阅读说明：本技术 一种灵芝多糖的提取装置及提取工艺 (Extraction device and extraction process of ganoderma lucidum polysaccharide ) 是由 郭韵 尹世界 于 2020-06-30 设计创作，主要内容包括：本发明属于灵芝多糖提取领域,涉及一种灵芝多糖的提取装置及提取工艺,该装置包括按照流体流动方向依次通过管道连接的供水水源(70)、热水器(13)、水提取容器(10)、预过滤器(20)、介电泳分离器(30)、储存罐(40)、浓缩容器(50)和醇沉容器(60)；水提取容器(10)内设有超声波发生器(11)和微波发生器(14)。与现有技术相比,本发明利用微波-超声协同辅助法,并利用预过滤结合介电泳分离进行固液分离,进一步将过滤的残渣进行重新提取,并优化提取工艺,有效提升了提取率和纯度。(The invention belongs to the field of extraction of ganoderma lucidum polysaccharide, and relates to a device and a process for extracting ganoderma lucidum polysaccharide, wherein the device comprises a water supply source (70), a water heater (13), a water extraction container (10), a prefilter (20), a dielectrophoresis separator (30), a storage tank (40), a concentration container (50) and an alcohol precipitation container (60) which are sequentially connected through pipelines according to the fluid flow direction; an ultrasonic generator (11) and a microwave generator (14) are arranged in the water extraction container (10). Compared with the prior art, the method utilizes a microwave-ultrasonic cooperative auxiliary method, and utilizes the combination of prefiltering and dielectrophoresis separation for solid-liquid separation, further re-extracts the filtered residues, optimizes the extraction process, and effectively improves the extraction rate and purity.)

1. A ganoderma lucidum polysaccharide extraction device is characterized by comprising a water supply source (70), a water heater (13), a water extraction container (10), a prefilter (20), a dielectrophoresis separator (30), a storage tank (40), a concentration container (50) and an alcohol precipitation container (60) which are sequentially connected through pipelines according to the fluid flow direction; an ultrasonic generator (11) and a microwave generator (14) are arranged in the water extraction container (10).

2. The apparatus for extracting ganoderan according to claim 1, wherein said water supply (70) is further connected to the pre-filter (20) and the dielectrophoresis separator (30), respectively, and the pre-filter (20) and the dielectrophoresis separator (30) are further connected to the water extraction container (10) through a residue return pipe for flushing the separated residue into the water extraction container (10) for further water extraction and for equipment cleaning.

3. The ganoderma lucidum polysaccharide extraction device as claimed in claim 2, wherein the outlets of the water supply source (70) to the pre-filter (20) and the dielectrophoresis separator (30) are provided with first valves (71), the pipe of the dielectrophoresis separator (30) to the storage tank (40) is provided with a second valve (31), and the residue return pipes of the pre-filter (20) and the dielectrophoresis separator (30) to the water extraction container (10) are provided with a third valve (21) and a fourth valve (32), respectively.

4. The apparatus for extracting ganoderan according to claim 1, wherein the pre-filter (20) is a centrifugal filter for filtering large solid particles before the fluid enters the dielectrophoresis separator (30).

5. The extraction device of ganoderma lucidum polysaccharide as claimed in claim 1, further comprising a power supply (80) for supplying power, wherein the power supply (80) is connected with the ultrasonic generator (11), the water heater (13), the microwave generator (14), the dielectrophoresis separator (30) and the concentration container (50) through cables.

