CN103044258B - A kind of novel technological method extracting white parmelia saxatilis tea stain element from wild white parmelia saxatilis - Google Patents
A kind of novel technological method extracting white parmelia saxatilis tea stain element from wild white parmelia saxatilis Download PDFInfo
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- CN103044258B CN103044258B CN201210595604.6A CN201210595604A CN103044258B CN 103044258 B CN103044258 B CN 103044258B CN 201210595604 A CN201210595604 A CN 201210595604A CN 103044258 B CN103044258 B CN 103044258B
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- parmelia saxatilis
- tea stain
- white parmelia
- macroporous resin
- lyophilize
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Abstract
The invention belongs to field of natural organic chemistry, relate to a kind of method extracting white parmelia saxatilis tea stain element from the wild white parmelia saxatilis of Daxing'an Mountainrange, particularly relating to one utilizes microwave counter current to extract, and macroporous resin purification obtains the novel method of high-purity tea stain element again in conjunction with lyophilize.Advantage of the present invention: simple to operation, cost is low, is applicable to large production.1, microwave counter current extractive technique is the combination of dynamic extraction, countercurrent extraction, decoction extraction process, and extraction rate is fast, and extracts active ingredients is abundant, extracts yield high.2, macroporous resin relies on Van der Waals force, and carry out physical adsorption by its huge specific surface, the effective constituent after microwave extraction be further purified, resin is reusable, and production cost reduces greatly, can industrialization use.The present invention utilizes microwave counter current extractive technique to make extracts active ingredients abundant, is further purified with macroporous resin, then through lyophilize, gained white parmelia saxatilis tea stain element is active high, and purity brings up to 98.5%.
Description
Technical field:
The invention belongs to field of natural organic chemistry, relate to a kind of method extracting white parmelia saxatilis tea stain element from the wild white parmelia saxatilis of Daxing'an Mountainrange, particularly relating to one utilizes microwave counter current to extract, and macroporous resin purification obtains the novel method of high-purity tea stain element again in conjunction with lyophilize.
Background technology:
Wild white parmelia saxatilis is born on rock and bark.Originate in Daxinganling District exhale in, the ground such as A Moore.The many wrinkles of Bai Shihua thallus, diameter about 30 centimetres, above canescence, edge splits into most irregular lobe; Sliver tip is circular, and edge fecula bud, smoothly, micro-glossy, the close life of central pin bud, and black is more coarse, and lower edge department is level and smooth, matt, has rhizoid.Sub-device is few, cup-shaped, and diameter about 1 centimetre, has short handle; Spore is oval, and Room 1 is colourless.Bai Shihua mainly containing sekikaic acid, parmelia saxatilis tea stain element, still contains orcinol carboxylate methyl ester etc. in addition.Domestic general alcohol heat reflux extraction method, also exists service temperature high, the shortcomings such as unstable product quality, and difference of the present invention is to adopt microwave loss mechanisms, and the later stage adopts macroporous resin purification again in conjunction with cryodesiccated novel method.
Summary of the invention:
Advantage of the present invention: the main microwave counter current that adopts extracts, and macroporous resin purification is again in conjunction with cryodesiccated novel method.The inventive method is simple to operation, and cost is low, is applicable to large production.
For achieving the above object, the technical solution used in the present invention is:
A kind of microwave counter current that adopts extracts, and macroporous resin purification obtains the novel method of high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) dry white parmelia saxatilis thallus is crushed to 40-60 order, and add the alkali lye of 60-80% concentration, microwave extraction, microwave power is 300 ~ 600W, frequency 3000 ~ 10000MHz, and extraction time 60-80min extracts under certain temperature and solid-liquid ratio;
(2) by extracting solution through purpose ceramic-film filter at filtering accuracy 0.2-0.5 micron, filter under filter pressure 02-0.3MPa, 5-10m/s filtering velocity, most of impurity can be removed;
(3) macroporous resin adsorption:
After reclaiming alkali lye, by macroporous resin adsorption on gained solution, flow velocity is 3-5BV/h, and adsorption temp is 40-45 DEG C, and the aspect ratio of resin column is 8: 1-15: 1;
(4) ethanol elution:
At normal temperatures and pressures, with 1-3BV/h flow velocity, first use the removal of impurities of 5-10% ethanol, wash the water-soluble impurities such as the pigment in solution, tannin, inorganic salts off;
(5) alkali lye wash-out:
Wash-out is carried out at 1-3BV/h flow velocity, elution volume under being 6-8BV again, elutriant thin-layer chromatography tracking monitor (with white parmelia saxatilis element for reference substance contrast) with alkaline solution;
(6) crude extract is obtained:
Collection elutriant concentrates, and reclaim alkali lye, drying under reduced pressure, obtaining content is more than 65% work in-process meal;
(7) silica gel column chromatography:
Gained meal is dissolved in alkali lye and adds proper silica gel stirring, dried 60-80 mesh sieve, dry method loading, upper technical grade post silica gel column chromatography, and carry out wash-out with chloroform-methanol with 95 ~ 85: 2 ratios, tlc tracing detection, collect each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) lyophilize:
24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and obtain high purity white parmelia saxatilis tea stain element, its content is more than 98%.
