CN1986029A - Effective plant component extracting process - Google Patents
Effective plant component extracting process Download PDFInfo
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- CN1986029A CN1986029A CN 200510130852 CN200510130852A CN1986029A CN 1986029 A CN1986029 A CN 1986029A CN 200510130852 CN200510130852 CN 200510130852 CN 200510130852 A CN200510130852 A CN 200510130852A CN 1986029 A CN1986029 A CN 1986029A
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Abstract
The effective plant component extracting process includes mechanically crushing the mixture of solid plant material and proper amount of chemical assistant, and the subsequent extraction of the effective component with water or alcohol. The mechanical crushing can produce micro shearing strain in the interface, break cell wall, expose fresh cut surface and produce mutual adsorption and other action between the grain clusters and molecular groups of the chemical assistant and the effective component, so as to alter the microscopic performance of the effective plant component, raise the leached amount by 80-400 %, short the extracting period greatly, raise the extracting efficiency obviously raise the extraction specificity and selectivity, minimize the organic solvent in use, lower the extraction cost and raise the bioavailability of the extracted matter.
Description
Technical field
The invention belongs to biological technical field, relate to effective plant component extracting process.
Background technology
The plant effective medicinal components is present in the vacuole in the cellular plasm usually, when cell is intact, the first infiltration of plants of solvent palpus surface, see through cell membrane and cell membrane then, enter cell tissue, dissolving active ingredient, born of the same parents form concentration difference outward in the born of the same parents, force the high concentration leachate to spread from inside to outside, rare leachate or fresh solvent are replaced dense leachate at any time, finish a leaching process.This is the conventional method dipping, diacolation, the basic principle of effective component extractings such as Soxhlet refluxing extraction and Dynamic Extraction, and complete cell membrane and cell membrane can form resistance to disengaging of active ingredient, resistance increases and increases with cell mass inner cell quantity, therefore conventional method only can rely on and use a large amount of organic solvents, prolong the extraction time, the re-extract step extracts repeatedly, this certainly will cause operating procedure lengthy and jumbled, time is long, the energy consumption high extracting efficiency is low, add because of particularly a large amount of uses of organic solvent of solvent, cause part active ingredient inactivation, loss, even harm humans health, pollute surrounding environment.Along with progress of science and technology and development, the appearance of extractive techniques such as ultrasonic wave, microwave, overcritical, ultramicro grinding, though compare with conventional art and to have marked improvement, but its essence all is the different physical means of utilization, make plant granule group or micel generation physical change, quicken active ingredient and be dissolved in solvent, do not change the dissolubility of active ingredient, be that original non-polar effective components still needs organic solvent to dissolve extraction, thus some active ingredient since poorly water-soluble, problem that bioavilability is low do not solved at all; And specificity is relatively poor, and some active ingredient can not realize the directed extraction of specificity; Because some technology of use of special installation also only limits to laboratory research, can't be applied to industrial production.Therefore the imperfection of upstream extractive technique is restricting more deep research of effective ingredients in plant and potential development prospect for a long time.
Summary of the invention
The objective of the invention is to overcome that the effective ingredients in plant extraction efficiency is lower in the prior art, effective component extraction rate is lower, the effective ingredient bioavilability is low, the technical problem of solvent contamination environment and effective ingredient provides a kind of method that effective ingredients in plant extracts that is used for.After being the mixture of mechanical crushing solid plant material and an amount of chemical assistant, select water or alcohol extract active ingredient for use, this method also can be called little shear-auxiliary agent and make technology mutually.
The present invention is used for the method that effective ingredients in plant extracts, it is characterized in that: the plant material that is extracted is pulverized, in the plant meal, add the chemical assistant of 0.5%-20% solid base, solid acid, sucrose or salt compounds powder, mechanical crushing together again, select water or ethanol dissolving crushed material for use, separated and collected solubility component obtains active ingredient.When utilizing mechanical crushing solid plant material, this method produces little shear between the interface, cell membrane is broken, fresh tangent plane is exposed, cluster of grains or the mutual absorption of micel or the principle of effect take place between chemical assistant and the active ingredient, overcome the shortcoming of existing technology, from the source, thoroughly solved the long-term at present technical bottleneck that restricts the plant extracts research and development.
