CN101709024B - Method for extracting and purifying resveratrol from polygonum cuspidatum - Google Patents
Method for extracting and purifying resveratrol from polygonum cuspidatum Download PDFInfo
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- CN101709024B CN101709024B CN200910212921.3A CN200910212921A CN101709024B CN 101709024 B CN101709024 B CN 101709024B CN 200910212921 A CN200910212921 A CN 200910212921A CN 101709024 B CN101709024 B CN 101709024B
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- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 235000021283 resveratrol Nutrition 0.000 title claims abstract description 14
- 229940016667 resveratrol Drugs 0.000 title claims abstract description 14
- 241001648835 Polygonum cuspidatum Species 0.000 title abstract 2
- 235000018167 Reynoutria japonica Nutrition 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000010612 desalination reaction Methods 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 244000153955 Reynoutria sachalinensis Species 0.000 claims description 42
- 235000003202 Reynoutria sachalinensis Nutrition 0.000 claims description 42
- 235000018991 trans-resveratrol Nutrition 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 239000000284 extract Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 238000011033 desalting Methods 0.000 claims description 10
- 150000001768 cations Chemical class 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 6
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 6
- 108010059892 Cellulase Proteins 0.000 claims description 5
- 229940106157 cellulase Drugs 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 235000013305 food Nutrition 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 235000012255 calcium oxide Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 108090000790 Enzymes Proteins 0.000 claims description 2
- 102000004190 Enzymes Human genes 0.000 claims description 2
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
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- PYIXHKGTJKCVBJ-UHFFFAOYSA-N Astraciceran Natural products C1OC2=CC(O)=CC=C2CC1C1=CC(OCO2)=C2C=C1OC PYIXHKGTJKCVBJ-UHFFFAOYSA-N 0.000 description 1
- NDVRQFZUJRMKKP-UHFFFAOYSA-N Betavulgarin Natural products O=C1C=2C(OC)=C3OCOC3=CC=2OC=C1C1=CC=CC=C1O NDVRQFZUJRMKKP-UHFFFAOYSA-N 0.000 description 1
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- 229930012538 Paclitaxel Natural products 0.000 description 1
- IHPVFYLOGNNZLA-UHFFFAOYSA-N Phytoalexin Natural products COC1=CC=CC=C1C1OC(C=C2C(OCO2)=C2OC)=C2C(=O)C1 IHPVFYLOGNNZLA-UHFFFAOYSA-N 0.000 description 1
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- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
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- 235000012054 meals Nutrition 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 229960001592 paclitaxel Drugs 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical class C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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- 239000001648 tannin Substances 0.000 description 1
- RCINICONZNJXQF-MZXODVADSA-N taxol Chemical compound O([C@@H]1[C@@]2(C[C@@H](C(C)=C(C2(C)C)[C@H](C([C@]2(C)[C@@H](O)C[C@H]3OC[C@]3([C@H]21)OC(C)=O)=O)OC(=O)C)OC(=O)[C@H](O)[C@@H](NC(=O)C=1C=CC=CC=1)C=1C=CC=CC=1)O)C(=O)C1=CC=CC=C1 RCINICONZNJXQF-MZXODVADSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for extracting and purifying resveratrol from polygonum cuspidatum, ethanol, iron salt and alkali are used as extraction media in the method, a multi-stage dynamic countercurrent extraction technology is adopted, and the steps of desalination, purification, acidification, enzymatic hydrolysis, concentration, impurity removal and the like are sequentially carried out extraction liquid, thereby preparing a resveratrol product. The method has the advantages of simple process, short operation time, low production cost, high extraction efficiency, no organic solvent and easy industrial production.
Description
Technical field
The present invention relates to the method for purification of chemical field, be specifically related to a kind of method of from giant knotweed, extracting purified resveratrol.
