CN1850766A - Method for extracting hypericin - Google Patents
Method for extracting hypericin Download PDFInfo
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- CN1850766A CN1850766A CN 200610078988 CN200610078988A CN1850766A CN 1850766 A CN1850766 A CN 1850766A CN 200610078988 CN200610078988 CN 200610078988 CN 200610078988 A CN200610078988 A CN 200610078988A CN 1850766 A CN1850766 A CN 1850766A
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- hypericin
- extracting method
- herba hyperici
- hyperici perforati
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Abstract
This invention discloses hypericin distillation method. It includes following procedures 1. Leaf weeping forsythia is dried and pulverized. 2. The forsythia powder is mixed with organic solvent as volume ratio 1-2 t 3, then they are distilled at 40-70 degree centigrade for 2-4 hours, extracting solution is collected, filtrated and filtration liquor is collected. 3. The filtration liquor is decompressed and concentrated, concentrated solution is recovered. 4. The liquor is concentrated by resin, and then eluted, eluent is collected. 5. The eluent is decompressed and concentrated, and then hypericin extractive is got. In this invention its operation is simple, easy for industrial application; its distillation cost is low. The extracting solution toxity is little, distilling period is short. Hypericin content in extract is high. So this invention takes important part in hypericin organism distillation.
Description
Technical field
The present invention relates to the extracting method of compound, particularly relate to the extracting method of hypericin.
Background technology
Hypericin ( hypericin 4,4,5,5,7,7-hexahydroxy--2,2-dimethyl-meta-meso-naphthadianthrene ketone) is the bioactive material of tool in the Herba Hyperici perforati (Hypericum Perforatum L.), has antiviral, antidepressant and photo-activity.
Since in the Herba Hyperici perforati herb content of hypericin have only ten thousand/several, therefore have only extract by chemical means refining.Extracting method commonly used both at home and abroad at present is as follows:
1, methyl alcohol or ethanol extraction method: after Herba Hyperici perforati herb drying, pulverizing, make solvent with ethanol or methyl alcohol, 80 ℃ of refluxing extraction 1-2h repeat to extract repeatedly, and united extraction liquid also concentrates, and obtains hypericin medicinal extract.The shortcoming that there is easy moisture absorption in the product that obtains in this way, is clamminess.
2, alkali liquor extraction method: take by weighing the Herba Hyperici perforati herb of a certain amount of drying, pulverizing, boil 2h, extract 3 times with 1% sodium hydroxide solution of 30 times of amounts, filter, merging filtrate, adding 0.1mol/L hydrochloric acid soln to pH value is 3, concentrating under reduced pressure, vacuum-drying obtains hypericin medicinal extract.This method exists institute to use to such an extent that solvent toxicity is bigger, extracting cycle length and the lower shortcoming of product content that obtains.
3, Tan Zengyi, Gao Rong (technical study of Herba Hyperici perforati medicinal extract [J]. the Chinese medicine magazine .2002 of basic unit, 16 (3): method 26) is: get dried medicinal material 1000g, be cut into 2cm length with scissors, mix rapidly with 70-80 ℃ of sodium hydroxide solution (0.2mol/L), in the plastics bag of packing into, wrap up with cotton-wool immediately, heat-preservation fermentation 5d when treating that whole herbal medicine becomes black and rots shape, adds methyl alcohol-acetone (blending ratio is 7: 3) 6000mL, 50 ℃ of temperature are soaked 12h, filter, so temperature is soaked merging filtrate 3 times, 60 ℃ of concentrating under reduced pressure, reclaim solvent, 60 ℃ of vacuum-dryings again obtain hypericin dry extract 86.4g.The toxicity of solvent for use is bigger in this extracting method, and extracting cycle is long, and the content of hypericin is lower in the extract.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of simple and economic and practical hypericin.