The objective of the invention is to realize by following further technical scheme:
1. plant material preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing is to the 40-100 order;
2. add the 0.5%-20% chemical assistant in the plant meal, the suitableeest addition is 1%-10%, and this chemical assistant can be that solid base, solid acid, sucrose or salt compounds are (as Na
2CO
3) etc.;
3. select for use equipment such as the planetary mills that can produce shear action or vibromill that the mixture that is obtained by step 2 is handled processing time 1～60min;
4. the crushed material of selecting for use the dissolving of water or ethanol to obtain by step 3, centrifugal, filter, collect soluble component;
5. the active ingredient that is obtained by step 4 may be the mixture of single active ingredient or plurality of active ingredients, is single active ingredient if extract purpose, can select for use proper method such as extraction, crystallization to further separation of mixture, purifying and refining;
6. by step 4 or the single active ingredient of 5 plants that obtain or mixture useful as drug, food, functional food, food additives, veterinary drug or the feed addictive of plurality of active ingredients.
The described method that is used for the effective ingredients in plant extraction, the plant of indication comprises Chinese herbal medicine, wild plant and agricultural byproducts.
The described method that is used for the effective ingredients in plant extraction is characterized in that: utilize this method can obtain single active ingredient or the mixture of plurality of active ingredients or the crushed material of whole plant of plant.
The inventive method is compared with existing technology, has following advantage:
1. during mechanical crushing, the mutual absorption or the interaction of chemical assistant and active ingredient chemical group have changed the micro-property of effective ingredients in plant, and ability water-soluble or ethanol significantly improves, and extracted amount improves 80%～400%;
2. some active ingredient is because of water-soluble enhancing, and biologically active improves, and bioavilability increases;
3. can realize a kind of of certain plant or a few active ingredient are carried out the directional selectivity extraction, reduce the separation and Extraction step;
4. chemical assistant can accelerate to destroy solid plant material surface, and the surface that has reduced cluster of grains or micel can, make easier depolymerization dispersion between cluster of grains or micel, play the auxiliary effect of pulverizing, shorten the pulverizing time, avoid the active ingredient inactivation, improve crush efficiency, reduce the wearing and tearing of mechanical implement;
5. simplify the extraction process of active ingredient, shorten extraction time, reach both shorten the production cycle, energy savings, improve the purpose of the comprehensive utilization ratio of raw material again;
With water or ethanol as primary solvent, reduce or avoided the use of organic reagent to greatest extent, the technical process environmental protection is nuisanceless;
7. the mechanical crushing equipment that can produce shear action routinizes, and the processing ability is strong, and practice is easy to put into production;
8. obtain the plant extracts free from extraneous odour, no solvent residue.
The specific embodiment
Embodiment 1
Wilsonii 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 60 order adds the Na of 10 grams
2CO
3, planetary mills is pulverized, and obtains handling powder N
1
Take by weighing every part of 5g respectively and handle powder N
1Pulverize 60 purpose wilsonii medicinal materials (GC) with routine, add 50ml distilled water, 20% ethanol respectively, normal temperature lixiviate 48 hours.After filtering with gauze, absorbent cotton, water carried with 20% alcohol extract place 50 ℃ of water bath methods, weigh respectively.Yield sees Table 1:
Table 1
| Sample | Quality (g) | Yield (%) |
| GC-water N 1-water GC-20% ethanol N 1-20% ethanol | 0.2458 0.4586 0.2528 0.4045 | 4.92 10.4 5.06 8.09 |
Embodiment 2
Wilsonii 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 60 order adds the NaHCO of 20 grams
3, planetary mills is pulverized, and obtains handling powder N
2
Take by weighing every part of 5g and handle powder N
2Pulverize 60 purpose wilsonii medicinal materials (GC) with routine, add 50ml distilled water, 20% ethanol respectively, normal temperature lixiviate 48 hours.After filtering with gauze, absorbent cotton, water carried with 20% alcohol extract place 50 ℃ of water bath methods, weigh respectively.Yield sees Table 2:
Table 2
| Sample | Quality (g) | Yield (%) |
| GC-water N 2-water GC-20% ethanol N 2-20% ethanol | 0.2458 0.5226 0.2528 0.3750 | 4.92 9.17 5.06 7.50 |
Embodiment 3
Wilsonii 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 60 order adds the NaOH of 5 grams, and planetary mills is pulverized, and obtains handling powder N
3
Take by weighing every part of 5g respectively and handle powder N
3Pulverize 60 purpose wilsonii medicinal materials (GC) with routine, add 50ml distilled water, 20% ethanol respectively, normal temperature lixiviate 48 hours.After filtering with gauze, absorbent cotton, water carried with 20% alcohol extract place 50 ℃ of water bath methods, weigh respectively.Yield sees Table 3:
Table 3
| Sample | Quality (g) | Yield (%) |
| GC-water N 3-water GC-20% ethanol N 3-20% ethanol | 0.2458 0.5900 0.2528 0.4510 | 4.92 11.8 5.06 9.02 |
Isofraxidin Determination on content and comparison in embodiment 4 wilsoniis
Wilsonii 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 60 order, planetary mills is pulverized and is obtained handling powder N.
