CN1242355A - Method for extracting total free anthraquinone from Chinese rhubarb - Google Patents
Method for extracting total free anthraquinone from Chinese rhubarb Download PDFInfo
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- CN1242355A CN1242355A CN 99114211 CN99114211A CN1242355A CN 1242355 A CN1242355 A CN 1242355A CN 99114211 CN99114211 CN 99114211 CN 99114211 A CN99114211 A CN 99114211A CN 1242355 A CN1242355 A CN 1242355A
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Abstract
The method for separating the rhubarb total free anthraquinones compounds from rhubarb extract includes the following steps: 1. adding acid in the rhubarb extract, heating to make hydrolysis, its optimized acid is hydrochloric acid; 2. adding alkali in the hydrolysate to regulate pH to 8-10; 3. making the alkalified hydrolysate pass through the anion-exchange resin separation column, removing effluent and water-washing to neutrality) 4. using potassium hydroxide-alcohol solution to make elution and collecting eluant; and 5. adding water in the eluant or no adding water, then distilling to remove alcohol, then adding acid to make precipitation to obtain the rhubarb total free anthraquinones, mainly including rheinlc acid, emodin, aloe-emodin, chrysophanol and emodin monomethyl ether.
Description
The present invention relates to a kind of method of extracting Radix Et Rhizoma Rhei total free anthraquinones.
From Radix Et Rhizoma Rhei extract, separate the existing report of Radix Et Rhizoma Rhei total free anthraquinones compounds [referring to " bulletin of Chinese materia medica " 12 (5), 1987, P286--288] at present.But this method formality is loaded down with trivial details, and the cost height is inflammable and explosive.
The purpose of this invention is to provide a kind of easier method of from Radix Et Rhizoma Rhei extract, separating the Radix Et Rhizoma Rhei total free anthraquinones compounds.
The objective of the invention is to be achieved through the following technical solutions.
A kind ofly isolate the method for Radix Et Rhizoma Rhei total free anthraquinones compounds from Radix Et Rhizoma Rhei extract, it is: (1) adds sour post-heating hydrolysis with Radix Et Rhizoma Rhei extract, and preferred acid is hydrochloric acid, and hydrolysis can be carried out under 40-70 ℃ of temperature, generally needs 0.5-2.5 hour.
(2) hydrolyzed solution with step (1) adds alkali adjusting pH to 8-10, and used alkali is sodium hydroxide or potassium hydroxide.
(3) anionite-exchange resin is soaked in water back dress post, elder generation's water is crossed post, alkali is crossed post then, is washed to neutrality, and post is crossed in acid again, be washed to neutrality, so alkaline purification, acid treatment repeat once to get the anionite-exchange resin separator column, and the hydrolyzed solution after the alkalization of step (2) is crossed the anionite-exchange resin separator column, discard effluent liquid, wash with water to neutrality, resin anion(R.A) is the weak anion exchange resin of big hole preferably.
(4) with the Radix Et Rhizoma Rhei total free anthraquinones compounds potassium hydroxide one alcoholic solution wash-out of step (3) upper prop, in elutriant, do not contain anthraquinone analog compound, collect elutriant.Potassium hydroxide one alcoholic solution can be methanol solution or ethanolic soln, can contain the water of 0-30% in methyl alcohol or the ethanol.
(5) after being added water or do not add water, the elutriant of step (4) boils off alcohol in the elutriant, add acid (preferably hydrochloric acid) then and be settled out total free rhubarb anthraquinone compound, filter collecting precipitation, wash with water to washings and be neutral, dry, promptly obtain the Radix Et Rhizoma Rhei total free anthraquinones compounds, include Schuttgelb, rhubarb yellow, rhabarberone, chrysophanol and rheochrysidin.
Used anionite-exchange resin separator column is through being washed to neutrality, and peracid is washed to and can repeats upper prop after the neutrality and separate the Radix Et Rhizoma Rhei total free anthraquinones compounds.
Separation method step of the present invention is simple, and separator column can be reused, and separation costs is low.
Embodiment 1
Get root, stem powder 200 grams of homemade sorrel, at room temperature soaked 8 hours with 50% ethanol 1000mL, filter, it is colourless that filter residue is washed till washings with 50% ethanol, merges washings and filtrate, and distillation is concentrated into 1/2 of original volume, promptly gets the rheum officinale concentrated extracting solution.
