CN101829164B - Biological preparation method of Hypericum perforatum L extractive - Google Patents
Biological preparation method of Hypericum perforatum L extractive Download PDFInfo
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- CN101829164B CN101829164B CN2010101654828A CN201010165482A CN101829164B CN 101829164 B CN101829164 B CN 101829164B CN 2010101654828 A CN2010101654828 A CN 2010101654828A CN 201010165482 A CN201010165482 A CN 201010165482A CN 101829164 B CN101829164 B CN 101829164B
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Abstract
The invention relates to a biological preparation method of a Hypericum perforatum L extractive, providing a preparation method which can utilize medicinal material resources adequately, has simple process, is suitable for large-scale production and can prepare the Hypericum perforatum L extractive in accordance with or higher than international standards. The method comprises the following steps of: drying the Hypericum perforatum L firstly and smashing into Hypericum perforatum L powder, then weighing enzyme, adding warm water in the enzyme to dissolve the enzyme, activating enzyme solution by water bath, mixing the Hypericum perforatum L powder with water, performing water bath, soaking, cooling, adjusting pH with hydrochloric acid, stirirng uniformly, heating by water bath, adding the actived enzyme solution, mixing uniformly, performing enzymolysis, filtering, abandoning the filter to obtain medicinal material powder after enzymolysis, adding ethanol and fluxing for extraction, filtering, combining the filtrate, condensing under reduced pressure, recycling ethanol, and drying to obtain the Hypericum perforatum L extractive. The invention improves the content of hypericin in the extractive and the abandoned filtrate after enzymolysis takes away a large amount of water-soluble impurities so that the moisture of the extractive is not needed to absorb again. The biological method is safe, pollution free and has simple operation and is easy for industrialized application.
Description
One, technical field
The present invention relates to field of medicaments, particularly a kind of biological preparation method of Herba Hyperici perforati extract.
Two, background technology
Hypericin (the hypericin that contains in the Herba Hyperici perforati (Hypericum Perforatum L.), chemistry is by name: 4,4,5,5,7,7-hexahydroxy-2,2-dimethyl-meta-meso-naphthadianthrene ketone) have superior bioactive, as antidepressant, antiviral, anticancer and photo-activity, especially depression and the nervous a series of neurological disorder diseases such as subhealth symptom that cause there are good elimination effect, paid attention to by international the world of medicine.The international market needs to increase day by day to Herba Hyperici perforati extract, also stimulated China in recent years to the production of Herba Hyperici perforati extract.
But the content of hypericin has only ten thousand in the Herba Hyperici perforati herb/and several, therefore, how preparing qualified (American Pharmacopeia 24 editions and extract are imported and exported standard and stipulated that all content 0.3% is for qualified) even the higher extract of hypericin content from the Herba Hyperici perforati herb is the focus of related scientific research and production unit research.
At present domestic extracting method commonly used mainly contains: 1, methanol or ethanol extraction method: with Herba Hyperici perforati herb drying, pulverize after, make solvent with ethanol or methanol, reflux, extract, repeatedly, merge extractive liquid, also concentrates, and obtains hypericin extractum.The shortcoming that there is easy moisture absorption in the product that obtains in this way, be clamminess (time precious traditional Chinese medical science traditional Chinese medicines .2009,20 (2), 404～405).
2, alkali liquor extraction method: Chinese patent 98114299.0 discloses a kind of extracting method of hypericin: the Herba Hyperici perforati medical material adds the NaOH solution that concentration is 0.01-1%, heated and boiled 8-15 minute, after filtration stand-by filtrate; Slag adds the consumption of 1/2-1/3 of the NaOH solution of above-mentioned same concentration, through heated and boiled 8-12 minute, filters to get filtrate, merging filtrate, hydrochloric acid is transferred pH to 1-5, and is extremely colourless substantially with ethanol elution then, reclaim the ethanol after drying and get finished product, hypericin content 0.48-0.66%.As everyone knows, the shortcoming that alkali liquor extracts is that extract obtained color and luster is relatively poor, and has a large amount of NaCl to carry secretly wherein in the product, for purification brings many inconvenience.
