CN101386615A - Method for extracting procyanidine from sea-buckthorn seed - Google Patents
Method for extracting procyanidine from sea-buckthorn seed Download PDFInfo
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- CN101386615A CN101386615A CNA2008101760336A CN200810176033A CN101386615A CN 101386615 A CN101386615 A CN 101386615A CN A2008101760336 A CNA2008101760336 A CN A2008101760336A CN 200810176033 A CN200810176033 A CN 200810176033A CN 101386615 A CN101386615 A CN 101386615A
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- fructus hippophae
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Abstract
The invention relates to a method for extracting proanthocyanidins from sea buckthorn seeds. The method comprises the following steps of: extracting sea buckthorn seed dregs by refluxing extraction, depressing and condensing the eluted liquid after filtering, absorbing and eluting, and drying the eluted liquid so as to obtain the proanthocyanidins product. The method has the characteristics of availability of raw material, low cost and environmental protection, and can meet the demands of developing various proanthocyanidins drugs and healthcare products.
Description
Technical field
The present invention relates to the extracting method of pycnogenols, relate in particular to a kind of method of extracting pycnogenols in the seed of Fructus Hippophae.
Background technology
Pycnogenols (Procyanidins) is the general name of a big class polyphenolic substance, be a kind of Vitamin P complex that special molecular structure is arranged, be generally the reddish-brown powder, little, the puckery of gas, water-soluble and most organic solvent is generally Semen Vitis viniferae extract or French maritime pine bark extract.1967, extraction separation from Pericarpium Vitis viniferae and Semen Vitis viniferae such as U.S. Joslyn went out 4 kinds of polyphenolic compounds, and these compounds heat in acidic medium all can produce anthocyanidin, so with these compound called after pycnogenolss.Pycnogenols is that the 4-glycol is polymerized by the flavan-3-alcohol of different numbers or flavane-3, and by the size of the polymerization degree, two are called oligomeric procyanidolics to the tetramer, then are called high poly-pycnogenols more than the pentamer.Pycnogenols has extensively, significant biochemistry and pharmacologically active, and wherein oligomeric procyanidolics, low toxicity efficient with it, high bioavailability have caused people's very big interest.Experiment showed, that oligomeric procyanidolics has direct or indirect prevention, therapeutic action to nearly more than 70 kinds of diseases, have purposes widely in fields such as medicine, makeup and healthcare products.
At present, the main raw material that extracts proanthocyanidin both at home and abroad is a Semen Vitis viniferae, and its composition is pycnogenols (monomer is a catechin), and mean polymerisation degree is lower; And the chemical structure of seed of Fructus Hippophae pycnogenols significantly is different from grape pip procyanidin, is mainly former delphinidin (monomer is the tangerine catechin), and mean polymerisation degree is about 12.8.Therefore, the anti-oxidant activity of seed of Fructus Hippophae pycnogenols is significantly higher than grape pip procyanidin.
Summary of the invention
It is the method for pycnogenols in raw material, the extraction seed of Fructus Hippophae with low cost with the seed of Fructus Hippophae that technical problem to be solved by this invention provides a kind of.
For addressing the above problem, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae of the present invention comprises the steps:
1. the seed of Fructus Hippophae slag is extracted with reflux extraction, get extracting solution; Reclaim extracting solution, get filtrate after filtration;
2. with filtrate behind absorption with macroporous adsorbent resin, water, ethanolic soln wash-out are successively collected elutriant;
3. elutriant is carried out concentrating under reduced pressure, reclaim ethanol, get the pycnogenols aqueous solution;
4. will get final product after the pycnogenols aqueous solution drying.
The seed of Fructus Hippophae slag of described step in 1. is meant and utilizes solvent-extraction process or supercritical CO
2The seed of Fructus Hippophae slag that is obtained behind the extraction Seabuckthorm Seed Oil.
