CN101530435A - Pretreatment method for extracting plant effective components - Google Patents
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- CN101530435A CN101530435A CN200910031200A CN200910031200A CN101530435A CN 101530435 A CN101530435 A CN 101530435A CN 200910031200 A CN200910031200 A CN 200910031200A CN 200910031200 A CN200910031200 A CN 200910031200A CN 101530435 A CN101530435 A CN 101530435A
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Abstract
The invention relates to a pretreatment method for extracting plant effective components. Before extraction, wet basis plant materials are radiated by vacuum microwaves first, and then mechanical extrusion force and shearing force are repeatedly applied to plant materials after the radiation by vacuum microwaves by a screw extruder. After the pretreatment, the plant effective components of the plant materials are extracted subsequently according to a conventional method so that the extraction of the plant effective components has higher yield. The method also has the advantages of high microwave utilization rate, no damage to target effective components, short processing time and low energy consumption, can avoid an explosion accident of an organic solvent because the organic solvent is not used in the pretreatment of plants, and is suitable to be applied to industrial production.
Description
Technical field
The present invention relates to the extracting method of effective ingredients in plant, be specifically related to before effective ingredients in plant extracts, plant be carried out pretreated method, by pretreatment plant cell wall is broken, thereby make the extraction of effective ingredients in plant that better yield be arranged.
Background technology
China is vast in territory, and geography and weather are with favourable conditions, is containing very abundant natural plant resource, kind surplus only higher plant just has 30000, wherein medicinal plants just has 11146 kinds, and its kind and quantity are the first in the world, and they have constituted the basis of Chinese nation's Chinese medicine medical science for thousands of years.Though China is the output big country of plant amedica, not the power that plant amedica is produced.At present China's plant amedica on plant amedica market, the world portion less than 5%, wherein major part or medicinal raw material, China is lower at the plant amedica market of developed country portion, account for 2% the Great Britain and America, be about 0.2% in Germany, China is lagging behind Japan and Korea S aspect plant amedica product development and the production.The content of effective ingredients in plant is often less relatively, and leaching process need expend a large amount of solvents and energy, and therefore extracting is most important operation during plant amedica is produced, and directly influences quality, production cost and the utilization ratio of raw materials etc. of product.How quick, efficient, simple and direct, at low cost medicinal the or nourishing healthy extracts active ingredients in the plant to be come out be plant extract research and " bottleneck " produced always, it is crucial developing energy-efficient extraction new technique and equipment, to accelerating the process of Chinese medicine production modernization, effectively the development and utilization Chinese herbal medicine resource has great significance.
The extracting method of conventional effective ingredients in plant is as decocting method, reflux extraction, soxhlet extraction, infusion process, percolation and steam distillation etc., these methods all are with plant and suitable solvent Hybrid Heating, solvent infiltrates in organization internal and the cell, the solubility composition is under the promotion of concentration difference, progressively move to the surface from material inside, transfer to again in the solvent, the time length of its transfer with add temperature great relation arranged.The limitation and the shortcoming of said method are: (1) substance transfer is slow, needs long-time heating, increases energy consumption greatly; (2) need a large amount of solvents, increased the back segment energy consumption; (3) long-time high-temperature process may cause effective ingredient to destroy; (4) production efficiency is low, be to improve production capacity, adopts usually to strengthen the extraction pot volume and with the methods of organizing extraction pot more; (5) take up an area of greatly operation inconvenience.Said method all belongs to the batch (-type) extracting method.
The extraction of effective ingredients in plant at present also has continuous dynamic countercurrent extraction method, and with separate, concentrate, prior art formation production process route such as drying.But its extraction equipment is huge, and extraction time is long.
