CN101744890A - Method for refining hypericin in hypericum perfortum extract - Google Patents
Method for refining hypericin in hypericum perfortum extract Download PDFInfo
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- CN101744890A CN101744890A CN200810204173A CN200810204173A CN101744890A CN 101744890 A CN101744890 A CN 101744890A CN 200810204173 A CN200810204173 A CN 200810204173A CN 200810204173 A CN200810204173 A CN 200810204173A CN 101744890 A CN101744890 A CN 101744890A
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Abstract
The invention takes a hypericum perfortum extract commonly sold in the market as a raw material of an extraction process and aims to provide a method for refining hypericin by using a biologically modified absorbing column. In the hypericum perfortum extract prepared by a preparation process of the invention and after HPLC detection, the content of the hypericin reaches over 50 percent; and the content of flavonoid, namely quereetin and rutoside reaches over 20 percent. The preparation method of the invention has the advantages of simple, convenient and quick operation; uniform and stable quality of the product, easy realization of production and accordance with industrialized production.
Description
(1) technical field
Involved in the present invention is that a kind of common Herba Hyperici perforati extract of being sold with existing market is a raw material, therefrom extract and obtain high-load hypericin hypericin and flavones ingredient, and the active method that can survey composition 〉=50%.
(2) background technology
Herba Hyperici perforati extract is one of product of favoring of the foreign vendor after Folium Ginkgo extract at present.Be used as the existing over one hundred year history of antidepressants abroad, and hypericin (hypericin) and flavone compound are antidepressant and main active antianxity in the Herba Hyperici perforati extract.Along with in the research of aspects such as antiviral, anticancer, antidepressant mechanism deeply, make it become current one of the research and development hot subject that compiles in recent years to Herba Hyperici perforati.For this reason, the extraction of active ingredients of Herba Hyperici perforati extract and purifying process also generally receive everybody concern.
At present domesticly mainly contain alcohol extracting method, aqueous alkali is carried.With ethanol is that solvent extraction hypericin (hypericin) is the method for comparison routine, but it is very big that hypericin in the extract (hypericin) content is influenced by extraction conditions, and the easy moisture absorption bonding of extract in bulk, by adding the hygroscopicity that cleaner, accent pH value etc. have solved product, but the content of hypericin in the product (hypericin) has only 0.7%, and hypericin is destroyed basically.If use means such as macroporous resin or solvent to make with extra care separation, though can obtain content higher effective component extract, cost is too high, and is consuming time quite long, is difficult to be accepted by market as common its production cost of extract dry powder.Report is also arranged, and in laboratory reason, hypericin content brings up to 28%, name but can't technology.So at domestic existing extract extraction process situation, necessity is improved existing preparation technology, the present invention is by effective method enrichment hypericin and flavones ingredient, makes hypericin content (hypericin) 〉=30%, can survey flavones ingredient 〉=20%.
(3) summary of the invention
The present invention is to be the extraction process raw material with the common Herba Hyperici perforati extract of selling on the market, and purpose is to provide a kind of method for refining hypericin of utilizing bio-modification.
The method of the refining hypericin of the present invention may further comprise the steps:
(1) take by weighing a certain amount of Herba Hyperici perforati extract, (10～20) doubly (1%～5%) diethanolamine aqueous solution of amount make dissolving, and solution filters by filter cloth (100～400 order), with this lucifuge.
(2) filtrate is passed through adsorption column (cht30) with certain flow velocity, then successively with (10～20) times water gaging, 0.1%～0.5% soda ash solution flushing adsorption column (cht30), the solution that elutes until soda is in trap≤0.3 at 350nm place, after the soda ash solution flushing finishes, add (10～20) doubly (70%～80%) alcoholic solution flushing pillar of amount (0.5%～1.5%) citric acid solution, (10～20) times water gaging, (15～30) times amount again successively again, discard eluent.
(3) doubly measure 0.5% diethanolamine ethanol (80% ethanol) eluant solution hypericin with (15～30), collect the hypericin eluent.
(4) hypericin eluent low temperature (＜45 ℃) vacuum concentration is concentrated into no ethanol flavor, and gained concentrated solution filtered while hot (first filter paper is after 0.45 μ m film) gets precipitate A.