3, organic solvent extraction-adsorbing material enriching and purifying method: Chinese patent 200610078988.9 discloses a kind of extracting method of hypericin: the Herba Hyperici perforati ethanol extraction, filtrate decompression concentrates, concentrated solution adsorbs with resin, eluting, collect eluent, concentrating under reduced pressure obtains hypericin extractum, the product that this method obtains contains higher hypericin, but technology relative complex, cost is higher, and the resin of absorption usefulness belongs to the macromolecular compound of chemosynthesis, wherein contain not synthetic chemical monomer, as benzene, divinylbenzene, toluene, organic residues such as dimethylbenzene, be not easy for food and take, because State Food and Drug Administration is to health food of producing with the macroporous adsorbent resin separation and purification and the regulation that strictness is arranged with the organic residue in the raw material of styrene matrix type resins, therefore, the method of purification with macroreticular resin Herba Hyperici perforati extract is restricted to a great extent, be difficult to reach the requirement of industrialized great production, mainly still rest on laboratory stage at present.
Because the effective ingredient in the plant is present in the plant cell usually, adopting the enzyme enzymolysis to destroy cell wall can impel the effective ingredient stripping to increase, thereby active constituent content in the raising extract, improve the utilization rate of medical material, but do not see the application of open report enzymolysis in the Herba Hyperici perforati extract preparation up to now as yet.
Three, summary of the invention
At above-mentioned situation, for overcoming the prior art defective, the present invention's purpose will provide a kind of exactly can make full use of herb resource, simple, the suitable large-scale production of technology, and can prepare the preparation method of the Herba Hyperici perforati extract that meets or be higher than current international practice standard.
The technical scheme that the present invention solves is, earlier with the Herba Hyperici perforati drying, be ground into the Herba Hyperici perforati powder, take by weighing 0.5%～2.5% enzyme of Herba Hyperici perforati powder weight again, 30～60 ℃ of warm water that the 10-20 of adding enzyme weight doubly measures in enzyme, dissolving, 30～60 ℃ of water-baths activate 5～30 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder mixes with 1: 10～20 weight ratio with water, and 40～90 ℃ of water-baths were soaked 20～90 minutes, be cooled to 18～25 ℃, transfer pH to 4.0～5.5 with hydrochloric acid, shake up, heating in water bath to 40～55 ℃, add above-mentioned activatory enzymatic solution, mixing, enzymolysis 2～12 hours, sucking filtration, discard filtrate, medicinal powder behind the enzymolysis, add the alcohol reflux 2～5 times of 6～20 times of amounts of the medicinal powder weight behind the enzymolysis in the medicinal powder behind enzymolysis, each 1～5 hour, filter, merging filtrate, 50～60 ℃ of concentrating under reduced pressure reclaim ethanol, drying gets Herba Hyperici perforati extract; Said enzyme is one or more the mixing among cellulase, pectase, xylanase, 1,4 beta-glucanase, the compound enzyme SPE-007A etc.
The present invention extracts after utilizing the biological preparation enzyme with Herba Hyperici perforati medical material enzymolysis, this process has not only improved the utilization rate of Herba Hyperici perforati medical material greatly, improved hypericin content in the extract, hypericin content employing reversed-phase high-performance liquid chromatography method detects and can reach 0.68%-0.81% in the gained finished product, and the filtrate that discards behind the enzymolysis has been taken away a large amount of water-solubility impurities, make no longer moisture absorption of extract, used biological method safety non-pollution, operation is simple and feasible, is easy to carry out industrial applications.
Four, the specific embodiment
Below in conjunction with practical situation the specific embodiment of the present invention is elaborated.
Embodiment 1:
With the Herba Hyperici perforati drying, pulverize 20 mesh sieves earlier, became the Herba Hyperici perforati powder, took by weighing Herba Hyperici perforati powder 1kg, took by weighing the cellulase of 5g again, in cellulase, added 32 ℃ of warm water of 50g, dissolving, 32 ℃ of water-baths activate 28 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder adds water 10000g and mixes, and 40 ℃ of water-baths were soaked 90 minutes, be cooled to 18 ℃, transfer pH to 5.3, shake up with hydrochloric acid, heating in water bath to 55 ℃ adds above-mentioned activatory enzymatic solution, mixing, enzymolysis 2 hours, sucking filtration discards filtrate, medicinal powder behind the enzymolysis, the alcohol reflux of 6 times of amounts of the medicinal powder weight in the medicinal powder behind enzymolysis behind the adding enzymolysis 3 times each 3 hours, filters, merging filtrate, 50 ℃ of concentrating under reduced pressure reclaim ethanol, drying, get Herba Hyperici perforati extract, yield is 8.51%, detects with known reversed-phase high-performance liquid chromatography method, and the content that records hypericin in the Herba Hyperici perforati extract is 0.73%.
