CN1473822A - Extracting process of flavone and poly saccharide in duckweed - Google Patents
Extracting process of flavone and poly saccharide in duckweed Download PDFInfo
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- CN1473822A CN1473822A CNA031344585A CN03134458A CN1473822A CN 1473822 A CN1473822 A CN 1473822A CN A031344585 A CNA031344585 A CN A031344585A CN 03134458 A CN03134458 A CN 03134458A CN 1473822 A CN1473822 A CN 1473822A
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Abstract
The present invention relates to the extraction process of flavone compound and polysaccharide from duckweed. The extraction of flavone compound includes ethanol reflux extraction, rotary concentration, eliminating impurity with chitosan to flocculate and membrane to filter, vacuum drying and other steps. The extraction of polysaccharide includes material drying, defatting, reflux extraction, eliminating protein with acetocaustin, ethanol precipitation, purifying, dialysis, freeze drying and other steps. In the purifying step, ion exchange gel column chromatography or quaternary ammonium salt precipitation is adopted. The extracted flavone compound has relatively high bioactivity, and the polysaccharide product has natural structure and bioactivity of the duckweed polysaccharide.
Description
Technical field:
The invention relates to the extraction and separation process of effective constituent in the duckweed, relate to the technology of extraction flavonoid compound effective ingredient from duckweed and the extraction and separation process of polysaccharide, belong to biological pharmacy technical field.
Background technology:
Duckweed (Common Ducksmeat Herb) is the herb of plant and of its applications duckweed spirodela or blue or green duckweed, and is hot, cold, goes into lung channel, dispel the wind, and the sweating diuresis, detumescence, row water, heat-clearing, the toxicide effect, and can control lip cancer etc.Modern science studies show that and contain multiple flavonoid compound in the duckweed, and the content of polysaccharose substance is than horn of plenty, but is not much accounted of and big quantity research always.
The mensuration of relevant duckweed Chemical Composition, pharmacological action had some reports in recent years, but did not then appear in the newspapers for the extraction process of duckweed flavones and polysaccharide.
Summary of the invention:
The purpose of this invention is to provide and a kind ofly from natural duckweed, extract flavones, and improve as far as possible flavones content in the product technology and a kind of from duckweed its polysaccharide component of extraction separation, and can keep its bioactive technology preferably.
Duckweed flavones extraction process comprises alcohol reflux, concentrates, removal of impurities, goes up steps such as column purification and vacuum-drying.Its concrete implementation process is as follows:
A, alcohol reflux step comprise mixes 50%～70% the ethanol solid-liquid ratio with 1: 20 with duckweed, on water-bath, 50 ℃～80 ℃ following refluxing extraction 1.5～2.5 hours, filter and also collect filtrate and residue.Residue is mixed with ethanolic soln with concentration with 1: 20 solid-liquid ratio again, and refluxing extraction is 1.5～2 hours under uniform temp, filters and also collects filtrate, merges twice filtrate;
B, enrichment step comprise filtrate are placed on the rotatory evaporator, concentrate 10～12 hours down at 45 ℃, to remove ethanol fully;
C, flocculation step adopt flocculation removal of impurities or membrane filtration removal of impurities.
The flocculation removal of impurities comprises between pH value to 4.0～4.5 of regulating concentrated solution, add hot filtrate to 60 ℃, measuring a certain amount of 1% chitosan solution adds in the concentrated solution, make that chitosan content reaches 0.03%～0.06% in the concentrated solution, regulate rotating speed to the 700～1000r/min of mechanical stirrer, stir after 1.5 minutes, speed is reduced to 50～200r/min, stirred 15 minutes.The liquid that will flocculate leaves standstill 24 hours after-filtration, collects filtrate.
The membrane filtration removal of impurities comprises that with concentrated solution be to be 0.22 micron membrane filtration again with the aperture behind 0.45 micron the membrane filtration with the aperture earlier, and collection is through twice filtering filtrate;
D, the step that goes up column purification comprise crosses macroporous adsorbent resin with the filtrate after the flocculation with the velocity flow of 2 times of column volumes per hour, cross resin with the distilled water of 4 times of column volumes with identical velocity flow then, the most of impurity of flush away, cross resin with 70%～90% ethanolic soln of 2 times of column volumes with identical velocity flow again, the flavones that adsorbs on the resin is eluted, collect the elutriant of this part.
E, vacuum drying step comprise elutriant ethanol be placed in the vacuum drying oven, and attemperation to 50～60 ℃ can get yellow product after the drying.