Background technology
Trans-resveratrol (Resveratrol is called for short Res) is the natural diphenylethylene polyphenol substance that produces in the plant materials, is a kind of non-flavonoid polyphenolic substance that contains the stilbene class formation.Trans-resveratrol is one type of phytoalexin that special medical health care function is arranged, HUMAN HEALTH is had remarkable effect; Because of its anticancer, reduce fat, prevent and treat cardiovascular disorder, anti-oxidant, delaying senility etc. plays a role clearly; And become another new green cancer therapy drug after taxol, being considered to the contemporary mankind has one of anti-cancer and cancer-preventing new drug of exploitation future most.This material has been widely used in industries such as food, Medicines and Health Product, the huge market demand at present.Particularly this material is after being proved it in 2006 hiv virus is had the obvious suppression effect; The market requirement further promotes; Worldwide started the exploitation and the research boom of trans-resveratrol once more, therefore, it is researched and developed had vast market prospect.
At present, see that the method for from giant knotweed, extracting trans-resveratrol that is stated from bibliographical information mainly contains Enzymatic Extraction, organic solvent extraction, alkaline aqueous solution extraction, microwave extraction and supercritical CO
2Extract etc.At publication number is that CN1566349A, name are called that disclosed technical scheme is in " a kind of method that from giant knotweed, prepare trans-resveratrol ": the giant knotweed extracting solution is added the enzymic hydrolysis extraction; Use the organic solvent extraction extracting solution; Reclaim organic solvent, further separate and make with extra care the trans-resveratrol product.At publication number is that CN1621401A, name are called that disclosed technical scheme is in " a kind of method of from giant knotweed, extracting high-purity resveratrol ": the giant knotweed dry rhizome meal of pre-treatment is added the certain amount of organic solvent refluxing extraction; Adopt the opposed polarity solvent refluxing to extract after reclaiming solvent; The recovery part solvent; Centrifugal, obtain the trans-resveratrol product after throw out water and the sorbent treatment.All need use more a large amount of toxic organic solvent in the employed technology of above-mentioned two schemes, be prone to cause organic solvent residual and environmental pollution in product, and there is more serious potential safety hazard in suitability for industrialized production.At publication number is that CN101348805A, name are called that disclosed technical scheme is in " a kind of technology of from plant, extracting trans-resveratrol ": extract with alkaline aqueous solution; Adjustment pH value is afterwards with the finings removal of impurities of flocculating; Filter; Filtrating adds enzymic hydrolysis, and filtration drying gets 50% trans-resveratrol bullion, and bullion gets 98% trans-resveratrol product after pH value gradient alkaline solution is handled.This scheme has overcome the shortcoming of using toxic organic solvent in the production engineering, but it exists the water yield big, and subsequent processing device pressure is big, the high deficiency of energy consumption; In addition, the control of the temperature of this technology is too high, and scope is too wide, is prone to cause the product oxygenolysis; Extract alkali and use sodium hydroxide, the viscosity that extracts solution is bigger, is prone to cause filter not smooth; Precipitate in the direct filtration aqueous solution the method for product, can make in a large amount of trans-resveratrol residuary water, cause productive rate to descend; Technology is not considered inorganic metal ion such as Ca
2+Removal, cause the product ash oontent to exceed standard.At publication number is in the report of CN1513822A, CN1513823A, has reported employing microwave and supercritical CO respectively
2Extract the method for trans-resveratrol, these method equipment costs are high, are difficult for suitability for industrialized production.
Summary of the invention
The objective of the invention is to: a kind of method of from giant knotweed, extracting purified resveratrol is provided, and this method is simple to operate, and production cost is low, and environmental pollution is little, and product purity and yield are high, are easy to suitability for industrialized production.