Embodiment:
Case study on implementation 1: a kind of microwave counter current that adopts extracts, and macroporous resin purification obtains the novel method of high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) get 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, be warming up to 50 DEG C of microwave counter currents and extract under 8 times of solid-liquid ratio conditions, forward feeding, reverse water inlet, the flowing of material and water is reverse continuous dynamic flow, obtains extracting solution;
(2) by extracting solution through purpose ceramic-film filter filtering accuracy 0.2 micron, filter under filter pressure 0.2MPa, 5m/s filtering velocity, most of impurity can be removed;
(3) reclaim alkali lye, by macroporous resin adsorption on gained solution, model is 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 DEG C;
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use 5% ethanol removal of impurities, wash the water-soluble impurities such as the pigment in solution, tannin, inorganic salts off;
(5) carrying out wash-out at 1BV/h flow velocity, elution volume under being 6BV with the alkaline solution of 40%, 50%, 60%, 70%, 85%, 95% again, take reference substance as contrast, and elutriant thin-layer chromatography tracking monitor, collects elutriant;
(6) concentrated by elutriant, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine work in-process 4.17g;
(7) alkali lye gained meal being dissolved in 80% concentration adds proper silica gel and stirs, dried 60-80 mesh sieve, dry method loading, upper technical grade post 300 order silica gel column chromatography, and carry out wash-out with chloroform-methanol with 95 ~ 85: 2 ratios, tlc tracing detection, collects each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) 24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and vacuum degree control is at 10pa, and time of drying is 3h, and obtain high purity atranorine 2.68g, its content is 98.3%.
Case study on implementation 2: a kind of microwave counter current that adopts extracts, and macroporous resin purification obtains the novel method of high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) get the dry white parmelia saxatilis of 500g and be crushed to 50 orders, add 70% sodium hydroxide solution, at 500W, frequency 6000MHz, time 70min, be warming up to 60 DEG C of microwave counter currents and extract under 10 times of solid-liquid ratio conditions, forward feeding, reverse water inlet, the flowing of material and water is reverse continuous dynamic flow, obtains extracting solution;
(2) by extracting solution through purpose ceramic-film filter filtering accuracy 0.4 micron, filter under filter pressure 0.3MPa, 8m/s filtering velocity, most of impurity can be removed;
(3) reclaim alkali lye, by macroporous resin adsorption on gained solution, model is 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 DEG C;
(4) at normal temperatures and pressures, with 2BV/h flow velocity, first use 10% ethanol removal of impurities, wash the water-soluble impurities such as the pigment in solution, tannin, inorganic salts off;
(5) carrying out wash-out at 2BV/h flow velocity, elution volume under being 7BV with the alkaline solution of 40%, 50%, 60%, 70%, 85%, 95% again, take reference substance as contrast, and elutriant thin-layer chromatography tracking monitor, collects elutriant;
(6) concentrated by elutriant, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine work in-process 4.17g;
(7) alkali lye gained meal being dissolved in 85% concentration adds proper silica gel and stirs, dried 60-80 mesh sieve, dry method loading, upper technical grade post 200 order silica gel column chromatography, and carry out wash-out with chloroform-methanol with the ethanol of 95 ~ 85: 2 ratios or 60-70% concentration, tlc tracing detection, collects each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) 24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and vacuum degree control is at 12pa, and time of drying is 4h, and obtain high purity atranorine 2.76g, its content is 98.5%.
Case study on implementation 3: a kind of microwave counter current that adopts extracts, and macroporous resin purification obtains the novel method of high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) get the dry white parmelia saxatilis of 500g and be crushed to 60 orders, add 80% sodium hydroxide solution, at 600W, frequency 8000MHz, time 80min, be warming up to 60 DEG C of microwave counter currents and extract under 15 times of solid-liquid ratio conditions, forward feeding, reverse water inlet, the flowing of material and water is reverse continuous dynamic flow, obtains extracting solution;
(2) by extracting solution through purpose ceramic-film filter filtering accuracy 0.4 micron, filter under filter pressure 0.3MPa, 8m/s filtering velocity, most of impurity can be removed;
(3) reclaim alkali lye, by macroporous resin adsorption on gained solution, model is 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 DEG C;
(4) at normal temperatures and pressures, with 3BV/h flow velocity, first use 10% ethanol removal of impurities, wash the water-soluble impurities such as the pigment in solution, tannin, inorganic salts off;
(5) carrying out wash-out at 2BV/h flow velocity, elution volume under being 7BV with the alkaline solution of 40%, 50%, 60%, 70%, 85%, 95% again, take reference substance as contrast, and elutriant thin-layer chromatography tracking monitor, collects elutriant.
(6) concentrated by elutriant, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% atranorine method finished product 4.21g;
(7) alkali lye gained meal being dissolved in 90% concentration adds proper silica gel and stirs, dried 60-80 mesh sieve, dry method loading, upper technical grade post 300 order silica gel column chromatography, and carry out wash-out with 70% ethanolic soln, tlc tracing detection, collects each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) 24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and vacuum degree control is at 10pa, and time of drying is 4h, and obtain high purity atranorine 2.74g, its content is 98.09%.