Duckweed polysaccharide extraction and separation process comprises steps such as raw material drying, degreasing, refluxing extraction, trichloroacetic acid method deproteinated, ethanol sedimentation, purifying, dialysis and lyophilize.Below be the specific descriptions of duckweed polysaccharide extraction and separation process:
A, raw material drying step comprise with commercially available duckweed herb under 60 ℃ of temperature vacuum-drying to constant weight;
B, defatting step comprise the ethanol ether mixing solutions that added in the duckweed raw material by 1: 10 solid-liquid ratio 1: 1, reflux 2～4 hours at 50～60 ℃, filter, and collect filter residue;
C, refluxing extraction step comprise that the material-water ratio by 1: 20 adds distilled water in filter residue, and refluxing extraction is 2～3 times under 90～100 ℃, condition of normal pressure, each 2～3 hours;
D, trichloroacetic acid method deproteinated step are included in and add 3%～10% trichoroacetic acid(TCA) solution to extracting solution pH value be about 2～3 in the extracting solution of refluxing extraction, 5～10 ℃ of refrigerations are after about 24 hours, with 4000 rev/mins of frozen centrifugations below 5 ℃ 15 minutes, collect supernatant liquor, in 50 ℃ of following concentrating under reduced pressure;
E, ethanol sedimentation step are included in spissated extracting solution and add dehydrated alcohol and to make pure content surpass 80%, leave standstill after about 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation;
F, purification step can carry out in two ways, be respectively the ion-exchange gel column chromatography and the quaternary amine precipitator method: the ion-exchange gel column chromatography is to carry out column chromatography with DEAE-Sephadex A-25, elutriant is distilled water and 0.2～1.0mol/lHAc buffered soln or 0.2～1.0mol/lNaCl solution, also can distilled water and 1.0mol/lNaCl solution mixing gradient elution; The quaternary amine precipitator method are to handle extracting solution with 6～10%CTAB, the centrifuging and taking precipitation is dissolved with 10～15%NaCl, behind alcohol precipitation, get component a, add boric acid in the supernatant after CTAB handles, with NaOH accent PH11, the centrifuging and taking precipitation with 10～15%NaCl dissolving, gets component b with acid neutralization back behind alcohol precipitation again, supernatant after centrifugal is transferred PH4～5 with HCl, get component c behind the alcohol precipitation.
G, dialysis step comprise that the dialysis tubing with molecular weight cut-off＞8000 carries out flowing water and distill water dialysis more than 24 hours to elutriant, get and do not see through the liquid concentrating under reduced pressure;
H, lyophilize step comprised the polysaccharide extraction liquid lyophilize in Freeze Drying Equipment after handling through above-mentioned steps, 12～24 hours time of drying.
The flavones extraction process is simple to operate, cost is low, production safety, and shows that through efficient liquid phase chromatographic analysis flavonoid content is higher, and has higher biological activity.Polysaccharide extracting process is simple to operate, cost is low, production safety, and it is higher that sulfuric acid-phynol method detects total sugar content, and the product of preparing has kept the natural structure and the biological activity of duckweed polysaccharide preferably, has very high using value.
Embodiment: embodiment 1: extraction separation duckweed flavones according to the following steps.
With duckweed 15 grams is raw material, after moisture is removed in oven dry, adds 20 times 50% ethanolic soln, places on the water-bath, and refluxing extraction is 1.5 hours under 50 ℃ of conditions, filtering and collecting filter liquid and residue.50% the ethanolic soln that adds 20 times again in residue, 1.5 hours after-filtration of refluxing extraction merge filtrate twice under the same conditions.Filtrate is placed on the rotatory evaporator, concentrate 10 hours down, obtain 200 milliliters of concentrated solutions in 45 ℃.Regulate the pH value to 4.0 of concentrated solution, and be heated to 60 ℃, 6 milliliters of the chitosan solutions of adding 1%, the rotating speed of regulating mechanical stirrer is to 700r/min, stirred 1.5 minutes, the re-adjustment rotating speed stirred 15 minutes to 50r/min, after the liquid that will flocculate left standstill 12 hours, filtrate was collected in the elimination flocks.Pack into after the AB-8 macroporous adsorbent resin cleaned in the adsorption column.200 milliliters filtrates are crossed resin with the velocity flow of 2 times of column volumes per hour, after treating that resin fully adsorbs flavones, distilled water with 4 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 70% ethanolic soln of 2 times of column volumes is crossed resin with identical velocity flow, flavones is eluted, collect elutriant.Elutriant is placed vacuum drying oven, in 50 ℃ down dry, get final product light yellow product.Embodiment 2: extraction separation duckweed flavones according to the following steps.