Technical solution of the present invention is that the step of this method is following:
(1) pulverizes: the giant knotweed rhizome is pulverized, crossed 14 mesh sieves and get the giant knotweed powder;
(2) extract: adding molysite and alkali get compound in the giant knotweed powder; Compound is placed four jars of pot group type dynamic counterflow extraction apparatus; The aqueous ethanolic solution that adds the concentration 60～70% of 4～6 times of giant knotweed grain weight amounts in jar; Gradation is stirred and is extracted under 45 ± 5 ℃ condition, and the plate-and-frame filter press of 300～500 order filter cloth specifications is crossed and filtered extracting solution;
(3) desalination: extracting solution is got desalting extracted liquid with the resin cation(R.C.) desalination;
(4) purifying: with the ethanol in the desalting extracted liquid reclaim the purifying extracting solution;
(5) acidifying: transfer pH to 4.5～5.5 to get acidizing extracting liquid the purifying extracting solution;
(6) enzymolysis: cellulase is added in the acidizing extracting liquid body, and enzyme dosage is 60～100Ug of giant knotweed grain weight amount
-1, 50 ± 5 ℃ of enzymolysis 6～8h of temperature get enzymolysis solution;
(7) concentrate: enzymolysis solution is concentrated, filters with imitative B strainer, separate throw out;
(8) removal of impurities: taking precipitate, the absolute ethyl alcohol of 10～20 times (W/V) of adding weight of precipitate, stirring and dissolving 20～30min filters, and filtrate recycling ethanol gets the trans-resveratrol product.
Wherein, the molysite in the said step (2) is food grade ferrous sulfate, ferric sulfate or bodied ferric sulfate, and its addition is 15～20% of a giant knotweed grain weight amount; Alkali is food grade calcium hydroxide or quicklime, and its addition is 8～10% of a giant knotweed grain weight amount; The time that the pot group type dynamic countercurrent extracts is a not good liquor 60～65min, two not good liquors, 50～55min, three not good liquors, 40～45min, four not good liquors, 30～35min.
Wherein, the resin cation(R.C.) model in the said step (3) is 001 * 14.5 or 001 * 16, and operational condition is flow velocity 3～5BVh
-1, blade diameter length ratio 1: 4～7.
Wherein, 45 ± 5 ℃ of the ethanol recovered temperatures in the said step (4), vacuum tightness-0.075～0.085MPa.
Wherein, the acidifying in the said step (5) is adopted Hydrogen chloride or is directly filled CO
2The gas adjust pH.
Wherein, the concentrated amount in the said step (7) is 1/2～1 times (W/V) of relative giant knotweed grain weight amount.
The present invention has following advantage:
1, extracts purge process not with an organic solvent, avoided the pollution of organic solvent environment and product.
2, adopt pot group type dynamic countercurrent technology, guaranteeing to have reduced solvent load greatly under the sufficient condition of extraction, saved energy consumption, reduced production cost, industrial prospect is good.
3, adopt ethanol liquid to add molysite and alkali, guaranteeing to have avoided the proposition of protein, phlegmatic temperament and tannin under the condition that target product fully extracts, realize extracting, the fusion of flocculation two steps, reduced extraction step, shortened the PT for extracting medium.
Embodiment
Through concrete embodiment technical solution of the present invention is detailed below, but technical solution of the present invention is not limited to following embodiment.
Embodiment 1:
The giant knotweed rhizome is crushed to 14 mesh sieves got the giant knotweed powder; Take by weighing 4 parts in 100kg giant knotweed powder, place the pot group type dynamic counterflow extraction apparatus respectively, each adds 15kg ferrous sulfate and 8kg quicklime; Each adds the aqueous ethanolic solution of 400kg concentration 60%, and 40 ℃ of gradation are stirred and extracted a not good liquor 60min; Two not good liquor 50min; Three not good liquor 40min, four not good liquor 30min, the plate-and-frame filter press of 300 order filter cloth specifications is crossed and is filtered extracting solution; Extracting solution is 3BVh with 001 * 14.5 resin cation(R.C.) in flow velocity
-1, blade diameter length ratio is that desalination gets desalting extracted liquid under 1: 4 the condition; Desalting extracted liquid is reclaimed ethanol in 40 ℃, vacuum tightness-0.075MPa get the purifying extracting solution; Transfer pH to 4.5 to get acidizing extracting liquid with Hydrogen chloride the purifying extracting solution; With cellulase 2.4 * 10
7U adds in the acidizing extracting liquid body, and 45 ℃ of temperature, enzymolysis 6h get enzymolysis solution; Enzymolysis solution is concentrated into 1/2 times (W/V) with respect to giant knotweed powder amount, filters with imitative B strainer, separate throw out; The absolute ethyl alcohol that adds its amount 10 times (W/V) in the throw out, stirring and dissolving 20min filters, and filtrate recycling ethanol gets trans-resveratrol product 4.47kg, and purity is 91.2%.
