resin, HZ816, HPD-100 and the D101.

Advantage of the present invention is: method adopts the macroporous resin adsorption enrichment, and simple to operate, treatment capacity is big, has simplified pre-treatment, has saved the consumption of follow-up sherwood oil and chloroform, reduces potential safety hazard and production cost; This law also adopts low alcohol to go up macroporous resin, solves Agrimopholum and separates out a difficult problem that is difficult for upper prop, also reduces the absorption of impurity, is beneficial to follow-up purifying.

 

To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.

Embodiment:

Embodiment 1:

Get the Herba Agrimoniae pulverizing medicinal materials, get 10kg, add 8 times of amount 60% ethanolic soln refluxing extraction 2 times, extracting solution added the 1kg activated carbon decolorizing 1 hour; Filter, be decompressed to determining alcohol 30%, add the absorption of 5L AB-8 macroporous resin column, washing is to there not being fried sugar; Get the 20L80% ethanol elution, collect elutriant and be evaporated to 500ml, pour separating funnel into and add the equal-volume chloroform extraction 3 times; Collect extraction liquid and reclaim reagent, crude extract 30g, use sherwood oil, alcohol reflux dissolving crystallized successively; Drying obtains yellowish crystallization 500mg, detects content 91.1% through HPLC.

Embodiment 2:

Get the Herba Agrimoniae pulverizing medicinal materials, get 10kg, add 6 times of amount 90% ethanolic soln refluxing extraction 3 times, extracting solution added the 2kg activated carbon decolorizing 1 hour; Filter, be decompressed to determining alcohol 40%, add the absorption of 5L HZ816 macroporous resin column, washing is to there not being fried sugar; Get the 25L70% ethanol elution, collect elutriant and be evaporated to 400ml, pour separating funnel into and add the equal-volume chloroform extraction 3 times; Collect extraction liquid and reclaim reagent, crude extract 24g, use sherwood oil, 99% alcohol reflux dissolving crystallized successively; Drying obtains yellowish crystallization 620mg, detects content 92.3% through HPLC.

Embodiment 3:

Get the Herba Agrimoniae pulverizing medicinal materials, get 10kg, add 6 times of amount 80% ethanolic soln refluxing extraction 3 times, extracting solution added the 2kg activated carbon decolorizing 1 hour; Filter, be decompressed to determining alcohol 20%, add the absorption of 5L HPD-100 macroporous resin column, washing is to there not being fried sugar; Get the 25L70% ethanol elution, collect elutriant and be evaporated to 400ml, pour separating funnel into and add the equal-volume chloroform extraction 3 times; Collect extraction liquid and reclaim reagent, crude extract 35g, use sherwood oil, 90% alcohol reflux dissolving crystallized successively; Drying obtains yellowish crystallization 540mg, detects content 90.3% through HPLC.

Embodiment 4:

Get the Herba Agrimoniae pulverizing medicinal materials, get 10kg, add 8 times of amount 80% ethanolic soln refluxing extraction 2 times, extracting solution added the 1.5kg activated carbon decolorizing 2 hours; Filter, be decompressed to determining alcohol 35%, add the absorption of 5L D101 macroporous resin column, washing is to there not being fried sugar; Get the 20L75% ethanol elution, collect elutriant and be evaporated to 300ml, pour separating funnel into and add the equal-volume chloroform extraction 3 times; Collect extraction liquid and reclaim reagent, crude extract 32g, use sherwood oil, 95% alcohol reflux dissolving crystallized successively; Drying obtains yellowish crystallization 560mg, detects content 90.5% through HPLC.

Claims (2)

1. method of from Herba Agrimoniae, extracting Agrimopholum is characterized in that comprising following steps:

1) get the Herba Agrimoniae pulverizing medicinal materials, add 5-10 and doubly measure 60-90% ethanolic soln refluxing extraction 2-3 time, extracting solution adds activated carbon decolorizing, filters, and is decompressed to determining alcohol 20-40%, gets liquid concentrator;

2) with the absorption of above-mentioned liquid concentrator adding macroporous resin column, washing is got 4-5BV 70-80% ethanol elution to there not being fried sugar, collects the elutriant concentrating under reduced pressure, and liquid concentrator is used chloroform extraction, and extraction liquid reclaims reagent, gets crude extract;

3) above-mentioned crude extract is used sherwood oil, alcohol crystal successively, crystallisate is drying to obtain.

2. from Herba Agrimoniae, extract the method for Agrimopholum according to claim 1, it is characterized in that said step 2) in a kind of among the optional AB-8 of macroporous resin, HZ816, HPD-100 and the D101.