With duckweed 15 grams is raw material, after moisture is removed in oven dry, adds 20 times 60% ethanolic soln, places on the water-bath, and refluxing extraction is 2 hours under 60 ℃ of conditions, filtering and collecting filter liquid and residue.60% the ethanolic soln that adds 20 times again in residue, 2 hours after-filtration of refluxing extraction merge filtrate twice under the same conditions.Filtrate is placed on the rotatory evaporator, concentrate 10～12 hours down, obtain 200 milliliters of concentrated solutions in 45 ℃.Regulate the pH value to 4.3 of concentrated solution, and be heated to 60 ℃, 8 milliliters of the chitosan solutions of adding 1%, the rotating speed of regulating mechanical stirrer is to 800r/min, stirred 1.5 minutes, the re-adjustment rotating speed stirred 15 minutes to 100r/min, after the liquid that will flocculate left standstill 24 hours, filtrate was collected in the elimination flocks.Pack into after the AB-8 macroporous adsorbent resin cleaned in the adsorption column.200 milliliters filtrates are crossed resin with the velocity flow of 2 times of column volumes per hour, after treating that resin fully adsorbs flavones, distilled water with 4 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 80% ethanolic soln of 2 times of column volumes is crossed resin with identical velocity flow, flavones is eluted, collect elutriant.Elutriant is placed vacuum drying oven, in 50 ℃ down dry, get final product the orange product.Embodiment 3: extraction separation duckweed flavones according to the following steps.
With duckweed 15 grams is raw material, after moisture is removed in oven dry, adds 20 times 70% ethanolic soln, places on the water-bath, and refluxing extraction is 2 hours under 70 ℃ of conditions, filtering and collecting filter liquid and residue.70% the ethanolic soln that adds 20 times again in residue, 2 hours after-filtration of refluxing extraction merge filtrate twice under the same conditions.Filtrate is placed on the rotatory evaporator, concentrate 10～12 hours down, obtain 200 milliliters of concentrated solutions in 45 ℃.Regulate the pH value to 4.5 of concentrated solution, and be heated to 60 ℃, 8 milliliters of the chitosan solutions of adding 1%, the rotating speed of regulating mechanical stirrer stirred 1.5 minutes to 1000r/min, and the re-adjustment rotating speed is to 150r/min, stirred 15 minutes, after the liquid that will flocculate left standstill 24 hours, filtrate was collected in the elimination flocks.Pack into after the AB-8 macroporous adsorbent resin cleaned in the adsorption column.200 milliliters filtrates are crossed resin with the velocity flow of 2 times of column volumes per hour, after treating that resin fully adsorbs flavones, distilled water with 4 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 90% ethanolic soln of 2 times of column volumes is crossed resin with identical velocity flow, flavones is eluted, collect elutriant.Elutriant is placed vacuum drying oven, in 60 ℃ down dry, get final product the tawny product.Embodiment 4: extraction separation duckweed flavones according to the following steps.
With duckweed 15g is raw material, after moisture is removed in oven dry, adds 20 times 60% ethanolic soln, places on the water-bath, and refluxing extraction is 2.5 hours under 80 ℃ of conditions, filtering and collecting filter liquid and residue.50% the ethanolic soln that adds 20 times again in residue, 2 hours after-filtration of refluxing extraction merge filtrate twice under the same conditions.Filtrate is placed on the rotatory evaporator, concentrate 10～12 hours down, obtain 200 milliliters of concentrated solutions in 45 ℃.Be behind 0.45 micron the membrane filtration with concentrated solution, filter with 0.22 micron film again, collect filtrate by the aperture.Pack into after the AB-8 macroporous adsorbent resin cleaned in the adsorption column.200 milliliters filtrates are crossed resin with the velocity flow of 2 times of column volumes per hour, after treating that resin fully adsorbs flavones, distilled water with 4 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 80% ethanolic soln of 2 times of column volumes is crossed resin with identical velocity flow, flavones is eluted, collect elutriant.Elutriant is placed vacuum drying oven, in 50 ℃ down dry, get final product the tawny product.Embodiment 5: extraction separation duckweed polysaccharide according to the following steps.