Wilsonii 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 60 order adds the KOH of 2.5 grams, and planetary mills is pulverized to such an extent that handle powder N
4
High performance liquid chromatography detects wilsonii (60 order), N, N
1, N
2, N
3And N
4Extract isofraxidin content (table 4).
Table 4
| Wilsonii (60 order) | N | N 1 | N 2 | N 3 | N 4 | |
| Isofraxidin (mg/g) | 0.027 | 0.050 | 0.080 | 0.079 | 0.082 | 0.071 |
Embodiment 5
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 70 order mixes with 1: 20 ratio with water, gets proper amount of normal-temperature and stirs and extract 40min, filter, crude extract 1 (XC1); Get equivalent refluxing extraction 40min again, filter, get crude extract 2 (XC2).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 70 order mixes with 1: 20 ratio with 90% methyl alcohol, gets proper amount of normal-temperature and stirs and extract 40min down, filter, crude extract 3 (XC3); Get equivalent refluxing extraction 40min again, filter, get crude extract 4 (XC4).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 70 order removal of impurities, drop in the high energy vibration grinder, grind 15min, get an amount of crushed material and mix with 1: 20 ratio with water, stirring at normal temperature is extracted 40min, and room temperature is centrifugal, collects supernatant (XJ1); Get equivalent refluxing extraction 40min again, room temperature is centrifugal, collects supernatant (XJ2).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 70 order removal of impurities, drop in the high energy vibration grinder, grind 15min, get an amount of crushed material and mix with 1: 20 ratio with 75% ethanol, extract 40min under the stirring at normal temperature, room temperature is centrifugal, collects supernatant (XJ3); Get equivalent again and mix with 1: 20 ratio with 75% ethanol, refluxing extraction 40min, room temperature is centrifugal, collects supernatant (XJ4).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 70 order removal of impurities, with the solid oxalic acid powder of 15 grams, drop in the high energy vibration grinder, grind 10min, take out material, mix with 1: 20 ratio with water, stirring at room is extracted 40min.Room temperature is centrifugal, collects supernatant, promptly gets crude extract (XHW1).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 70 order, with the solid benzoic acid powder of 25 grams, other operations are the same, must crude extract (XHW2).
Golden cypress 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 70 order mixes with the potassium dihydrogen phosphate powder of 15 grams, and other operations are the same, must crude extract (XHW3).
The mensuration of content of berberine in the golden cypress: get the each part mentioned above crude extract, cross the filtration of 0.45 μ m filter membrane and promptly get need testing solution.Use high performance liquid chromatography, detect content of berberine in each extract.
Table 6
Embodiment 6
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 100 order mixes with 1: 20 ratio with water, gets proper amount of normal-temperature and stirs and extract 40min, filter, crude extract 1 (YC1); Get equivalent refluxing extraction 40min again, filter, get crude extract 2 (YC2).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 100 order mixes with 1: 20 ratio with 80% ethanol, gets proper amount of normal-temperature and stirs and extract 40min down, filter, crude extract 3 (YC3); Get equivalent refluxing extraction 40min again, filter, get crude extract 4 (YC4).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 100 order removal of impurities, drop into centrifugal mill, handle 15min, get an amount of crushed material and mix with 1: 20 ratio with water, stirring at normal temperature is extracted 40min, and room temperature is centrifugal, collects supernatant (YJ1); Get equivalent refluxing extraction 40min again, room temperature is centrifugal, collects supernatant (YJ2).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 100 order removal of impurities, drop into centrifugal mill, handle 10min, get an amount of crushed material and mix with 1: 20 ratio with 65% ethanol, extract 40min under the stirring at normal temperature, room temperature is centrifugal, collects supernatant (YJ3); Get equivalent again and mix with 1: 20 ratio with 65% ethanol, refluxing extraction 40min, room temperature is centrifugal, collects supernatant (YJ4).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 100 order with the KOH powder of 5 grams, drops into centrifugal mill, handles 8min, takes out material, mixes stirring at room extraction 40min with 1: 20 ratio with water.Room temperature is centrifugal, collects supernatant, promptly gets crude extract (YHW1).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, and coarse crushing to 100 order is with the Na of 7.5 grams
2C0
3Powder, other operations are the same, get crude extract (YHW2).
