CN103044258A - Novel technology method for extracting lichen parmeliae tinctori atranorine from wild lichen parmeliae tinctori - Google Patents
Novel technology method for extracting lichen parmeliae tinctori atranorine from wild lichen parmeliae tinctori Download PDFInfo
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- CN103044258A CN103044258A CN2012105956046A CN201210595604A CN103044258A CN 103044258 A CN103044258 A CN 103044258A CN 2012105956046 A CN2012105956046 A CN 2012105956046A CN 201210595604 A CN201210595604 A CN 201210595604A CN 103044258 A CN103044258 A CN 103044258A
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Abstract
The invention belongs to the field of natural organic chemistry, and relates to a method for extracting lichen parmeliae tinctori atranorine from wild lichen parmeliae tinctori in great khingan, in particular to a novel method for obtaining high-purity atranorine by conducting microwave countercurrent extraction and macroporous resin purification and then combining with freeze drying. The method has the advantages that the method is simple and easy to operate, and low in cost, and is suitable for mass production. 1, a microwave countercurrent extraction technique is a combination of dynamic extraction, countercurrent extraction and a decocting extraction technologies; an extraction speed is high; effective components are extracted fully; the extraction yield is high; and 2, macroporous resin performs physical adsorption via a large specific surface of the macroporous resin and by depending on a van der waals force, and further purifies the effective components after the microwave extraction; the resin can be reused; the production cost is lowered greatly; and the method is applicable to industrial use. The method adopts the microwave countercurrent extraction technique, so that the effective components are extracted fully; the macroporous resin is used for further purification; then the freeze drying is conducted; obtained lichen parmeliae tinctori atranorine is high in activity; and the purity is increased to 98.5%.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of method of extracting white parmelia saxatilis tea stain element in the wild white parmelia saxatilis of Daxing'an Mountainrange, particularly relate to a kind of microwave counter current that utilizes and extract, macroporous resin purification obtains the novel method of high-purity tea stain element again in conjunction with lyophilize.
Background technology:
The wild white parmelia saxatilis is born on rock and the bark.Originate in Daxinganling District exhale in, the ground such as A Muer.Bai Shihua thallus is wrinkled more, 30 centimetres of diameters, above canescence, the edge splits into most irregular lobes; The sliver tip is circular, and the edge the fecula bud, and is level and smooth, little glossy, the close life of central pin bud, and black, more coarse, lower edge department is level and smooth, and tarnish has rhizoid.Sub-device is few, cup-shaped, and 1 centimetre of diameter has short handle; Spore is oval, and Room 1 is colourless.Bai Shihua mainly contains sekikaic acid, parmelia saxatilis tea stain element, still contains in addition orcinol carboxylate methyl ester etc.The domestic general alcohol heat reflux extraction method of using exists service temperature high, the shortcomings such as unstable product quality, and difference of the present invention is to adopt the microwave extraction method, and the later stage adopts macroporous resin purification again in conjunction with cryodesiccated novel method.
Summary of the invention:
Advantage of the present invention: mainly adopt microwave counter current to extract, macroporous resin purification is again in conjunction with cryodesiccated novel method.The inventive method is simple to operation, and cost is low, is fit to large production.
For achieving the above object, the technical solution used in the present invention is:
A kind of employing microwave counter current extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows:
(1) dry white parmelia saxatilis thallus is crushed to the 40-60 order, adds the alkali lye of 60-80% concentration, microwave extraction, and microwave power is 300～600W, frequency 3000～10000MHz, extraction time 60-80min extracts under certain temperature and solid-liquid ratio;
(2) with extracting solution through purpose ceramic-film filter at filtering accuracy 0.2-0.5 micron, filter pressure 02-0.3MPa filters under the 5-10m/s filtering velocity, can remove most of impurity;
(3) macroporous resin adsorption:
After reclaiming alkali lye, with macroporous resin adsorption on the gained solution, flow velocity is 3-5BV/h, and adsorption temp is 40-45 ℃, and the aspect ratio of resin column is 8: 1-15: 1;
(4) ethanol elution:
At normal temperatures and pressures, with the 1-3BV/h flow velocity, use first the removal of impurities of 5-10% ethanol, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) alkali lye wash-out:
Be to carry out wash-out under the 6-8BV with alkaline solution at 1-3BV/h flow velocity, elution volume again, elutriant is with thin-layer chromatography tracking monitor (contrast take white parmelia saxatilis element as reference substance);
(6) get crude extract:
The collection elutriant is concentrated, reclaims alkali lye, drying under reduced pressure, and obtaining content is 65% above work in-process meal;
(7) silica gel column chromatography:
The gained meal is dissolved in alkali lye adds the proper silica gel stirring, dried the 60-80 mesh sieve, the dry method loading, upper technical grade post silica gel column chromatography, and with chloroform-methanol solution with 95～85: 2 ratios are carried out wash-out, and tlc follow the tracks of to detect, and collect white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) lyophilize:
24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, obtains the white parmelia saxatilis tea stain of high purity element, and its content is more than 98%.