Some new extractive techniques have appearred in recent years, as supercritical Fluid Extraction Technology, microwave auxiliary extraction technology, ultrasonic auxiliary extraction technology, enzyme auxiliary extraction technology etc.These new techniques respectively have its characteristics, have enriched the means of extracting to a certain extent, have improved extraction ratio and extraction rate.Wherein, microwave auxiliary extracting method (Microwave Assisted Extraction, be called for short MAE) be the extraction new technique of tool potentiality, the extraction principle of MAE mainly is to utilize the heat characteristic of microwave, microwave can see through vascular bundle and the glandular cell system that medium arrives material inside that extract, cause intracellular polar substances especially hydrone absorb microwave energy and produce a large amount of heats, make that temperature rises rapidly in the cell, the pressure that the aqueous water vaporization produces breaks through cell wall/film or forms small hole.In addition, the electromagnetic field that microwave produced also can quicken to be extracted the diffusion rate of component in solvent.
But above-mentioned existing microwave auxiliary extracting method exists technology, economy and security bottleneck in plant-scale application.Lot of domestic and foreign scholar's research microwave-assisted extracts, with microwave oven or microwave experiment instrument etc. is means, a large amount of tests have been carried out, observe the facilitation of microwave to extracting, and a large amount of relevant papers have been delivered, but these work all rest on a small scale and laboratory level, fail the application of succeeding in plant-scale plant extract so far.Microwave extraction is transformed into commercial scale from laboratory scale needs to solve a series of problems such as production capacity, extraction efficiency, production cost and production equipment comprehensively.The limitation that influences the microwave extraction effect is: the penetration depth of microwave in liquid is limited, as the penetration depth of microwave in water of 2450 MHz 30mm only, surpass this degree of depth, microwave is absorbed by solvent mostly, the effect of microwave is extremely faint, the utilization rate of microwave is low, can influence its industrial application thus; Microwave is transformed by electric energy, and its energy consumption cost than the expensive 5-6 of primary energy doubly because the volume of production of industrial extraction effective ingredients in plant is big, if the energy consumption cost of microwave is excessive, also is difficult to accept in industrial large-scale production; In addition, if the solvent of effective ingredients in plant is an organic solvent, there is the probability of blast in the microwave radiation organic solvent.
Comprehensive existing literature and domestic and international patent, attempting has two classes in commercial scale substantially with the using method of microwave applications in effective ingredients in plant extracts, first kind method is that microwave is directly introduced in extraction pot or the pipeline, as United States Patent (USP) 5002784,7001629B1, Chinese patent CN1391972A, CN101041116A, CN101209384A, CN101020126A, CN101041117A, CN1824364A, ZL200610044442.1 makes the microwave penetration solvent enter extract inside, destroys plant tissue or fortification of plants organization internal mass transport process.This method is to using the more weak non-polar solvent extract effect of absorption microwave ability better, because absorbed few during the microwave penetration solvent by solvent, most of microwave can arrive plant tissue inside and be absorbed, the utilization rate of microwave is higher, for example can use transparent solvent (not absorbing microwave) in analytical chemistry.But in commercial production, plant extract mostly is to use water or the stronger solvent of pure isopolarity, is difficult to use transparent solvent.Chinese patent CN1391972A, CN101041116A add microwave in extraction pot, beyond tank skin 30mm, microwave is extremely faint, have had a strong impact on effect and efficient that microwave-assisted extracts; And Chinese patent CN101209384A, CN101020126A, CN101041117A adopt material to flow in pipeline and accept the form of microwave radiation, can solve the penetrance problem, but microwave absorbs by solvent mostly, and the problem that utilization rate is low still can not solve; United States Patent (USP) 7001629B1; Chinese patent CN1824364A; ZL200610044442.1 is evacuation in the microwave radiation jar or in the bottle; reduced the boiling point of solvent; help protecting the active effective ingredient of thermal sensitivity; but the low problem of above-mentioned depth of microwave penetration finite sum microwave utilization rate still exists, and is not suitable for suitability for industrialized production.Second class methods are microwave pretreatment extraction methods, as Chinese patent CN1422685A, CN1546194A, CN1273206C, this method is before traditional extraction process, uses earlier microwave pretreatment, its objective is the organizational structure that changes plant, so that subsequent extracted becomes easy.Pretreated principle is with the wet material of microwave Fast Heating, and the liquid in the material is vaporized fast, changes the organizational structure of material.The characteristics of the method be microwave treatment be the wet stock that does not have too much free solvent, microwave irradiation time is short, requirement is few, treating capacity is big, be easy to realize suitability for industrialized production, but above-mentioned preprocessing process adopts the normal pressure microwave radiation, temperature of charge after the processing often surpasses 100 ℃, can cause the thermal sensitivity effective ingredient destroyed, has seriously restricted the practical application of this method.