The extracting method of hypericin provided by the present invention may further comprise the steps:
1, with Herba Hyperici perforati drying, pulverizing;
2, the Herba Hyperici perforati meal is 1-2 by volume with organic solvent: 3 mix, and extract 2-4 hour down at 40-70 ℃, collect extracting solution, filter, and collect filtered liquid; Described organic solvent can be 80-100% (V/V) ethanol;
3,, reclaim concentrated solution to the filtered liquid concentrating under reduced pressure;
4, concentrated solution is adsorbed with resin, wash-out is collected elutriant;
5,, obtain hypericin medicinal extract to the elutriant concentrating under reduced pressure.
In the said extracted method, for obtaining purer hypericin, the Herba Hyperici perforati of drying, pulverizing in the step 1 can be carried out removal of impurities with ether earlier, carry out step 2-step 5 again.
Organic solvent in the described step 2 is preferably 98% ethanol; Herba Hyperici perforati meal and organic solvent blended volume ratio are preferably 2: 3; Filtering required filter membrane aperture is 0.45um.
For obtaining better extraction effect, step 2 can be repeated 15-20 time, merge filtered liquid.
Concentrating under reduced pressure in step 3 and the step 5 is preferably under 50-60 ℃ and carries out.
Used resin is special-purpose polymeric adsorbent of LSA-5B or macroporous adsorbent resin in the step 4; The available elutriant is 80-100% (V/V) ethanol.
The invention provides a kind of extracting method of effective hypericin.This extracting method has the following advantages: 1, simple to operate, be easy to carry out industrial applications; 2, extraction cost is cheap; 3, the toxicity of used extraction solvent is less, and extracting cycle is short; 4, hypericin content height in the extract, content can reach 0.9-1.4%, and yield is about 2/10000ths to 5.The present invention lays a good foundation for the scale operation of hypericin, will play a great role in effective utilization of hypericin.
Below in conjunction with specific embodiment the present invention is described in further details
Description of drawings
Fig. 1 is the schema of hypericin extraction process of the present invention
Fig. 2 A is hypericin standard RPLC figure
Fig. 2 B is the RPLC figure of the hypericin sample of extraction
Fig. 3 is the hydrogen nuclear magnetic resonance spectrogram of the hypericin sample of extraction
Embodiment
Method therefor is ordinary method if no special instructions among the following embodiment.
The extraction of embodiment 1, hypericin
The method of current series invention is carried out the biological extraction of hypericin, and schema is seen Fig. 1, may further comprise the steps:
1, with the Herba Hyperici perforati drying, be crushed to 24 orders, precision takes by weighing Herba Hyperici perforati flour 2Kg;
2, Herba Hyperici perforati meal dress diacolation post adds in batches, removes impurity with ether, and lucifuge is dried in the shade;
3, being to mix at 1: 3 by volume with Herba Hyperici perforati and 80% (V/V) ethanol of removal of impurities, extracting 4 hours down at 40 ℃, collect extracting solution, is the membrane filtration of 0.45um with the aperture, collects filtered liquid, repeats this step 15 time, merging filtered liquid;
4, under 60 ℃, filtered liquid is evaporated to thickly, reclaims concentrated solution;
5, concentrated solution is adsorbed with macroporous adsorbent resin,, collect elutriant rosy with 80% (V/V) ethanol elution;
6, under 60 ℃, elutriant is evaporated to absence of liquid and flows out, obtain hypericin medicinal extract.
Now the hypericin medicinal extract that extracts is detected with reversed-phased high performace liquid chromatographic, measure content simultaneously, the RPLC detected result is (Fig. 2 A is the detected result of hypericin standard substance) shown in Fig. 2 B, the hydrogen nuclear magnetic resonance spectrogram as shown in Figure 3, the result shows and has obtained the higher hypericin extract of purity, hypericin content in the extract is 0.9%, and yield is about 2/10000ths.