(5) filtrate transfers to (1～2) with 18% hydrochloric acid ph value, separates out precipitation, and room temperature leaves standstill.It is centrifugal to wait to precipitate complete back, and discarded centrifugal supernatant gets deposit B.
(6) clean centrifugation B with distilled water, until neutrality.
(7) cleaned deposit B and precipitate A are put into vacuum drying oven, and 40 ℃ of vacuum dryings promptly obtain the hypericin finished product.
Adopt the Herba Hyperici perforati extract of prepared of the present invention, its hypericin content detects through HPLC and reaches more than 50%, and flavones ingredient Quercetin and rutin detect through HPLC and also reach more than 20% respectively.And the reagent that is used in the technology all is the conventional reagent of national regulation, is fit to suitability for industrialized production.
Use the Herba Hyperici perforati extract of the present invention's preparation and use the quality of the extract of additive method extraction to be compared as follows table:
(4) description of drawings
Adopted more intuitively process flow diagram to represent technical process of the present invention.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1:
Take by weighing Herba Hyperici perforati extract 500g, add 10L 5% diethanolamine aqueous solution and make dissolving, solution filters by 400 order filter clothes, filtrate is by the 4kgcht30 post, be about 40kg/h, 0.5% sodium carbonate liquor 150kg flow velocity with the 10L water flow velocity successively then and be about 23kg/h flushing cht30 post, after the soda ash solution flushing finishes, add the 80% alcoholic solution flushing pillar of 10kg 1.5% citric acid solution, 10L water, 14kg again successively again, discard eluent.With 20kg 0.5% diethanolamine 80% alcoholic solution eluting cht30 post, collect eluent.Eluent low temperature (＜45 ℃) vacuum concentration is concentrated into no ethanol flavor, and gained concentrated solution filtered while hot (first filter paper is after 0.45 μ m film) must precipitate. and filtrate transfers to 1 with 18% hydrochloric acid ph value, separates out precipitation, and room temperature leaves standstill.It is centrifugal to wait to precipitate complete back, discarded centrifuged supernatant, precipitation again.Merge precipitation, clean centrifugation with distilled water, until neutrality.Cleaned precipitation is put into vacuum drying oven, 40 ℃ of vacuum dryings promptly obtain hypericin extract 315.4g, and it is 51.6% that HPLC detects hypericin content, and rutin content is 26%, quercetin content is 3%, and detecting total flavones through ultraviolet spectrophotometry is 31%.
Embodiment 2:
Take by weighing Herba Hyperici perforati extract 500g, add 10L 5% diethanolamine aqueous solution and make dissolving, solution filters by 400 order filter clothes, filtrate is by the 5kgcht30 post, be about 36kg/h, 0.3% sodium carbonate liquor 180kg flow velocity with the 8L water flow velocity successively then and be about 25kg/h flushing cht30 post, after the soda ash solution flushing finishes, add the 80% alcoholic solution flushing pillar of 12kg 1.5% citric acid solution, 10L water, 15kg again successively again, discard eluent.With 18kg0.5% diethanolamine 80% alcoholic solution eluting cht30 post, collect eluent.Eluent low temperature (＜45 ℃) vacuum concentration is concentrated into no ethanol flavor, and gained concentrated solution filtered while hot (first filter paper is after 0.45 μ m film) must precipitate. and filtrate transfers to 1 with 18% hydrochloric acid ph value, separates out precipitation, and room temperature leaves standstill.It is centrifugal to wait to precipitate complete back, discarded centrifuged supernatant, precipitation again.Merge precipitation, clean centrifugation with distilled water, until neutrality.Cleaned precipitation is put into vacuum drying oven, 40 ℃ of vacuum dryings promptly obtain hypericin extract 357.3g, and it is 49.4% that HPLC detects hypericin content, and rutin content is 28%, quercetin content is 3.5%, and detecting total flavones through ultraviolet spectrophotometry is 32.5%.