Case study on implementation 4: a kind of microwave counter current that adopts extracts, and macroporous resin purification obtains the novel method of high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) get the dry white parmelia saxatilis of 500g and be crushed to 50 orders, add 80% sodium hydroxide solution, at 500W, frequency 10000MHz, time 70min, be warming up to 70 DEG C of microwave counter currents and extract under 10 times of solid-liquid ratio conditions, forward feeding, reverse water inlet, the flowing of material and water is reverse continuous dynamic flow, obtains extracting solution;
(2) by extracting solution through purpose ceramic-film filter filtering accuracy 0.5 micron, filter under filter pressure 0.2MPa, 10m/s filtering velocity, most of impurity can be removed;
(3) reclaim alkali lye, by macroporous resin adsorption on gained solution, model is 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 DEG C;
(4) at normal temperatures and pressures, with 3BV/h flow velocity, with 5% ethanol removal of impurities, the water-soluble impurities such as the pigment in solution, tannin, inorganic salts are washed off;
(5) wash-out is carried out at 2BV/h flow velocity, elution volume under being 7BV with the alkaline solution of 40%, 50%, 60%, 70%, 85%, 95% again.Take reference substance as contrast, elutriant thin-layer chromatography tracking monitor, collects elutriant;
(6) concentrated by elutriant, reclaim alkali lye, drying under reduced pressure, obtaining content is 65.47% tea stain element work in-process 4.13g;
(7) alkali lye gained meal being dissolved in 95% concentration adds proper silica gel and stirs, dried 60-80 mesh sieve, dry method loading, upper technical grade post 200 order silica gel column chromatography, and carry out wash-out with 60% ethanolic soln, tlc tracing detection, collects each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) 24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and vacuum degree control is at 12pa, and time of drying is 3h, and obtain high purity atranorine 2.71g, its content is 98.3%.
Claims (4)
1. one kind adopts microwave counter current to extract, and macroporous resin purification obtains the method for high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, its step is as follows:
(1) dry white parmelia saxatilis thallus is crushed to 40-60 order, and add the alkali lye of 60-80% concentration, microwave counter current extracts, and microwave power is 300 ~ 600W, frequency 3000 ~ 10000MHz, and extraction time 60-80min extracts under certain temperature and solid-liquid ratio;
(2) by extracting solution through purpose ceramic-film filter at filtering accuracy 0.2-0.5 micron, filter under filter pressure 0.2-0.4MPa, 5-10m/s filtering velocity, most of impurity can be removed;
(3) macroporous resin adsorption:
After reclaiming alkali lye, by macroporous resin adsorption on gained solution, flow velocity is 3-5BV/h, and adsorption temp is 40-45 DEG C; The aspect ratio of resin column is 8:1-15:1;
(4) ethanol elution:
At normal temperatures and pressures, with 1-3BV/h flow velocity, first use the removal of impurities of 5-10% ethanol, wash the water-soluble impurity in solution off, described water-soluble impurity is pigment, tannin, inorganic salts;
(5) alkali lye wash-out:
Wash-out is carried out at 1-3BV/h flow velocity, elution volume under being 6-8BV, elutriant thin-layer chromatography tracking monitor again, with white parmelia saxatilis element for reference substance contrast with alkaline solution;
(6) crude extract is obtained:
Collection elutriant concentrates, and reclaim alkali lye, drying under reduced pressure, obtaining content is more than 65% work in-process meal;
(7) silica gel column chromatography:
Gained meal is dissolved in alkali lye and adds proper silica gel stirring, dried 60-80 mesh sieve, dry method loading, upper technical grade post silica gel column chromatography, and carry out wash-out with chloroform-methanol with 95 ~ 85:2 ratio, tlc tracing detection, collect each stepwise elution liquid of white parmelia saxatilis tea stain element;
(8) lyophilize:
24h is frozen in gained liquid cooling, is placed in vacuum dryer, vacuumizes, and Heating temperature is 45 DEG C, takes out after dry certain hour, and obtain high purity white parmelia saxatilis tea stain element, its content is more than 98%;
Wherein, in described step (1), solid-liquid ratio is 1:5-10, and Extracting temperature is 40-50 DEG C;
Wherein, in described step (8), vacuum degree control is at 10 to 12pa, and time of drying is 3-4h.
2. one according to claim 1 adopts microwave counter current to extract, macroporous resin purification obtains the method for high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, it is characterized in that: in described step (3), resin model is the one in DA201, D101, HPD300, AB-8 resin.
3. one according to claim 2 adopts microwave counter current to extract, and macroporous resin purification obtains the method for high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, it is characterized in that: in described step (5), wash-out concentration of lye is 40%-95%.
4. one according to claim 3 adopts microwave counter current to extract, macroporous resin purification obtains the method for high purity white parmelia saxatilis tea stain element again in conjunction with lyophilize, it is characterized in that: in described step (7), silica gel 200-300 order, concentration of lye is 80%-95%.
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| 微波辅助提取天然产物有效成分工艺研究;王丽昀;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20110115(第01期);B016-439 * |
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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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