The extraction of embodiment 2, hypericin
The method of current series invention is carried out the biological extraction of hypericin, may further comprise the steps:
1) with Herba Hyperici perforati drying, powder essence to 24 order, precision takes by weighing Herba Hyperici perforati flour 3Kg;
2) being to mix at 2: 3 by volume with Herba Hyperici perforati and 90% (V/V) ethanol of removal of impurities, extracting 3 hours down at 60 ℃, collect extracting solution, is the membrane filtration of 0.45um with the aperture, collects filtered liquid, repeats this step 20 time, merging filtered liquid;
3) under 60 ℃, filtered liquid is evaporated to thickly, reclaims concentrated solution;
4) concentrated solution is adsorbed with the special-purpose polymeric adsorbent of LSA-5B,, collect elutriant rosy with 90% (V/V) ethanol elution;
5) under 60 ℃, elutriant is evaporated to absence of liquid and flows out, obtain hypericin medicinal extract.
Now use the method identical with embodiment 1 that the hypericin medicinal extract that extracts is detected, measure content simultaneously, show to have obtained the higher hypericin extract of purity, the hypericin content in the extract is 0.95%, and yield is about 2.2/10000ths.
The extraction of embodiment 3, hypericin
The method of current series invention is carried out the biological extraction of hypericin, may further comprise the steps:
1) with Herba Hyperici perforati drying, powder essence to 24 order, precision takes by weighing Herba Hyperici perforati flour 2Kg;
2) Herba Hyperici perforati flour dress diacolation post adds in batches, removes impurity with ether, and lucifuge is dried in the shade;
3) being to mix at 2: 3 by volume with Herba Hyperici perforati and 98% (V/V) ethanol of removal of impurities, extracting 2 hours down at 70 ℃, collect extracting solution, is the membrane filtration of 0.45um with the aperture, collects filtered liquid, repeats this step 20 time, merging filtered liquid;
4) under 50 ℃, filtered liquid is evaporated to thickly, reclaims concentrated solution;
5) concentrated solution is adsorbed with the special-purpose polymeric adsorbent of LSA-5B,, collect elutriant rosy with 98% (V/V) ethanol elution;
6) under 50 ℃, elutriant is evaporated to absence of liquid and flows out, obtain hypericin medicinal extract.
Now use the method identical with embodiment 1 that the hypericin medicinal extract that extracts is detected, measure content simultaneously, show to have obtained the higher hypericin extract of purity, the hypericin content in the extract is 1.0%, and yield is about 2.5/10000ths.
Detected result in the foregoing description shows that method of the present invention can be used in the industrialization extraction of hypericin.
Claims (6)
1, a kind of extracting method of hypericin may further comprise the steps:
1) with Herba Hyperici perforati drying, pulverizing;
2) the Herba Hyperici perforati powder is 1-2 by volume with organic solvent: 3 mix, and extract 2-4 hour down at 40-70 ℃, collect extracting solution, filter, and collect filtered liquid; Described organic solvent is a 80-100% ethanol;
3), reclaim concentrated solution to the filtered liquid concentrating under reduced pressure;
4) concentrated solution is adsorbed with resin, wash-out is collected elutriant;
5), obtain hypericin medicinal extract to the elutriant concentrating under reduced pressure.
2, extracting method according to claim 1 is characterized in that: described extracting method also comprises carry out step 2 with drying, pulverizing Herba Hyperici perforati in the step 1) again with the step that ether carries out removal of impurities)-step 5).
3, extracting method according to claim 1 and 2 is characterized in that: the organic solvent described step 2) is 98% ethanol; Herba Hyperici perforati powder and organic solvent blended volume ratio are 2: 3; Filtering required filter membrane aperture is 0.45um.
4, extracting method according to claim 1 and 2 is characterized in that: with step 2) repeat 15-20 time, merge filtered liquid.
5, extracting method according to claim 1 and 2 is characterized in that: the concentrating under reduced pressure in described step 3) and the step 5) carries out under 50-60 ℃.