Embodiment:
Case study on implementation 1: a kind of employing microwave counter current extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows:
(1) gets the dry white parmelia saxatilis of 500g and be crushed to 40 orders, add 60% sodium hydroxide solution, be 300W at microwave power, frequency 3000～MHz, extraction time 600min is warming up to 50 ℃ of microwave counter currents and extracts under 8 times of solid-liquid ratio conditions, forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water gets extracting solution;
(2) with extracting solution through purpose ceramic-film filter 0.2 micron of filtering accuracy, filter pressure 0.2MPa filters under the 5m/s filtering velocity, can remove most of impurity;
(3) reclaim alkali lye, with macroporous resin adsorption on the gained solution, model is the DA201 resin, and the blade diameter length ratio of resin column is 8: 1, and upper column flow rate is 3BV/h, and adsorption temp is 40 ℃;
(4) at normal temperatures and pressures, with the 1BV/h flow velocity, use first 5% ethanol removal of impurities, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) be to carry out wash-out under the 6BV with 40%, 50%, 60%, 70%, 85%, 95% alkaline solution at 1BV/h flow velocity, elution volume again, take reference substance as contrast, elutriant thin-layer chromatography tracking monitor is collected elutriant;
(6) elutriant is concentrated, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine work in-process 4.17g;
(7) alkali lye that the gained meal is dissolved in 80% concentration adds proper silica gel and stirs, dried the 60-80 mesh sieve, the dry method loading, upper technical grade post 300 order silica gel column chromatographies, and with chloroform-methanol solution with 95～85: 2 ratios are carried out wash-out, tlc is followed the tracks of and is detected, and collects white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) 24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, and vacuum degree control is at 10pa, and be 3h time of drying, obtains high purity atranorine 2.68g, and its content is 98.3%.
Case study on implementation 2: a kind of employing microwave counter current extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows:
(1) gets the dry white parmelia saxatilis of 500g and be crushed to 50 orders, add 70% sodium hydroxide solution, at 500W, frequency 6000MHz, time 70min is warming up to 60 ℃ of microwave counter currents and extracts under 10 times of solid-liquid ratio conditions, forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water gets extracting solution;
(2) with extracting solution through purpose ceramic-film filter 0.4 micron of filtering accuracy, filter pressure 0.3MPa filters under the 8m/s filtering velocity, can remove most of impurity;
(3) reclaim alkali lye, with macroporous resin adsorption on the gained solution, model is the D101 resin, and the blade diameter length ratio of resin column is 10: 1, and upper column flow rate is 4BV/h, and adsorption temp is 45 ℃;
(4) at normal temperatures and pressures, with the 2BV/h flow velocity, use first 10% ethanol removal of impurities, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) be to carry out wash-out under the 7BV with 40%, 50%, 60%, 70%, 85%, 95% alkaline solution at 2BV/h flow velocity, elution volume again, take reference substance as contrast, elutriant thin-layer chromatography tracking monitor is collected elutriant;
(6) elutriant is concentrated, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine work in-process 4.17g;
(7) alkali lye that the gained meal is dissolved in 85% concentration adds proper silica gel and stirs, dried the 60-80 mesh sieve, the dry method loading, upper technical grade post 200 order silica gel column chromatographies, and with chloroform-methanol solution with 95～85: the ethanol of 2 ratios or 60-70% concentration carries out wash-out, tlc is followed the tracks of and is detected, and collects white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) 24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, and vacuum degree control is at 12pa, and be 4h time of drying, obtains high purity atranorine 2.76g, and its content is 98.5%.