The refluxing extraction condition of described step in 1. is: 30～60 ℃ of temperature, and feed liquid volume ratio is by weight counted 1:5～1:10, and alcohol concn is 30～95%.
The alcohol concn of described step in 2. is 30%～95%.
The drying means of described step in 4. is lyophilize or spraying drying.
The present invention compared with prior art has the following advantages:
1, be solvent owing to the present invention adopts ethanol, therefore safe and reliable in leaching process, be easy to suitability for industrialized production.
2, because the sea-buckthorn that the present invention's employing is easy to obtain is a raw material, therefore greatly reduce production cost, the while also provides reliable guidance for the deep development and the utilization of sea buckthorn resources.
3, because the present invention is a solvent with alcohol in leaching process, and by absorption with macroporous adsorbent resin, therefore can effectively improve product purity, make the product procyanidin content reach 80%; Guarantee no solvent residue simultaneously, can satisfy various pycnogenols class medicines and protective foods demands of developing.
Embodiment
Embodiment 1: a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. will utilize the seed of Fructus Hippophae slag 1kg 10L that is obtained behind the solvent-extraction process extraction Seabuckthorm Seed Oil, 70% ethanolic soln to extract 4 times each 2.5 hours extraction times down at 60 ℃; Merge No. four times extracting solution,, get the aqueous solution, and after 200 order filter clothes filter, get filtrate with the concentrated ethanol that reclaims of the 20L Rotary Evaporators of Jiangsu Xing Hai Instrument and Equipment Company production;
2. behind the D101 type absorption with macroporous adsorbent resin that Chemical Plant of Nankai Univ. of the treated mistake of 2.5L filtrate is produced, first water be eluted to colourless after, do not stop wash-out, collection elutriant with 95% ethanol elution when pycnogenols flows out to having again;
3. to elutriant through 20L Rotary Evaporators concentrating under reduced pressure, reclaim ethanol, the pycnogenols aqueous solution (being mother liquor);
4. the 6L Freeze Drying Equipment that the pycnogenols aqueous solution is placed U.S. LABCONCO to produce, at-30 ℃ of precooling 3h, carry out vacuum-drying 36h again after, powdery pycnogenols product 23.8g, this moment, procyanidin content was 78.8%.
Wherein: the solvent-extraction process that the seed of Fructus Hippophae slag is adopted is meant after seed of Fructus Hippophae is pulverized and utilizes organic solvent to carry out the heating and refluxing extraction Seabuckthorm Seed Oil.
The treatment process of macroporous adsorbent resin is after at first adopting the HCL solution of 5% NaOH solution and 5% to soak 24h respectively, to be neutral, standby with distilled water flushing to pH value.
The employing ammonium ferric sulfate solution detects when judging pycnogenols wash-out situation, exists if any pycnogenols, can show red when adding ammonium ferric sulfate solution, if do not have then nondiscoloration.
Embodiment 2: a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. will utilize supercritical CO
2The seed of Fructus Hippophae slag 10kg 70L that is obtained behind the extraction Seabuckthorm Seed Oil, 95% ethanolic soln extract 3 times down at 50 ℃, each 1.5 hours extraction times; Merge No. three times extracting solution, use the 20L Rotary Evaporators to concentrate and reclaim ethanol, get the aqueous solution, and after 200 order filter clothes filter, get filtrate;
2. behind the D101 type absorption with macroporous adsorbent resin with the treated mistake of 6L filtrate, first water be eluted to colourless after, do not stop wash-out to having when pycnogenols flows out with 65% ethanol elution again, collect elutriant;
3. to elutriant through 20L Rotary Evaporators concentrating under reduced pressure, reclaim ethanol, the pycnogenols aqueous solution (being mother liquor);
4. the Mini Spray Dryer B one 29 type spray-dryers that the pycnogenols aqueous solution placed Switzerland BUCHI to produce, to set tower wind-warm syndrome degree be 160 ℃, go out the tower wind-warm syndrome is that 80 ℃, airshed are 20m/h, get powdery pycnogenols product 196.5g after spray-dried, this moment, procyanidin content was 71.3%.