Embodiment 2:
With the Herba Hyperici perforati drying, pulverize 20 mesh sieves earlier, became the Herba Hyperici perforati powder, took by weighing Herba Hyperici perforati powder 2kg, took by weighing pectase 30g again, in pectase, added 45 ℃ of warm water of 450g, dissolving, 45 ℃ of water-baths activate 20 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder adds water 30000g and mixes, and 70 ℃ of water-baths were soaked 50 minutes, be cooled to 20 ℃, transfer pH to 4, shake up with hydrochloric acid, heating in water bath to 47 ℃ adds above-mentioned activatory enzymatic solution, mixing, enzymolysis 5 hours, sucking filtration discards filtrate, medicinal powder behind the enzymolysis, the alcohol reflux of 13 times of amounts of the medicinal powder weight in the medicinal powder behind enzymolysis behind the adding enzymolysis 2 times each 1.5 hours, filters, merging filtrate, 60 ℃ of concentrating under reduced pressure reclaim ethanol, drying, get Herba Hyperici perforati extract, yield is 8.16%, detects with known reversed-phase high-performance liquid chromatography method, and the content that records hypericin in the Herba Hyperici perforati extract is 0.68%.
Embodiment 3:
With the Herba Hyperici perforati drying, pulverize 20 mesh sieves earlier, became the Herba Hyperici perforati powder, took by weighing Herba Hyperici perforati powder 3kg, took by weighing xylanase 75g again, in xylanase, added 58 ℃ of warm water of 1500g, dissolving, 58 ℃ of water-baths activate 8 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder adds water 60000g and mixes, and 90 ℃ of water-baths were soaked 20 minutes, be cooled to 25 ℃, transfer pH to 4.5, heating in water bath to 40 ℃ with hydrochloric acid, add above-mentioned activatory enzymatic solution, mixing, enzymolysis 11 hours, sucking filtration, discard filtrate, medicinal powder behind the enzymolysis, add the alcohol reflux 5 times of 20 times of amounts of the medicinal powder weight behind the enzymolysis in the medicinal powder behind enzymolysis, each 5 hours, filter merging filtrate, 55 ℃ of concentrating under reduced pressure, reclaim ethanol, drying gets Herba Hyperici perforati extract, and yield is 8.33%, detect with known reversed-phase high-performance liquid chromatography method, the content that records hypericin in the Herba Hyperici perforati extract is 0.81%.
In sum, technology of the present invention is simple, can be used for food and take, hypericin content height, the present invention extracts after utilizing the biological preparation enzymolysis with Herba Hyperici perforati medical material enzymolysis, improved the utilization rate of Herba Hyperici perforati medical material greatly, improved hypericin content in the extract, by the testing result of gained in the foregoing description as can be known, make that with the inventive method hypericin content has improved more than 10 times in the extract, the extract color and luster is good, safety non-pollution, the extract yield height, operation is simple and feasible, is easy to carry out industrial applications.
Claims (3)
1. the biological preparation method of a Herba Hyperici perforati extract, it is characterized in that, earlier with the Herba Hyperici perforati drying, be ground into the Herba Hyperici perforati powder, take by weighing 0.5%～2.5% enzyme of Herba Hyperici perforati powder weight again, 30～60 ℃ of warm water that the 10-20 of adding enzyme weight doubly measures in enzyme, dissolving, 30～60 ℃ of water-baths activate 5～30 minutes, become activatory enzymatic solution, standby; The Herba Hyperici perforati powder mixes with 1: 10～20 weight ratio with water, and 40～90 ℃ of water-baths were soaked 20～90 minutes, be cooled to 18～25 ℃, transfer pH to 4.0～5.5 with hydrochloric acid, shake up, heating in water bath to 40～55 ℃, add above-mentioned activatory enzymatic solution, mixing, enzymolysis 2～12 hours, sucking filtration, discard filtrate, medicinal powder behind the enzymolysis, add the alcohol reflux 2～5 times of 6～20 times of amounts of the medicinal powder weight behind the enzymolysis in the medicinal powder behind enzymolysis, each 1～5 hour, filter, merging filtrate, 50～60 ℃ of concentrating under reduced pressure reclaim ethanol, drying gets Herba Hyperici perforati extract; Said enzyme is one or more the mixing among cellulase, pectase, xylanase, 1,4 beta-glucanase, the compound enzyme SPE-007A.