Radix Isatidis 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 100 order, with the gluconic acid sodium salt powder of 100 grams, other operations are the same, must crude extract (YHW3).
Capillary electrophoresis detects organic acid content in the said extracted liquid respectively.
Table 7
Embodiment 7
Buy homemade stabilizing rice bran, take by weighing 100g, dose the sucrose of 3.5 grams behind coarse crushing 90 orders, take out after handling 7min in the multidimensional of packing into the swing type ball mill, be dissolved in water (1: 5) centrifugal 25min, the content of γ-Hi-Z in the determined by ultraviolet spectrophotometry centrifugate.
Table 8
| Hydrotrope recovery rate (%) | γ-Hi-Z content (%) | |
| Conventional method this law | 12.5 30.8 | 0.75 1.44 |
Embodiment 8
Sophora bud 500g preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 40 order removal of impurities, ultra violet lamp deactivation rue enzyme adds 50kg water, adds the 4g borax, transferring pH value of solution with milk of lime is 8, behind the refluxing extraction 2h, transfer pH value of solution 2～3 with hydrochloric acid, placement is spent the night, crystallization is all separated out, suction filtration gets the rutin crude product, add boiling water recrystallization after, faint yellow rutin.In oven dry below 80 ℃, mensuration content is 46.5g.
Sophora bud 500g, preliminary treatment, is dried to water content and is not higher than 20%, coarse crushing to 40 order removal of impurities, ultra violet lamp deactivation rue enzyme, add the borax of 50 grams and the mixture of milk of lime, planetary mills is handled 5min, takes out to be dissolved in 50Kg water, transfer pH value of solution 2～3 with hydrochloric acid, suction filtration gets the rutin crude product behind the 3h, add boiling water recrystallization after, faint yellow rutin.In oven dry below 80 ℃, mensuration content is 90.6g.
Sophora bud 500g, preliminary treatment, is dried to water content and is not higher than 20% removal of impurities, coarse crushing to 40 order, ultra violet lamp deactivation rue enzyme adds the Na of 40 grams
3PO
4Mixture, planetary mills is handled 5min, takes out to be dissolved in 50Kg water, transfers pH value of solution 2～3 with hydrochloric acid, suction filtration gets the rutin crude product behind the 3h, add the boiling water recrystallization after, faint yellow rutin.In oven dry below 80 ℃, mensuration content is 88.4g.
Claims (6)
1. one kind is used for the method that effective ingredients in plant extracts, it is characterized in that: the plant material that is extracted is pulverized, in the plant meal, add the chemical assistant of 0.5%-20% solid base, solid acid, sucrose or salt compounds powder, mechanical crushing together again, select water or ethanol dissolving crushed material for use, separated and collected solubility component obtains active ingredient.
2. the method that is used for the effective ingredients in plant extraction according to claim 1 is characterized in that: realize by following step:
Step 1: plant material is dried to water content and is not higher than 20%, and coarse crushing is to the 40-100 order;
Step 2: in the plant meal, add 1%-10% chemical assistant, mechanical crushing;
Step 3: select water or ethanol dissolving crushed material for use, centrifugal, collect soluble component.
3. the method that is used for the effective ingredients in plant extraction according to claim 1, it is characterized in that: the addition of chemical assistant is 1%-10%.
4. according to claim 1 or the 2 or 3 described methods that are used for the effective ingredients in plant extraction, it is characterized in that: the plant of indication comprises Chinese herbal medicine, wild plant and agricultural byproducts.
5. according to claim 1 or the 2 or 3 described methods that are used for the effective ingredients in plant extraction, it is characterized in that: utilize this method can obtain single active ingredient or the mixture of plurality of active ingredients or the crushed material of whole plant of plant.
6. describedly be used for the methods that effective ingredients in plant extracts according to claim 1 or 2 or 3, it is characterized in that: utilize the single active ingredient of the plant that this method obtains or mixture useful as drug, food, functional food, food additives, veterinary drug or the feed addictive of plurality of active ingredients.
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|---|---|---|---|
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| CN110860107A (en) * | 2019-11-29 | 2020-03-06 | 林东楷 | Microcapsule embedding phytosterol extraction element |
| CN112590157A (en) * | 2020-11-05 | 2021-04-02 | 江苏虹驰家居科技有限公司 | POE material-based bionic silkworm cocoon structure processing technology |
| CN112590157B (en) * | 2020-11-05 | 2022-08-23 | 江苏虹驰家居科技有限公司 | POE material-based bionic silkworm cocoon structure processing technology |
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