Get under 60 ℃ of temperature of 15g duckweed herb vacuum-drying to constant weight; The ethanol ether mixing solutions 150ml that adds 1: 1 in raw material refluxed 2 hours at 50 ℃, filtered, and collected filter residue; Add distilled water 300ml in filter residue, refluxing extraction is 3 hours under 90 ℃, condition of normal pressure, and suction filtration adds distilled water 300ml again in filter residue, and with condition refluxing extraction 2 hours, suction filtration merged filtrate twice; In extracting solution, add 3% trichoroacetic acid(TCA) solution to extracting solution pH value and be 2,5 ℃ of refrigerations after 24 hours,, collect supernatant liquor, under 50 ℃, be evaporated to 20ml with 4000 rev/mins of frozen centrifugations 15 minutes; In spissated extracting solution, adding dehydrated alcohol 80ml, leave standstill after 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation; The DEAE-SephadexA-25 column chromatography, normal temperature, flow velocity 15ml/h, elutriant are distilled water and 0.5mol/lHAc buffered soln, collect this two portions elutriant respectively; With the dialysis tubing of molecular weight cut-off 8000 elutriant is carried out 24 hours flowing water and distill water dialysis, get and do not see through the liquid concentrating under reduced pressure; Polysaccharide extraction liquid lyophilize in Freeze Drying Equipment that will be after above-mentioned steps is handled, 12 hours time of drying, white and tawny polysaccharide powder material.Embodiment 6: extraction separation duckweed polysaccharide according to the following steps.
Get under 60 ℃ of temperature of 20g duckweed herb vacuum-drying to constant weight; The ethanol ether mixing solutions 200ml that adds 1: 1 in raw material refluxed 4 hours at 60 ℃, filtered, and collected filter residue; Add distilled water 400ml in filter residue, refluxing extraction is 3 hours under 100 ℃, condition of normal pressure, and suction filtration repeats this operation twice with condition, merges three times filtrate; In extracting solution, add 6% trichoroacetic acid(TCA) solution to extracting solution pH value and be 3,10 ℃ of refrigerations after 24 hours,, collect supernatant liquor, under 50 ℃, be evaporated to 40ml with 4000 rev/mins of frozen centrifugations 15 minutes; In spissated extracting solution, adding dehydrated alcohol 160ml, leave standstill after 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation; DEAE-Sephadex A-25 column chromatography, normal temperature, flow velocity 15ml/h, elutriant are distilled water and 0.5mol/lNaCl buffered soln, collect this two portions elutriant respectively; With the dialysis tubing of molecular weight cut-off 14000 elutriant is carried out 48 hours flowing water and distill water dialysis, get and do not see through the liquid concentrating under reduced pressure; Polysaccharide extraction liquid lyophilize in Freeze Drying Equipment that will be after above-mentioned steps is handled, 24 hours time of drying, white and faint yellow polysaccharide powder material.Embodiment 7: extraction separation duckweed polysaccharide according to the following steps.
Get under 60 ℃ of temperature of 15g duckweed herb vacuum-drying to constant weight; The ethanol ether mixing solutions 150ml that adds 1: 1 in raw material refluxed 3 hours at 60 ℃, filtered, and collected filter residue; Add distilled water 300ml in filter residue, refluxing extraction is 3 hours under 100 ℃, condition of normal pressure, and suction filtration adds distilled water 300ml again in filter residue, and with condition refluxing extraction 3 hours, suction filtration merged filtrate twice; In extracting solution, add 10% trichoroacetic acid(TCA) solution to extracting solution pH value and be 2.5,5 ℃ of refrigerations after 24 hours,, collect supernatant liquor, under 50 ℃, be evaporated to 20ml with 4000 rev/mins of frozen centrifugations 15 minutes; In spissated extracting solution, adding dehydrated alcohol 80ml, leave standstill after 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation; DEAE-Sephadex A-25 column chromatography, normal temperature, flow velocity 15ml/h, with distilled water and 1.0mol/lNaCl solution mixing gradient elution, sulfuric acid-phynol method detects, and collects elutriant by peak position; With the dialysis tubing of molecular weight cut-off 14000 elutriant is carried out 48 hours flowing water and distill water dialysis, get and do not see through the liquid concentrating under reduced pressure; Polysaccharide extraction liquid lyophilize in Freeze Drying Equipment that will be after above-mentioned steps is handled, 18 hours time of drying, oyster white and faint yellow polysaccharide powder material.Embodiment 8: extraction separation duckweed polysaccharide according to the following steps.