Case study on implementation 3: a kind of employing microwave counter current extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows:
(1) gets the dry white parmelia saxatilis of 500g and be crushed to 60 orders, add 80% sodium hydroxide solution, at 600W, frequency 8000MHz, time 80min is warming up to 60 ℃ of microwave counter currents and extracts under 15 times of solid-liquid ratio conditions, forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water gets extracting solution;
(2) with extracting solution through purpose ceramic-film filter 0.4 micron of filtering accuracy, filter pressure 0.3MPa filters under the 8m/s filtering velocity, can remove most of impurity;
(3) reclaim alkali lye, with macroporous resin adsorption on the gained solution, model is the HPD300 resin, and the blade diameter length ratio of resin column is 12: 1, and upper column flow rate is 4BV/h, and adsorption temp is 40 ℃;
(4) at normal temperatures and pressures, with the 3BV/h flow velocity, use first 10% ethanol removal of impurities, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) be to carry out wash-out under the 7BV with 40%, 50%, 60%, 70%, 85%, 95% alkaline solution at 2BV/h flow velocity, elution volume again, take reference substance as contrast, elutriant thin-layer chromatography tracking monitor is collected elutriant.
(6) elutriant is concentrated, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine method finished product 4.21g;
(7) alkali lye that the gained meal is dissolved in 90% concentration adds proper silica gel and stirs, and dries the 60-80 mesh sieve, the dry method loading, upper technical grade post 300 order silica gel column chromatographies, and carry out wash-out with 70% ethanolic soln, tlc is followed the tracks of and is detected, and collects white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) 24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, and vacuum degree control is at 10pa, and be 4h time of drying, obtains high purity atranorine 2.74g, and its content is 98.09%.
Case study on implementation 4: a kind of employing microwave counter current extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows:
(1) gets the dry white parmelia saxatilis of 500g and be crushed to 50 orders, add 80% sodium hydroxide solution, at 500W, frequency 10000MHz, time 70min is warming up to 70 ℃ of microwave counter currents and extracts under 10 times of solid-liquid ratio conditions, forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water gets extracting solution;
(2) with extracting solution through purpose ceramic-film filter 0.5 micron of filtering accuracy, filter pressure 0.2MPa filters under the 10m/s filtering velocity, can remove most of impurity;
(3) reclaim alkali lye, with macroporous resin adsorption on the gained solution, model is the AB-8 resin, and the blade diameter length ratio of resin column is 15: 1, and upper column flow rate is 5BV/h, and adsorption temp is 45 ℃;
(4) at normal temperatures and pressures, with the 3BV/h flow velocity, with 5% ethanol removal of impurities, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) be to carry out wash-out under the 7BV with 40%, 50%, 60%, 70%, 85%, 95% alkaline solution at 2BV/h flow velocity, elution volume again.Take reference substance as contrast, elutriant thin-layer chromatography tracking monitor is collected elutriant;
(6) elutriant is concentrated, reclaim alkali lye, drying under reduced pressure, obtaining content is that 65.47% tea steeps plain work in-process 4.13g;
(7) alkali lye that the gained meal is dissolved in 95% concentration adds proper silica gel and stirs, and dries the 60-80 mesh sieve, the dry method loading, upper technical grade post 200 order silica gel column chromatographies, and carry out wash-out with 60% ethanolic soln, tlc is followed the tracks of and is detected, and collects white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) 24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, and vacuum degree control is at 12pa, and be 3h time of drying, obtains high purity atranorine 2.71g, and its content is 98.3%.