Wherein: the supercritical CO that the seed of Fructus Hippophae slag is adopted
2Method is meant that the supercritical extraction instrument that utilizes Huaan, Nantong supercritical extraction equipment company limited to produce extracts the seed oil in the seed of Fructus Hippophae, and postcritical extraction parameter is 30～50 ℃ of extraction temperature, and extracting pressure is 20～35Mpa, and the extraction time is 1～3h.
The treatment process of macroporous adsorbent resin and judgement pycnogenols wash-out situation are with embodiment 1.
Embodiment 3: a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. will utilize solvent-extraction process or supercritical CO
2The seed of Fructus Hippophae slag 20kg 100L that is obtained behind the extraction Seabuckthorm Seed Oil, 30% ethanolic soln extract 1 time down at 30 ℃, each 2.5 hours extraction times; Use the 20L Rotary Evaporators to concentrate extracting solution and reclaim ethanol, get the aqueous solution, and after 200 order filter clothes filter, get filtrate;
2. behind the D101 type absorption with macroporous adsorbent resin with the treated mistake of 8L filtrate, first water be eluted to colourless after, do not stop wash-out to having when pycnogenols flows out with 30% ethanol elution again, collect elutriant;
3. to elutriant through 20L Rotary Evaporators concentrating under reduced pressure, reclaim ethanol, the pycnogenols aqueous solution (being mother liquor);
4. get powdery pycnogenols product 436.6g after pycnogenols solution being adopted lyophilize or spraying drying, this moment, procyanidin content was 31.5%.
The treatment process of macroporous adsorbent resin and judgement pycnogenols wash-out situation are with embodiment 1.
Claims (5)
1, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. the seed of Fructus Hippophae slag is extracted with reflux extraction, get extracting solution; Reclaim extracting solution, get filtrate after filtration;
2. with filtrate behind absorption with macroporous adsorbent resin, water, ethanolic soln wash-out are successively collected elutriant;
3. elutriant is carried out concentrating under reduced pressure, reclaim ethanol, get the pycnogenols aqueous solution;
4. will get final product after the pycnogenols aqueous solution drying.
2, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae as claimed in claim 1 is characterized in that: the seed of Fructus Hippophae slag of described step in 1. is meant and utilizes solvent-extraction process or supercritical CO
2The seed of Fructus Hippophae slag that is obtained behind the extraction Seabuckthorm Seed Oil.
3, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae as claimed in claim 1 is characterized in that: the refluxing extraction condition of described step in 1. is: 30～60 ℃ of temperature, and feed liquid volume ratio is by weight counted 1:5～1:10, and alcohol concn is 30～95%.
4, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae as claimed in claim 1 is characterized in that: the alcohol concn of described step in 2. is 30%～95%.
5, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae as claimed in claim 1 is characterized in that: the drying means of described step in 4. is lyophilize or spraying drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101760336A CN101386615A (en) | 2008-11-05 | 2008-11-05 | Method for extracting procyanidine from sea-buckthorn seed |
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| CNA2008101760336A CN101386615A (en) | 2008-11-05 | 2008-11-05 | Method for extracting procyanidine from sea-buckthorn seed |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432578A (en) * | 2011-11-18 | 2012-05-02 | 马映原 | Method for extracting proanthocyanidins from seabuckthorm seeds |
| CN102579591A (en) * | 2011-12-20 | 2012-07-18 | 北京宝得瑞食品有限公司 | Formula of health product for adjusting blood fat and reducing blood viscosity |
| CN103652859A (en) * | 2013-11-13 | 2014-03-26 | 西安医学院 | Health-care food with oxidation resistance and preparation method thereof |
| CN103992299A (en) * | 2014-04-09 | 2014-08-20 | 中国科学院西北高原生物研究所 | Method for simultaneously separating and purifying bioactive components in seabuckthorn fruit seed meal |
| CN104585871A (en) * | 2015-01-20 | 2015-05-06 | 川渝中烟工业有限责任公司 | Seabuckthorn flavone antioxidant electronic cigarette juice |
| CN109593075A (en) * | 2018-09-25 | 2019-04-09 | 宝得瑞（湖北）健康产业有限公司 | A kind of method that room temperature efficient high-pressure difference continous way extracts seabuckthorn seeds procyanidine |
| CN109954008A (en) * | 2017-12-14 | 2019-07-02 | 邹玮 | A kind of sea buckthorn procyanidins soft capsule and preparation method for killing Eradication Therapy of Helicobacter pylori Infection gastric ulcer |
| CN113558125A (en) * | 2021-08-20 | 2021-10-29 | 甘肃农业大学 | Seabuckthorn tea rich in seabuckthorn seed procyanidine and capable of preventing alcoholic intestinal injury |
-
2008
- 2008-11-05 CN CNA2008101760336A patent/CN101386615A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432578B (en) * | 2011-11-18 | 2015-06-10 | 北京宝得瑞食品有限公司 | Method for extracting proanthocyanidins from seabuckthorm seeds |
| CN102432578A (en) * | 2011-11-18 | 2012-05-02 | 马映原 | Method for extracting proanthocyanidins from seabuckthorm seeds |
| CN102579591A (en) * | 2011-12-20 | 2012-07-18 | 北京宝得瑞食品有限公司 | Formula of health product for adjusting blood fat and reducing blood viscosity |
| CN102579591B (en) * | 2011-12-20 | 2014-12-24 | 北京宝得瑞食品有限公司 | Health product for adjusting blood fat and reducing blood viscosity |
| CN103652859A (en) * | 2013-11-13 | 2014-03-26 | 西安医学院 | Health-care food with oxidation resistance and preparation method thereof |
| CN103652859B (en) * | 2013-11-13 | 2016-03-09 | 西安医学院 | A kind of health food with anti-oxidation function and preparation method thereof |
| CN103992299A (en) * | 2014-04-09 | 2014-08-20 | 中国科学院西北高原生物研究所 | Method for simultaneously separating and purifying bioactive components in seabuckthorn fruit seed meal |
| CN103992299B (en) * | 2014-04-09 | 2016-03-23 | 中国科学院西北高原生物研究所 | The method of multiple bioactive ingredients in separation and purification sea-buckthorn seed cake while of a kind of |
| CN104585871B (en) * | 2015-01-20 | 2016-02-03 | 川渝中烟工业有限责任公司 | The anti-oxidant tobacco juice for electronic smoke of a kind of Hippophate flavone |
| CN104585871A (en) * | 2015-01-20 | 2015-05-06 | 川渝中烟工业有限责任公司 | Seabuckthorn flavone antioxidant electronic cigarette juice |
| CN109954008A (en) * | 2017-12-14 | 2019-07-02 | 邹玮 | A kind of sea buckthorn procyanidins soft capsule and preparation method for killing Eradication Therapy of Helicobacter pylori Infection gastric ulcer |
| CN109593075A (en) * | 2018-09-25 | 2019-04-09 | 宝得瑞（湖北）健康产业有限公司 | A kind of method that room temperature efficient high-pressure difference continous way extracts seabuckthorn seeds procyanidine |
| CN113558125A (en) * | 2021-08-20 | 2021-10-29 | 甘肃农业大学 | Seabuckthorn tea rich in seabuckthorn seed procyanidine and capable of preventing alcoholic intestinal injury |
| CN113558125B (en) * | 2021-08-20 | 2023-09-29 | 甘肃农业大学 | Sea buckthorn tea rich in sea buckthorn seed procyanidine and capable of preventing alcoholic intestinal injury |
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Application publication date: 20090318 |