The content of invention
Applicant of the present invention exists the above-mentioned depth of microwave penetration limited in industrial applications at the microwave current assisted extraction, the microwave utilization rate is low, the energy consumption cost height, material after the normal pressure microwave radiation processing tends to cause the destroyed and microwave radiation problems such as probability that existence is exploded to the organic solvent solvent of thermal sensitivity effective ingredient, carried out improving research, the preprocess method that another kind of effective ingredients in plant extracts has been proposed, before extracting, effective ingredients in plant at first utilize this method that plant is carried out pretreatment, plant cell wall is effectively broken, carry out the subsequent extracted of effective ingredients in plant after the pretreatment again according to conventional method, so the extraction to effective ingredients in plant has higher yield.This method microwave utilization rate height does not destroy the target effective composition, and the processing time is short, energy consumption is low and plant is carried out in the pretreatment not with an organic solvent not avoiding the blast of organic solvent, is fit to be applied in the suitability for industrialized production.
Technical scheme of the present invention is as follows:
The preprocess method that a kind of effective ingredients in plant extracts at first adopted vacuum microwave radiation wet basis plant material before extracting, with screw extruder described plant material through the vacuum microwave radiation is applied mechanical presses power and shearing force repeatedly then.
Its further technical scheme is:
For the butt plant material, before described vacuum microwave radiation, at first use the water preimpregnation of 2 to 6 times of its weight ratios, 30 minutes～1 hour preimpregnation time, become the wet basis plant material; For fresh plant material,, directly it is carried out described vacuum microwave radiation then as the wet basis plant material.For the plant material of doing, before the water preimpregnation, need cut into slices or pulverize, be not more than 8mm to granularity.
The radiating power density of above-mentioned vacuum microwave is 1～5 watt/every gram wet basis plant material, and when vacuum was 10～85Kpa, the temperature of described wet basis plant material was 50～90 ℃, radiated time 3～10 minutes.
Above-mentioned screw extruder is single screw rod or twin (double) screw extruder, and the volume extrusion ratio of its screw rod is 1:2～1:6.
Useful technique effect of the present invention is:
The present invention adopts vacuum microwave in conjunction with attrition crushing the wet basis plant material to be carried out pretreatment, most of plant cell wall is broken or is made the weakened of cell wall, cell wall separates with Cytoplasm, cellularity is loose, apply mechanical presses power, shearing force etc. afterwards more repeatedly, can tear cell wall further more complete, more up hill and dale, change and the organizational structure of the plant of breaking, making in the subsequent extracted of effective ingredients in plant has higher yield.The present invention avoids placing the solvent that polarity is stronger in extraction pot or the pipeline (for example water) to carry out microwave radiation processing plant material in the prior art, but only use solvent (for example water) to carry out preimpregnation plant material, become the wet basis plant material and carry out microwave radiation, perhaps to fresh plant material, as described wet basis plant material, directly it is carried out microwave radiation, because the strict consumption of having controlled solvent, microwave energy only acts on intracellular solvent, so both utilized solvent (for example water) to help the organizational structure of the change and the plant of breaking, when avoiding using the stronger solvent of volume water isopolarity again to the decay absorption of microwave, thereby make the utilization rate height of microwave energy, need the radiating time short.The present invention adopts the vacuum microwave radiation, by control vacuum, can control the temperature (general 50～100 ℃) of any needs, avoids the rising of temperature and destroys the thermal sensitivity active component.In addition under the vacuum microwave condition because the residing ambient pressure of material is lower, plant cell is also than easier to be expanded and break under the normal pressure microwave radiation condition.Processing time of the present invention is short, treating capacity is big.