2. the biological preparation method of Herba Hyperici perforati extract according to claim 1, it is characterized in that,, pulverized 20 mesh sieves earlier with the Herba Hyperici perforati drying, become the Herba Hyperici perforati powder, take by weighing Herba Hyperici perforati powder 1kg, take by weighing the cellulase of 5g again, in cellulase, add 32 ℃ of warm water of 50g, dissolving, 32 ℃ of water-baths activate 28 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder adds water 10000g and mixes, and 40 ℃ of water-baths were soaked 90 minutes, were cooled to 18 ℃, transfer pH to 5.3 with hydrochloric acid, shake up, heating in water bath to 55 ℃ adds above-mentioned activatory enzymatic solution, mixing, enzymolysis 2 hours, sucking filtration discards filtrate, medicinal powder behind the enzymolysis, add the alcohol reflux 3 times of 6 times of amounts of the medicinal powder weight behind the enzymolysis in the medicinal powder behind enzymolysis, each 3 hours, filter merging filtrate, 50 ℃ of concentrating under reduced pressure, reclaim ethanol, drying gets Herba Hyperici perforati extract.
3. the biological preparation method of Herba Hyperici perforati extract according to claim 1, it is characterized in that,, pulverized 20 mesh sieves earlier with the Herba Hyperici perforati drying, become the Herba Hyperici perforati powder, take by weighing Herba Hyperici perforati powder 2kg, take by weighing pectase 30g again, in pectase, add 45 ℃ of warm water of 450g, dissolving, 45 ℃ of water-baths activate 20 minutes, become activatory enzymatic solution, and are standby; The Herba Hyperici perforati powder adds water 30000g and mixes, and 70 ℃ of water-baths were soaked 50 minutes, be cooled to 20 ℃, transfer pH to 4 with hydrochloric acid, shake up, heating in water bath to 47 ℃, add above-mentioned activatory enzymatic solution, mixing, enzymolysis 5 hours, sucking filtration, discard filtrate, medicinal powder behind the enzymolysis, add the alcohol reflux 2 times of 13 times of amounts of the medicinal powder weight behind the enzymolysis in the medicinal powder behind enzymolysis, each 1.5 hours, filter, merging filtrate, 60 ℃ of concentrating under reduced pressure reclaim ethanol, drying gets Herba Hyperici perforati extract.
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| RU2541134C2 (en) * | 2012-12-06 | 2015-02-10 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Профессионального Образования "Дагестанский Государственный Технический Университет" (Дгту) | Method for preparing dry herbal extract of st. john's wort |
| CN103520285A (en) * | 2013-09-27 | 2014-01-22 | 河南牧翔动物药业有限公司 | Veterinary honeysuckle and fructus forsythiae soluble powder and preparation method thereof |
| CN105777522B (en) * | 2014-12-18 | 2017-12-26 | 安徽农达生物技术有限公司 | A kind of method that hypericin is extracted from hypericum perforatum |
| CN105085224B (en) * | 2015-08-31 | 2017-08-11 | 桂林三宝生物科技有限公司 | A kind of method that hypericin is extracted from hypericum perforatum |
| CN106821102A (en) * | 2016-12-29 | 2017-06-13 | 安徽比伦生活用纸有限公司 | A kind of antibacterial facial tissue |
| CN107049848A (en) * | 2016-12-29 | 2017-08-18 | 安徽比伦生活用纸有限公司 | A kind of natural no stimulation wet tissue soak |
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| CN109394843B (en) * | 2019-01-03 | 2021-03-26 | 重庆工商大学 | Method for preparing hypericum perforatum extract rich in hypericin |
| CN111494271B (en) * | 2020-06-19 | 2022-10-28 | 广州智尚生物科技有限公司 | Atractylodes lancea rhizome and hypericum perforatum mixed extract and preparation method and application thereof |
| CN115316539B (en) * | 2022-09-02 | 2023-10-10 | 山东和美集团有限公司 | Nutritional feed for suckling pigs in transitional period and preparation method thereof |
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| 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 |
| CN1615927A (en) * | 2003-11-14 | 2005-05-18 | 韩全文 | Oriental wormwood biological oral liquor |
| CN100404489C (en) * | 2006-04-29 | 2008-07-23 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting hypericin |
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