Claims (7)
1. the preparation method of a Herba Hyperici perforati extract, be to be that raw material makes hypericin extract finished product by the following method with the common Herba Hyperici perforati extract of selling on the market, hypericin content 〉=30%, flavone can be surveyed composition Quercetin and rutin 〉=20%, its preparation method: Herba Hyperici perforati extract, a certain amount of diethanolamine aqueous solution makes dissolving, solution filters by filter cloth, filtrate is passed through adsorption column (cht30) with certain flow velocity, successively with water, soda ash solution flushing adsorption column (cht 30), after the soda ash solution flushing finishes, adding citric acid solution more successively again, water, alcoholic solution flushing pillar, discard eluent, 0.5% diethanolamine ethanol (80% ethanol) eluant solution hypericin is collected the hypericin eluent; Hypericin eluent low temperature (＜45 ℃) vacuum concentration is concentrated into no ethanol flavor, and gained concentrated solution filtered while hot (first filter paper is after 0.45 μ m film) must precipitate; Filtrate transfers to 1 with 18% hydrochloric acid pH value, separates out precipitation, and room temperature leaves standstill.It is centrifugal to wait to precipitate complete back, and discarded centrifugal supernatant must precipitate, and cleans centrifugation with distilled water, until neutrality, merges twice precipitation and puts into vacuum drying oven, and 40 ℃ of vacuum dryings promptly obtain the hypericin finished product.
2. it is characterized in that according to claim 1 is described: employed trapping agent model is (cht 30), and consumption is a Herba Hyperici perforati extract: (cht 30)=1: 1～1: 10.
3. according to claim 1, its preparation technology's feature is: Herba Hyperici perforati extract is doubly measured (1%～5%) diethanolamine aqueous solution with (10～20) and is made dissolving, and solution filters by yellow filter cloth (100～400 order).
4. according to claim 1, it is characterized in that: filtrate is passed through adsorption column (cht 30) with certain flow velocity, successively with (10～20) times water gaging, 0.1%～0.5% soda ash solution flushing adsorption column (cht 30), after the soda ash solution flushing finishes, add (10～20) doubly (70%～80%) alcoholic solution flushing pillar of amount (0.5%～1.5%) citric acid solution, (10～20) times water gaging, (15～30) times amount again successively again, discard eluent.
5. according to claim 1, it is characterized in that: doubly measure 0.5% diethanolamine ethanol (80% ethanol) eluant solution hypericin with (15～30), collect the hypericin eluent.
6. according to claim 1, it is characterized in that: filtrate transfers to (1～2) with 18% hydrochloric acid pH value, and employed hydrochloric acid solution is a mass ratio.
7. according to claim 1, it is characterized in that: the hypericin eluent concentrates and reclaims ethanol is criterion to there being the ethanol flavor, 30 ℃ all the time～45 ℃ of temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115872848A (en) * | 2022-12-27 | 2023-03-31 | 陕西嘉禾药业有限公司 | Method for preparing hypericin qualified in polycyclic aromatic hydrocarbon by using hypericum perforatum |
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| CN1198097A (en) * | 1995-09-29 | 1998-11-04 | 威廉施瓦布博士有限公司 | Stable extract of hypericum perforatum L., process for preparing the same and pharmaceutical compositions |
| CN1247071A (en) * | 1998-09-09 | 2000-03-15 | 中国科学院沈阳应用生态研究所 | Process for extracting high-content hypericin from Hypericum perforatum |
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- 2008-12-08 CN CN200810204173A patent/CN101744890A/en active Pending
Patent Citations (4)
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| CN1198097A (en) * | 1995-09-29 | 1998-11-04 | 威廉施瓦布博士有限公司 | Stable extract of hypericum perforatum L., process for preparing the same and pharmaceutical compositions |
| CN1304314A (en) * | 1998-06-10 | 2001-07-18 | 因迪纳有限公司 | Extracts of i(hypericum perforatum) and formulations containing them |
| CN1247071A (en) * | 1998-09-09 | 2000-03-15 | 中国科学院沈阳应用生态研究所 | Process for extracting high-content hypericin from Hypericum perforatum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115872848A (en) * | 2022-12-27 | 2023-03-31 | 陕西嘉禾药业有限公司 | Method for preparing hypericin qualified in polycyclic aromatic hydrocarbon by using hypericum perforatum |
| CN115872848B (en) * | 2022-12-27 | 2024-03-26 | 陕西嘉禾药业有限公司 | Method for preparing hypericin qualified by polycyclic aromatic hydrocarbon by using Hypericum perforatum |
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Application publication date: 20100623 |