The present invention only makes water as the preimpregnation solvent in preprocessing process, and the strict consumption of having controlled water, and preimpregnation moisture most of carburation by evaporation in vacuum microwave radiation heating process, so do not influence the concentration requirement (concentration that organic solvent extraction uses is generally between 70～90%) of organic solvent in follow-up conventional the extraction.Explosion-proof problem when having solved the organic solvent microwave radiation well.
The present invention makes whole energy become possibility.Though the vacuum microwave radiation consumes certain microwave energy and mechanical energy in conjunction with the attrition crushing pretreatment, but because the consumption that strict control is soaked in advance in vacuum microwave material handling process, microwave acts on intracellular moisture substantially, the functioning efficiency height of microwave, the radiation treatment time of microwave only needs several minutes.The broken mechanical energy that consumes of mechanical presses is also limited, breaking of plant cell wall after treatment, making follow-up continuous dynamic countercurrent extraction or pot type stir the mass transfer velocity that extracts accelerates greatly, it is big that required extraction time and solvent load reduce degree, and overall energy consumption cost can descend on the contrary by a relatively large margin.
The invention enables the exploitation of continous vacuum microwave radiation processing equipment to become possibility.In the exploitation of existing vacuum microwave drying equipment, (vacuum represents that system's actual pressure is lower than the numerical value of atmospheric pressure owing to required vacuum, that is: vacuum=atmospheric pressure-absolute pressure) bigger, more than 95KPa, the continuous vacuum microwave dryer does not also have so far and can successfully develop in China.And this project is because between 50～100 ℃ of the temperature that vacuum microwave is handled, the highest corresponding vacuum is about 85KPa, because the reduction that vacuum requires can be developed continous vacuum microwave radiation processing equipment fully, big to adapt to the commercial production treating capacity, the requirement of automated production.
The specific embodiment
Below by three embodiment the present invention is specifically described.
Embodiment one: the extraction of ganoderan.
To do Ganoderma powder and be broken into 20～50 orders, and take by weighing 100g with electronic balance, the weight 500g of soakage water stirs, and soaks into vacuum microwave radiation 7 minutes, 2.5～3.0 watts/gram (w/g) of the power density of microwave, vacuum 75Kpa 1 hour; Ganoderma after the vacuum microwave radiation enters single-screw extrusion machine immediately, the compression ratio 1:3 of screw rod; The follow-up Soxhlet method that adopts is again extracted, 80 ℃ of heating and refluxing extraction 2.5 hours (h), and the extraction yield of ganoderan is 1.753%.
The present invention adds follow-up existing Soxhlet method and extracts and relatively seeing Table 1 (raw material is identical with the condition of existing Soxhlet method extraction and result separately, experiment repeats 3 times and gets average), data as can be known from table 1, with do not have pretreated Soxhlet method extract phase ratio, the present invention can reduce solvent (water) amount 33.3% of extracting, and extraction time minimizing 58.3% is by pretreatment of the present invention, the yield effect that improves the extraction of effective ingredient ganoderan is remarkable, and the yield of ganoderan improves 33.70%.
Table 1: the influence that the present invention extracts the Oletum Trogopterori polysaccharide
| Extracting method | Soak into ratio of water to material | Infiltrating time (h) | Soxhlet extraction time (h) | Total solid-liquid ratio that extracts | Polysaccharide extract rate (%) | The deviation of extraction ratio (RSD%) |
| Soxhlet is extracted | 5:1 | 1 | 6 | 1:30 | 1.311 | 0.063 |
| Vacuum microwave and extruding combination pretreatment+Soxhlet are extracted | 5:1 | 1 | 2.5 | 1:20 | 1.753 | 0.072 |
In the table 1:
m
d: the quality of polysaccharide (g); m
t: the quality of Ganoderma raw material (g, butt).