Claims (6)
1. one kind is adopted microwave counter current to extract, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and its step is as follows;
(1) dry white parmelia saxatilis thallus is crushed to the 40-60 order, adds the alkali lye of 60-80% concentration, microwave extraction, and microwave power is 300～600W, frequency 3000～10000MHz, extraction time 60-80min extracts under certain temperature and solid-liquid ratio;
(2) with extracting solution through purpose ceramic-film filter at filtering accuracy 0.2-0.5 micron, filter pressure 0.2-0.4MPa filters under the 5-10m/s filtering velocity, can remove most of impurity;
(3) macroporous resin adsorption:
After reclaiming alkali lye, with macroporous resin adsorption on the gained solution, flow velocity is 3-5BV/h, and adsorption temp is 40-45 ℃; The aspect ratio of resin column is 8: 1-15: 1;
(4) ethanol elution:
At normal temperatures and pressures, with the 1-3BV/h flow velocity, use first the removal of impurities of 5-10% ethanol, wash the water-soluble impurities such as pigment in the solution, tannin, inorganic salts off;
(5) alkali lye wash-out:
Be to carry out wash-out under the 6-8BV with alkaline solution at 1-3BV/h flow velocity, elution volume again, elutriant is with thin-layer chromatography tracking monitor (contrast take white parmelia saxatilis element as reference substance);
(6) get crude extract:
The collection elutriant is concentrated, reclaims alkali lye, drying under reduced pressure, and obtaining content is 65% above work in-process meal;
(7) silica gel column chromatography:
The gained meal is dissolved in alkali lye adds the proper silica gel stirring, dried the 60-80 mesh sieve, the dry method loading, upper technical grade post silica gel column chromatography, and with chloroform-methanol solution with 95～85: 2 ratios are carried out wash-out, and tlc follow the tracks of to detect, and collect white each stepwise elution liquid of parmelia saxatilis tea stain element;
(8) lyophilize:
24h is frozen in the gained liquid cooling, is placed in the vacuum dryer, vacuumizes, and Heating temperature is 45 ℃, takes out behind the dry certain hour, obtains the white parmelia saxatilis tea stain of high purity element, and its content is more than 98%.
2. a kind of employing microwave counter current according to claim 1 extracts, macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, it is characterized in that: in described step (1), solid-liquid ratio is 1: 5-10, extracting temperature is 40-50 ℃.
3. a kind of employing microwave counter current according to claim 2 extracts, macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, it is characterized in that: in described step (3), the resin model is a kind of in DA201, D101, HPD300, the AB-8 resin.
4. a kind of employing microwave counter current according to claim 3 extracts, and macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, and it is characterized in that: in described step (5), the wash-out concentration of lye is 40%-95%.
5. a kind of employing microwave counter current according to claim 4 extracts, macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, it is characterized in that: in described step (7), silica gel 200-300 order, concentration of lye are 80%-95%.
6. a kind of employing microwave counter current according to claim 5 extracts, macroporous resin purification obtains the novel method of the white parmelia saxatilis tea stain of high purity element again in conjunction with lyophilize, it is characterized in that: in described step (8), vacuum degree control is 10 to 12pa, and be 3-4h time of drying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832022A (en) * | 2015-12-04 | 2017-06-13 | 威海市宇王集团有限公司 | A kind of method for extracting fucoidan |
| CN110128272A (en) * | 2019-06-04 | 2019-08-16 | 扬州工业职业技术学院 | A kind of fanshaped corallodiscus herb acid extract and its application in prevention and treatment rice sheath blight disease |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1500520A (en) * | 2002-11-18 | 2004-06-02 | 大兴安岭林格贝有机食品有限责任公司 | Lichen bacteriophage and its production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1500520A (en) * | 2002-11-18 | 2004-06-02 | 大兴安岭林格贝有机食品有限责任公司 | Lichen bacteriophage and its production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王丽昀: "微波辅助提取天然产物有效成分工艺研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 01, 15 January 2011 (2011-01-15), pages 016 - 439 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832022A (en) * | 2015-12-04 | 2017-06-13 | 威海市宇王集团有限公司 | A kind of method for extracting fucoidan |
| CN110128272A (en) * | 2019-06-04 | 2019-08-16 | 扬州工业职业技术学院 | A kind of fanshaped corallodiscus herb acid extract and its application in prevention and treatment rice sheath blight disease |
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Address after: Small town Songling District 165000 Yongxing street be immensely proud of Heilongjiang area of Greater Khingan Range Province Applicant after: DAXINGANLING LINGOBERRY BOREAL BIOTECH Co.,Ltd. Address before: 165000 Heilongjiang Province, Jiagedaqi Xinyuan District Changhong community road Beilin Gebe AGA group Applicant before: Daxinganling Lingonberry Organic Foodstuffs Co.,Ltd. |
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