Embodiment 2:
The giant knotweed rhizome is crushed to 14 mesh sieves got the giant knotweed powder; Take by weighing 4 parts in 100kg giant knotweed powder, place the pot group type dynamic counterflow extraction apparatus respectively, each adds 17.5kg ferric sulfate and 9kg calcium hydroxide; Each adds the aqueous ethanolic solution of 500kg concentration 65%, and 45 ℃ of gradation are stirred and extracted a not good liquor 62min; Two not good liquor 52min; Three not good liquor 42min, four not good liquor 32min, the plate-and-frame filter press of 400 order filter cloth specifications is crossed and is filtered extracting solution; Extracting solution with 001 * 16 resin cation(R.C.) in flow velocity 4BVh
-1, blade diameter length ratio is that desalination gets desalting extracted liquid under 1: 5.5 condition; Desalting extracted liquid is got the purifying extracting solution in 45 ℃, the condition recover ethanol of vacuum tightness-0.08MPa; In the purifying extracting solution, charge into CO
2Gas transfers pH to 5.0 to get acidizing extracting liquid; With cellulase 3.2 * 10
7U adds in the acidizing extracting liquid body, and 50 ℃ of temperature, enzymolysis 7h get enzymolysis solution; Enzymolysis solution is concentrated into 3/4 times (W/V) with respect to giant knotweed grain weight amount, filters with imitative B strainer, separate throw out; The absolute ethyl alcohol that adds its amount 15 times (W/V) in the throw out, stirring and dissolving 25min filters, and filtrate recycling ethanol gets trans-resveratrol product 5.23kg, and purity is 93.1%.
Embodiment 3:
The giant knotweed rhizome is crushed to 14 mesh sieves got the giant knotweed powder; Take by weighing 4 parts in 100kg giant knotweed powder, place the pot group type dynamic counterflow extraction apparatus respectively, each adds 20kg bodied ferric sulfate and 10kg calcium hydroxide; Each adds the aqueous ethanolic solution of 600kg concentration 70%, and 50 ℃ of gradation are stirred and extracted a not good liquor 65min; Two not good liquor 55min; Three not good liquor 45min, four not good liquor 35min, the plate-and-frame filter press of 500 order filter cloth specifications is crossed and is filtered extracting solution; Extracting solution with 001 * 16 resin cation(R.C.) in flow velocity 5BVh
-1, blade diameter length ratio is that desalination gets desalting extracted liquid under 1: 7 the condition; Desalting extracted liquid is got the purifying extracting solution in 50 ℃, the condition recover ethanol of vacuum tightness-0.085MPa; Transfer pH to 5.5 to get acidizing extracting liquid in purifying extracting solution Hydrogen chloride; With cellulase 4.0 * 10
7U adds in the acidizing extracting liquid body, and 55 ℃ of temperature, enzymolysis 8h get enzymolysis solution; Enzymolysis solution is concentrated into 1 times (W/V) with respect to giant knotweed grain weight amount, filters with imitative B strainer, separate throw out; The absolute ethyl alcohol that adds its amount 20 times (W/V) in the throw out, stirring and dissolving 30min filters, and filtrate recycling ethanol gets trans-resveratrol product 3.64kg, and purity is 89.4%.