Embodiment two: the extraction of Folium Bambosae flavone in the Folium Bambusae
Take by weighing dried Folium Bambusae (10～30 order) 200g with electronic balance, soakage water is 800g, stirs, and soaks into vacuum microwave radiation 10 minutes, the power density 1.5～2.0w/g of microwave, vacuum 65Kpa 0.5 hour; Folium Bambusae after the vacuum microwave radiation enters single-screw extrusion machine immediately, the compression ratio 1:2 of screw rod.Follow-uply adopt traditional heating in water bath method to extract again, 90 ℃ of bath temperatures, the extraction solvent is a water, heating extraction 1 hour (h), the extraction ratio of Folium Bambosae flavone is 2.027%.
The present invention adds follow-up existing heating in water bath method and extracts and relatively the seeing Table 2 (raw material the is identical of condition of independent existing heating in water bath method extraction and result, experiment repeats 3 times and gets average, the computational methods of flavone extraction ratio are with table 1), data as can be known from table 2, with do not have pretreated heating in water bath method extract phase ratio, the inventive method can reduce extracts solvent (water) 37.5%, extraction time reduces 52%, by pretreatment of the present invention, the yield effect that improves the extraction of effective ingredient Folium Bambosae flavone is remarkable, and the yield of Folium Bambosae flavone improves 24.3%.
Table 2: the influence that the present invention extracts Folium Bambosae flavone
| Extracting method | Soak into ratio of water to material | Infiltrating time (h) | Heating in water bath extraction time (h) | Total solid-liquid ratio that extracts | Flavone extraction ratio % | The deviation of extraction ratio (RSD%) |
| Heating in water bath extracts | 4:1 | 1.0 | 2.5 | 1:40 | 1.631 | 0.054 |
| Vacuum microwave and extruding combination pretreatment+heating in water bath extract | 4:1 | 1.0 | 1.2 | 1:25 | 2.027 | 0.067 |
Embodiment three: the extraction of flavone in the bright leaf of Semen Ginkgo
The fresh gingko leaf is suitably shredded, take by weighing Folium Ginkgo 3Kg, vacuum microwave radiation 5 minutes, the power density 4.0～4.5w/g of microwave, vacuum 45Kpa with electronic balance; Folium Ginkgo after the vacuum microwave radiation enters single-screw extrusion machine immediately, the compression ratio 1:5 of screw rod.Follow-uply adopt existing dynamic continuity method to extract again, extract solvent and adopt 50% alcoholic solution, 90 ℃ of solvent temperatures, the material time of arrheaing in dynamic continuous extractor is 1.2h, and the extraction ratio of bright Folium Ginkgo flavone is 1.150%.
The present invention adds the subsequent dynamic continuity method and extracts and relatively seeing Table 3 (raw material is identical with the condition of existing dynamic continuity method extraction and result separately, experiment repeats 3 times and gets average, the computational methods of flavone extraction ratio are with table 1), data as can be known from table 3, with do not have pretreated existing dynamic continuity method extract phase ratio, the inventive method can reduce extracts solvent (water) 44.4%, and extraction time reduces 60%.By pretreatment of the present invention, the yield effect that improves the bright Folium Ginkgo flavone extraction of effective ingredient is remarkable, and the yield of bright Folium Ginkgo flavone improves 26.34%.