Get under 60 ℃ of temperature of 15g duckweed herb vacuum-drying to constant weight; The ethanol ether mixing solutions 150ml that adds 1: 1 in raw material refluxed 3 hours at 60 ℃, filtered, and collected filter residue; Add distilled water 300ml in filter residue, refluxing extraction is 3 hours under 100 ℃, condition of normal pressure, and suction filtration adds distilled water 300ml again in filter residue, and with condition refluxing extraction 3 hours, suction filtration merged filtrate twice; In extracting solution, add 10% trichoroacetic acid(TCA) solution to extracting solution pH value and be 2.5,5 ℃ of refrigerations after 24 hours,, collect supernatant liquor, under 50 ℃, be evaporated to 20ml with 4000 rev/mins of frozen centrifugations 15 minutes; In spissated extracting solution, adding dehydrated alcohol 80ml, leave standstill after 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation; Dissolution precipitation is also handled with 6%CTAB, the centrifuging and taking precipitation is dissolved with 10%NaCl, behind alcohol precipitation, get component a, add boric acid in the supernatant after CTAB handles, with NaOH accent PH11, the centrifuging and taking precipitation with the 10%NaCl dissolving, gets component b with acid neutralization back behind alcohol precipitation again, supernatant after centrifugal is transferred PH5 with HCl, get component c behind the alcohol precipitation; With the dialysis tubing of molecular weight cut-off 14000 elutriant is carried out 48 hours flowing water and distill water dialysis, get and do not see through the liquid concentrating under reduced pressure; Polysaccharide extraction liquid lyophilize in Freeze Drying Equipment that will be after above-mentioned steps is handled, 18 hours time of drying, the polysaccharide powder material.Embodiment 9: extraction separation duckweed polysaccharide according to the following steps.
Get under 60 ℃ of temperature of 20g duckweed herb vacuum-drying to constant weight; The ethanol ether mixing solutions 200ml that adds 1: 1 in raw material refluxed 4 hours at 60 ℃, filtered, and collected filter residue; Add distilled water 400ml in filter residue, refluxing extraction is 3 hours under 100 ℃, condition of normal pressure, and suction filtration repeats this operation twice with condition, merges three times filtrate; In extracting solution, add 6% trichoroacetic acid(TCA) solution to extracting solution pH value and be 3,10 ℃ of refrigerations after 24 hours,, collect supernatant liquor, under 50 ℃, be evaporated to 40ml with 4000 rev/mins of frozen centrifugations 15 minutes; In spissated extracting solution, adding dehydrated alcohol 160ml, leave standstill after 24 hours with 4000 rev/mins centrifugal 15 minutes, collecting precipitation; Dissolution precipitation is also handled with 10%CTAB, the centrifuging and taking precipitation is dissolved with 15%NaCl, behind alcohol precipitation, get component a, add boric acid in the supernatant after CTAB handles, with NaOH accent PH11, the centrifuging and taking precipitation with the 15%NaCl dissolving, gets component b with acid neutralization back behind alcohol precipitation again, supernatant after centrifugal is transferred PH4 with HCl, get component c behind the alcohol precipitation; With the dialysis tubing of molecular weight cut-off 14000 elutriant is carried out 48 hours flowing water and distill water dialysis, get and do not see through the liquid concentrating under reduced pressure; Polysaccharide extraction liquid lyophilize in Freeze Drying Equipment that will be after above-mentioned steps is handled, 24 hours time of drying, white and faint yellow polysaccharide powder material.
Claims (5)
1. technology of from duckweed, extracting flavonoid compound, comprise alcohol reflux, concentrate, removal of impurities, go up steps such as column purification, vacuum-drying, it is characterized in that, alcohol reflux is to be 50%～70% ethanol with 1: 20 solid-liquid ratio in 50 ℃～80 ℃ following refluxing extraction 1.5～2.5h with concentration, and the ethanol of using same concentrations again was with solid-liquid ratio refluxing extraction 1.5～2h under same temperature of 1: 20; Concentrating is under 45 ℃, and extracting solution is placed vacuum rotary evaporator, concentrates 10～12 hours, to remove ethanol fully; Removal of impurities can be adopted flocculate with chitosan method or membrane filter method; Last column purification is that the filtrate after the flocculation is carried out purifying through macroporous adsorbent resin, and it is 70%～90% ethanol that elutriant is selected concentration for use, collects elutriant; Drying is after elutriant is removed most of ethanol, to place vacuum drying oven, can get the yellow product of slightly carrying after 50～60 ℃ of following dryings.