The ratio that adds 1 part of volume concentrated hydrochloric acid in 20 parts of extracting liquid volumes adds concentrated hydrochloric acid, and hydrolysis is 2.5 hours in 40 ℃ of water-baths, adds 5%KOH solution then and regulates pH to 9, filters, and filtrate is prepared upper prop.
Get 703 resins (big hole weak anion exchange resin), 400 grams that Shanghai Resin Factory produces, add water (distilled water, down together) after the immersion, (Φ 5 * 50cm), the about 600mL of resin volume for the glass chromatography column of packing into, cross post with 6000mL water, cross post with the NaOH solution of the 1mol/L concentration of 12000mL again, use the 6000mL water washing again, then cross post with the hydrochloric acid of 6000mL 1mol/L, repeat once above-mentioned NaOH-HCL treating processes, wash with 3000mL at last.
The above-mentioned excessively separator column of handling well of hydrolyzed solution with after the alkalization discards effluent liquid, is washed to neutrality, with the methanol solution wash-out of 1%KOH, being washed till does not have anthraquinone compounds, about 5000mL in the elutriant, collect washings, add water 1000mL, boil off and add hydrochloric acid behind the methyl alcohol and generate pale brown look precipitation, after precipitation is complete, filter, filter cake is washed till neutrality, gets pale brown look throw out, after the drying, get pale brown toner end, be free Radix Et Rhizoma Rhei anthraquinone, weigh 11.2 grams, through liquid-phase chromatographic analysis, wherein contain Schuttgelb 32%, rhubarb yellow 10%, rhabarberone 18%, chrysophanol 11%, rheochrysidin 20%.
Liquid-phase chromatographic analysis:
Chromatographic instrument: U.S. Waters company produces
Chromatographic column: Kromasil C
184.6 * 200mm (Sweden)
Moving phase: methyl alcohol: water: Glacial acetic acid: chloroform=80: 20: 0.5: 0.4 (V/V)
Detector: UV254nm
Retention time: rhabarberone 5.42min; Rhubarb yellow 7.37min; Schuttgelb 13.78min; Chrysophanol 20.68min; Rheochrysidin 33.02min.
Embodiment 2
Get the concentrated extracting solution as described roots and stems of rhubarb powder 200 grams of embodiment 1, add the ratio of 0.5 part of dense HCL of volume in 20 parts of filtrate volumes, hydrolysis is 1.5 hours in 50 ℃ of water-baths, adds 5%KOH solution then and regulates pH to 9.5, filters.Filtrate is crossed embodiment 1 described separator column, discard effluent liquid, be washed to neutrality, elutriant wash-outs of forming with 20 parts of volume 5%KOH aqueous solution and 80 parts of volume ethanol then do not have anthraquinone analog compound, about 5000mL to elutriant, collect elutriant, after boiling off ethanol, add hydrochloric acid and be settled out the Radix Et Rhizoma Rhei total free anthraquinones compounds, filter, filter cake is washed till neutrality, get pale brown toner end after the drying, be Radix Et Rhizoma Rhei total free anthraquinones, weigh 11.3 grams.Use liquid-phase chromatographic analysis, analytical results is identical with embodiment 1.
Embodiment 3
Get the concentrated extracting solution as described roots and stems of rhubarb powder 200 grams of embodiment 1, add the ratio of 1.5 parts of dense HCL of volume in 20 parts of filtrate volumes, hydrolysis is 0.5 hour in 70 ℃ of water-baths, adds 5%KOH solution then and regulates pH to 8.5, filters.Filtrate is crossed embodiment 1 described separator column, but 703 resins change 709 macroporous resins of Shanghai production of resins into, discard effluent liquid, be washed to neutrality, elutriant wash-outs of forming with 30 parts of volume 4%KOH aqueous solution and 70 parts of ethanol then do not have anthraquinone analog compound to elutriant, about 6000mL collects elutriant, after water-bath boils off ethanol, add hydrochloric acid and be settled out the Radix Et Rhizoma Rhei total free anthraquinones compounds, filter, filter cake is washed till neutrality, gets pale brown toner end after the drying, be free Radix Et Rhizoma Rhei anthraquinone, weigh 11.1 grams.Use liquid-phase chromatographic analysis, the result is identical with embodiment 1.