6, extracting method according to claim 1 and 2 is characterized in that: the type of resin is special-purpose polymeric adsorbent of LSA-5B or macroporous adsorbent resin in the described step 4); Elutriant is a 80-100% ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100789889A CN100404489C (en) | 2006-04-29 | 2006-04-29 | Method for extracting hypericin |
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| CNB2006100789889A CN100404489C (en) | 2006-04-29 | 2006-04-29 | Method for extracting hypericin |
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| CN1850766A true CN1850766A (en) | 2006-10-25 |
| CN100404489C CN100404489C (en) | 2008-07-23 |
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| CNB2006100789889A Expired - Fee Related CN100404489C (en) | 2006-04-29 | 2006-04-29 | Method for extracting hypericin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744795A (en) * | 2010-03-11 | 2010-06-23 | 中国人民解放军第三军医大学第三附属医院 | Medicinal composition for treating nevus flammeus and preparation method thereof |
| CN101829164A (en) * | 2010-05-07 | 2010-09-15 | 河南中医学院 | Biological preparation method of Hypericum perforatum L extractive |
| CN105693494A (en) * | 2016-02-27 | 2016-06-22 | 蚌埠医学院 | Process for extracting and purifying hypericin from hypericum perforatum |
| CN105777522A (en) * | 2014-12-18 | 2016-07-20 | 六安裕发农业科技有限公司 | Method for extracting hypericin from Hypericum perforatum |
| CN107308203A (en) * | 2017-05-25 | 2017-11-03 | 中国农业科学院兰州畜牧与兽药研究所 | A kind of preparation method of the Hypericum Perforatum P.E of high dianthracene ketone content |
| CN113633590A (en) * | 2021-08-31 | 2021-11-12 | 广东轻工职业技术学院 | Application of hypericum perforatum extract with strong anti-aging effect in preparing anti-aging cosmetics |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100367976C (en) * | 2004-04-21 | 2008-02-13 | 上海市中药研究所 | Hypericum perforatum extract and its preparation process |
-
2006
- 2006-04-29 CN CNB2006100789889A patent/CN100404489C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744795A (en) * | 2010-03-11 | 2010-06-23 | 中国人民解放军第三军医大学第三附属医院 | Medicinal composition for treating nevus flammeus and preparation method thereof |
| CN101744795B (en) * | 2010-03-11 | 2012-07-04 | 中国人民解放军第三军医大学第三附属医院 | Medicinal composition for treating nevus flammeus and preparation method thereof |
| CN101829164A (en) * | 2010-05-07 | 2010-09-15 | 河南中医学院 | Biological preparation method of Hypericum perforatum L extractive |
| CN105777522A (en) * | 2014-12-18 | 2016-07-20 | 六安裕发农业科技有限公司 | Method for extracting hypericin from Hypericum perforatum |
| 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 |
| CN105693494A (en) * | 2016-02-27 | 2016-06-22 | 蚌埠医学院 | Process for extracting and purifying hypericin from hypericum perforatum |
| CN107308203A (en) * | 2017-05-25 | 2017-11-03 | 中国农业科学院兰州畜牧与兽药研究所 | A kind of preparation method of the Hypericum Perforatum P.E of high dianthracene ketone content |
| CN113633590A (en) * | 2021-08-31 | 2021-11-12 | 广东轻工职业技术学院 | Application of hypericum perforatum extract with strong anti-aging effect in preparing anti-aging cosmetics |
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| CN100404489C (en) | 2008-07-23 |
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Owner name: LANZHOU LIVESTOCK AND ANIMAL DRUG INST., CHINESE Free format text: FORMER OWNER: LANZHOU LIVESTOCK AND ANIMAL DRUG INST., CHINESE ACADEMY OF AGRICULTURAL SCIENCE Effective date: 20081024 |
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Effective date of registration: 20081024 Address after: Gansu city of Lanzhou province West Lake Qilihe district base along the 335 zip code: 730050 Co-patentee after: Modern Physics Inst., Chinese Academy of Sciences Patentee after: Lanzhou Institute of animal husbandry and veterinary medicine, Chinese Academy of Agricultural Sciences Address before: Gansu city of Lanzhou province West Lake Qilihe district base along the 335 zip code: 730050 Patentee before: Lanzhou Inst. of Animal Husbandary & Veterinary Medicine, Chinese Academy of Agr |
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Granted publication date: 20080723 Termination date: 20100429 |