Table 3: the influence that the present invention extracts flavone in the bright leaf of Semen Ginkgo
| Extracting method | Dynamic countercurrent continuous extraction time (h) | Total solid-liquid ratio that extracts | Flavone extraction ratio (%) | The deviation of extraction ratio (RSD%) |
| Dynamic countercurrent extracts continuously | 2.0 | 1:18 | 1.150 | 0.067 |
| Vacuum microwave and extruding combination pretreatment+dynamic countercurrent extract continuously | 0.8 | 1:10 | 1.453 | 0.078 |
Above-described only is preferred implementation of the present invention, the invention is not restricted to above embodiment.Be appreciated that other improvement and variation that those skilled in the art directly derive or associate under the prerequisite that does not break away from spirit of the present invention and design, all should think to be included within protection scope of the present invention.
Claims (5)
1. the preprocess method that extracts of an effective ingredients in plant, it is characterized in that: before extracting, at first adopt vacuum microwave radiation wet basis plant material, with screw extruder described plant material through the vacuum microwave radiation is applied mechanical presses power and shearing force repeatedly then.
2. the preprocess method that effective ingredients in plant according to claim 1 extracts, it is characterized in that:, before described vacuum microwave radiation, at first use the water preimpregnation of 2 to 6 times of its weight ratios for the butt plant material, 30 minutes～1 hour preimpregnation time, become described wet basis plant material; For fresh plant material,, directly it is carried out described vacuum microwave radiation then as described wet basis plant material.
3. the preprocess method that effective ingredients in plant according to claim 2 extracts is characterized in that: for the butt plant material, before the water preimpregnation, cut into slices or pulverize, be not more than 8mm to granularity full-size.
4. the preprocess method that effective ingredients in plant according to claim 1 and 2 extracts, it is characterized in that: the radiating power density of described vacuum microwave is 1～5 watt/every gram wet basis plant material, when vacuum is 10～85Kpa, the temperature of described wet basis plant material is 50～90 ℃, radiated time 3～10 minutes.
5. the preprocess method that effective ingredients in plant according to claim 1 extracts, it is characterized in that: described screw extruder is single-screw extrusion machine or twin (double) screw extruder, the volume extrusion ratio of its screw rod is 1:2～1:6.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786606A (en) * | 2012-09-05 | 2012-11-21 | 龙海市颖欣农业科技有限公司 | Processing method of lentinan |
| CN102993145A (en) * | 2011-09-19 | 2013-03-27 | 北大方正集团有限公司 | Lovastatin extraction and purification method |
| CN106512470A (en) * | 2016-11-16 | 2017-03-22 | 揭阳市腾晟科技咨询有限公司 | Pretreatment method for extracting effective ingredients of plant |
| CN107050099A (en) * | 2017-04-21 | 2017-08-18 | 贵阳中医学院 | The high efficiency extraction equipment and its extracting method of a kind of caragana general flavone |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171653C (en) * | 2002-12-17 | 2004-10-20 | 广西大学 | Microwave-pretreating extraction method for effective component of plant |
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2009
- 2009-04-29 CN CN2009100312002A patent/CN101530435B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993145A (en) * | 2011-09-19 | 2013-03-27 | 北大方正集团有限公司 | Lovastatin extraction and purification method |
| CN102786606A (en) * | 2012-09-05 | 2012-11-21 | 龙海市颖欣农业科技有限公司 | Processing method of lentinan |
| CN102786606B (en) * | 2012-09-05 | 2015-05-20 | 龙海市颖欣农业科技有限公司 | Processing method of lentinan |
| CN106512470A (en) * | 2016-11-16 | 2017-03-22 | 揭阳市腾晟科技咨询有限公司 | Pretreatment method for extracting effective ingredients of plant |
| CN107050099A (en) * | 2017-04-21 | 2017-08-18 | 贵阳中医学院 | The high efficiency extraction equipment and its extracting method of a kind of caragana general flavone |
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Assignee: Shaanxi Hao Qi Jun Pharmaceutical Co., Ltd. Assignor: Jiangnan University Contract record no.: 2011320010064 Denomination of invention: Pretreatment method for extracting plant effective components Granted publication date: 20101229 License type: Exclusive License Open date: 20090916 Record date: 20110622 |
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