Claims (6)
1. method of from giant knotweed, extracting purified resveratrol is characterized in that the step of this method is following:
(1) pulverizes: the giant knotweed rhizome is pulverized, crossed 14 mesh sieves and get the giant knotweed powder;
(2) extract: adding molysite and alkali get compound in the giant knotweed powder; Compound is placed four jars of pot group type dynamic counterflow extraction apparatus; The aqueous ethanolic solution that adds the concentration 60～70% of 4～6 times of giant knotweed grain weight amounts in jar; Gradation is stirred and is extracted under 45 ± 5 ℃ condition, and the plate-and-frame filter press of 300～500 order filter cloth specifications is crossed and filtered extracting solution;
(3) desalination: extracting solution is got desalting extracted liquid with the resin cation(R.C.) desalination;
(4) purifying: with the ethanol in the desalting extracted liquid reclaim the purifying extracting solution;
(5) acidifying: transfer pH to 4.5～5.5 to get acidizing extracting liquid the purifying extracting solution;
(6) enzymolysis: cellulase is added in the acidizing extracting liquid body, and enzyme dosage is 60～100Ug of giant knotweed grain weight amount
-1, 50 ± 5 ℃ of enzymolysis 6～8h of temperature get enzymolysis solution;
(7) concentrate: enzymolysis solution is concentrated, filters with imitative B strainer, separate throw out;
(8) removal of impurities: taking precipitate, the absolute ethyl alcohol of 10～20 times of W/V of adding weight of precipitate, stirring and dissolving 20～30min filters, and filtrate recycling ethanol gets the trans-resveratrol product.
2. a kind of method of from giant knotweed, extracting purified resveratrol according to claim 1, it is characterized in that: the molysite in the said step (2) is food grade ferrous sulfate, ferric sulfate or bodied ferric sulfate, its addition is 15～20% of a giant knotweed grain weight amount; Alkali is food grade calcium hydroxide or quicklime, and its addition is 8～10% of a giant knotweed grain weight amount; The time that the pot group type dynamic countercurrent extracts is a not good liquor 60～65min, two not good liquors, 50～55min, three not good liquors, 40～45min, four not good liquors, 30～35min.
3. a kind of method of from giant knotweed, extracting purified resveratrol according to claim 1, it is characterized in that: the resin cation(R.C.) model in the said step (3) is 001 * 14.5 or 001 * 16, operational condition is flow velocity 3～5BVh
-1, blade diameter length ratio 1: 4～7.
4. a kind of method of from giant knotweed, extracting purified resveratrol according to claim 1 is characterized in that: 45 ± 5 ℃ of the ethanol recovered temperatures in the said step (4), and vacuum tightness-0.075～-0.085MPa.
5. a kind of method of from giant knotweed, extracting purified resveratrol according to claim 1, it is characterized in that: the acidifying in the said step (5) is adopted Hydrogen chloride or is directly filled CO
2The gas adjust pH.
6. a kind of method of from giant knotweed, extracting purified resveratrol according to claim 1, it is characterized in that: the concentrated amount in the said step (7) is 1/2～1 times of W/V of relative giant knotweed grain weight amount.
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| CN200910212921.3A CN101709024B (en) | 2009-11-06 | 2009-11-06 | Method for extracting and purifying resveratrol from polygonum cuspidatum |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1251361A (en) * | 1999-09-24 | 2000-04-26 | 四川省凉山州生物研究所 | Process for extracting resveratrol from Chinese medicine giant knotweed root |
| CN101348805A (en) * | 2007-07-20 | 2009-01-21 | 上海诺德生物实业有限公司 | Process for extracting resveratrol from plant |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1251361A (en) * | 1999-09-24 | 2000-04-26 | 四川省凉山州生物研究所 | Process for extracting resveratrol from Chinese medicine giant knotweed root |
| CN101348805A (en) * | 2007-07-20 | 2009-01-21 | 上海诺德生物实业有限公司 | Process for extracting resveratrol from plant |
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