Claims (6)
1. isolate the method for Radix Et Rhizoma Rhei total free anthraquinones compounds from Radix Et Rhizoma Rhei extract for one kind, it is characterized in that:
(1) Radix Et Rhizoma Rhei extract is added sour post-heating hydrolysis,
(2) hydrolyzed solution is added alkali and regulates pH to 8-10,
(3) hydrolyzed solution after will alkalizing is crossed the anionite-exchange resin separator column, discards effluent liquid, wash with water to neutrality,
(4) with potassium hydroxide one alcoholic solution wash-out, collect elutriant,
(5) in elutriant, add water or do not add water after boil off alcohol, add Acid precipitation then and go out the Radix Et Rhizoma Rhei total free anthraquinones compounds, filter collecting precipitation.
2. separation method according to claim 1 is characterized in that described anionite-exchange resin is the macropore weak anion exchange resin.
3. separation method according to claim 1 is characterized in that described potassium hydroxide one alcoholic solution is the methanol solution or the ethanolic soln of potassium hydroxide.
4. according to claim 1 or 3 described separation methods, it is characterized in that the alcoholic solvent of described potassium hydroxide one alcoholic solution contains the water of 0-30%.
5. separation method according to claim 1 is characterized in that preferably hydrochloric acid of described acid.
6. separation method according to claim 1 is characterized in that described alkali is sodium hydroxide or potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114211 CN1242355A (en) | 1999-05-19 | 1999-05-19 | Method for extracting total free anthraquinone from Chinese rhubarb |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114211 CN1242355A (en) | 1999-05-19 | 1999-05-19 | Method for extracting total free anthraquinone from Chinese rhubarb |
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| Publication Number | Publication Date |
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| CN1242355A true CN1242355A (en) | 2000-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 99114211 Pending CN1242355A (en) | 1999-05-19 | 1999-05-19 | Method for extracting total free anthraquinone from Chinese rhubarb |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441557C (en) * | 2006-01-25 | 2008-12-10 | 北京盖雅环境科技有限公司 | Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis |
| CN100450990C (en) * | 2006-03-31 | 2009-01-14 | 江阴南极星生物制品有限公司 | Method for treating asphalt like slag in preparing rheinic acid and diacerein process with aloe |
| CN102188501A (en) * | 2011-04-29 | 2011-09-21 | 栗进才 | Rhubarb anthraquinones component extracting and separating method |
| CN101698638B (en) * | 2009-10-23 | 2012-09-19 | 中国科学院武汉植物园 | Method for extracting highly purified chrysophanic acid from roots and stems of rhubarb |
| CN101698637B (en) * | 2009-10-23 | 2012-10-03 | 中国科学院武汉植物园 | High-purity emodin separation method |
| CN105012283A (en) * | 2014-04-25 | 2015-11-04 | 西安世纪盛康药业有限公司 | Medicine composition containing parietic acid and pharmaceutical purpose of medicine composition |
-
1999
- 1999-05-19 CN CN 99114211 patent/CN1242355A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441557C (en) * | 2006-01-25 | 2008-12-10 | 北京盖雅环境科技有限公司 | Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis |
| CN100450990C (en) * | 2006-03-31 | 2009-01-14 | 江阴南极星生物制品有限公司 | Method for treating asphalt like slag in preparing rheinic acid and diacerein process with aloe |
| CN101698638B (en) * | 2009-10-23 | 2012-09-19 | 中国科学院武汉植物园 | Method for extracting highly purified chrysophanic acid from roots and stems of rhubarb |
| CN101698637B (en) * | 2009-10-23 | 2012-10-03 | 中国科学院武汉植物园 | High-purity emodin separation method |
| CN102188501A (en) * | 2011-04-29 | 2011-09-21 | 栗进才 | Rhubarb anthraquinones component extracting and separating method |
| CN105012283A (en) * | 2014-04-25 | 2015-11-04 | 西安世纪盛康药业有限公司 | Medicine composition containing parietic acid and pharmaceutical purpose of medicine composition |
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