2. the extraction process of flavonoid compound in the duckweed according to claim 1, it is characterized in that removal of impurities employing flocculate with chitosan method, its process is the chitosan solution of adding a certain amount of 1% in concentrated solution, make the chitosan concentration in the concentrated solution reach 0.03%～0.06%, and regulate pH value to 4.0～5.0 of concentrated solution, temperature to 60 ℃, stirred soon 1.5 minutes, slowly stirred 15 minutes, and left standstill 24 hours after-filtration then, collect whole filtrates.
3. the extraction process of duckweed flavones according to claim 1 is characterized in that it is to be earlier 0.45 micron membrane filtration with the aperture with extracting concentrated solution that membrane filter method, its process are adopted in removal of impurities, is 0.22 micron membrane filtration again with the aperture.
4, a kind of technology of from duckweed, extracting polysaccharide, comprise steps such as raw material drying, degreasing, refluxing extraction, trichloroacetic acid method deproteinated, ethanol sedimentation, purifying, dialysis and lyophilize, it is characterized in that: defatting step is the ethanol ether mixing solutions that added in the duckweed raw material by 1: 10 solid-liquid ratio 1: 1, refluxes 2～4 hours at 50～60 ℃; The refluxing extraction step is to add distilled water by 1: 20 material-water ratio in filter residue, and refluxing extraction is 2～3 times under 90～100 ℃, condition of normal pressure, each 2～3 hours; Trichloroacetic acid method deproteinated step is at the trichoroacetic acid(TCA) solution that adds 3%～10% in the extracting solution of refluxing extraction, and 5～10 ℃ of refrigerations are after about 24 hours, with 4000 rev/mins of frozen centrifugations below 5 ℃; The ethanol sedimentation step is to add dehydrated alcohol and make pure content surpass 80% in spissated extracting solution, leaving standstill after about 24 hours centrifugal 15 minutes with 4000 rev/mins; Purification step is to handle with the ion-exchange gel column chromatography or with the quaternary amine precipitator method; The dialysis step is that the dialysis tubing with molecular weight cut-off＞8000 carries out flowing water and distill water dialysis more than 24 hours to elutriant.
5, according to the purification step of the described duckweed polysaccharide of claim 4 extraction and separation process, it is characterized in that: the ion-exchange gel column chromatography is to carry out column chromatography with DEAE-Sephadex A-25, elutriant is distilled water and 0.2～1.0mol/lHAc buffered soln or 0.2～1.0mol/lNaCl solution, also can distilled water and 1.0mol/lNaCl solution mixing gradient elution; The quaternary amine precipitator method are to handle extracting solution with 6～10%CTAB, the centrifuging and taking precipitation is dissolved with 10～15%NaCl, behind alcohol precipitation, get component a, add boric acid in the supernatant after CTAB handles, with NaOH accent PH11, the centrifuging and taking precipitation with 10～15%NaCl dissolving, gets component b with acid neutralization back behind alcohol precipitation again, supernatant after centrifugal is transferred PH4～5 with HCl, get component c behind the alcohol precipitation.
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| WO2007017244A2 (en) * | 2005-08-10 | 2007-02-15 | Sandoz Ag | A PROCESS FOR THE PURIFICATION OF SUBSTITUTED 2-(2-PYRIDYLMETHYL)SULFINYL-lH-BENZIMIDAZOLE COMPOUNDS BY PRECIPITATION IN THE PRESENCE OF A QUATERNARY AMMONIUM SALT |
| WO2007017244A3 (en) * | 2005-08-10 | 2007-04-26 | Sandoz Ag | A PROCESS FOR THE PURIFICATION OF SUBSTITUTED 2-(2-PYRIDYLMETHYL)SULFINYL-lH-BENZIMIDAZOLE COMPOUNDS BY PRECIPITATION IN THE PRESENCE OF A QUATERNARY AMMONIUM SALT |
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| CN103417757A (en) * | 2013-08-03 | 2013-12-04 | 武汉诺贝药业有限公司 | Emulsifiable paste for treating eczema |
| CN103417758A (en) * | 2013-08-03 | 2013-12-04 | 武汉诺贝药业有限公司 | Application of nuphar pumilum total flavone extract in preparation of medicine for treating eczema |
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