6. The ganoderma lucidum polysaccharide extraction device as claimed in claim 5, wherein the dielectrophoresis separator (30) comprises a vertical cylindrical container (301), electrodes (302), an inlet porous plate (303), an outlet porous plate (304) and a plurality of high dielectric constant medium rods (305); the top end and the bottom end of the vertical cylindrical container (301) are sealed by a flange plate (306), a fluid inlet (307) is arranged on the flange plate (306) at the top end, and a fluid outlet (308) is arranged on the flange plate (306) at the bottom end; the electrode (302) is arranged in the vertical cylindrical container (301) along the central axis of the vertical cylindrical container (301) and is connected with the power supply (80), and the electrode (302) and the vertical cylindrical container (301) have opposite polarities, so that an electromagnetic field is generated between the electrode (302) and the vertical cylindrical container (301); a plurality of high dielectric constant dielectric rods (305) are vertically arranged and surround the electrode (302), and an inlet porous plate (303) and an outlet porous plate (304) are respectively arranged at two ends of the high dielectric constant dielectric rods (305) and are respectively separated from flange plates (306) at the top end and the bottom end of the vertically arranged cylindrical container (301) by gaps.

7. The ganoderma lucidum polysaccharide extraction device as claimed in claim 1, wherein a first pump (12) is arranged on a pipeline of the water extraction container (10) leading to the pre-filter (20), a second pump (41) is arranged on a pipeline of the storage tank (40) leading to the concentration container (50), and a third pump (51) is arranged on a pipeline of the concentration container (50) leading to the alcohol precipitation container (60).

8. An extraction process of ganoderma lucidum polysaccharide, which is characterized by adopting the extraction device as claimed in any one of claims 1 to 7, and comprises the following steps:

s1: putting the ganoderma lucidum spores into a water extraction container (10) for hot water immersion and boiling, and using an ultrasonic generator (11) and a microwave generator (14) for assistance;

s2: after the digestion, the feed liquid is prefiltered by a prefilter (20) to obtain coarse liquid, the coarse liquid enters a dielectrophoresis separator (30) to be subjected to solid-liquid separation to obtain ganoderma lucidum polysaccharide clear liquid, and the ganoderma lucidum polysaccharide clear liquid is stored in a storage tank (40);

s3: cleaning the solid residue in the pre-filter (20) and the dielectrophoresis separator (30) by using clean water in a water supply source (70), and flowing into the water extraction container (10) through a residue return pipe;

s4: repeating steps S1 and S2;

s5: conveying the ganoderma lucidum polysaccharide clear liquid in the storage tank (40) to a concentrator (50) for concentration to obtain a concentrated ganoderma lucidum polysaccharide solution;

s6: and (3) conveying the concentrated ganoderma lucidum polysaccharide solution to an alcohol precipitation container (60), and performing alcohol precipitation to obtain the high-purity ganoderma lucidum polysaccharide.

9. The extraction process of ganoderma lucidum polysaccharide according to claim 8, wherein in step S1, the ultrasonic power is 320W, the microwave power is 284W, the liquid-material ratio is 11.6mL:1g, and the temperature is 55 ℃.

10. The process of claim 8, wherein the step S1, the soaking in hot water is 40 min.

Technical Field

The invention belongs to the field of ganoderma lucidum polysaccharide extraction, relates to a solid-liquid separation technology of a wall-broken spore powder extract, and particularly relates to an extraction device and an extraction process of ganoderma lucidum polysaccharide.

Background

Ganoderma lucidum is also called Linzhongling, which has the best effect for growing in the forest. The ganoderma lucidum is characterized by containing rich polysaccharide and polysaccharide III, wherein the ganoderma lucidum polysaccharide is glucan which is formed by three strands of monosaccharide chains and has a spiral three-dimensional configuration (a three-level structure), the three-dimensional configuration of the glucan is similar to deoxyribonucleic acid (DNA) and ribonucleic acid (RNA), the glucan is a macromolecular compound, the molecular weight of the glucan is thousands to hundreds of thousands, and the glucan is a substance extracted from ganoderma lucidum spore powder or ganoderma lucidum. Insoluble in high concentration alcohol, slightly soluble in low concentration alcohol and cold water, and completely soluble in hot water. Ganoderan is present on the inner wall of the cell wall of ganoderma lucidum. Ganoderma polysaccharides contain glucose, and monosaccharide such as arabinose, xylose, galactose, fucose, and mannose, but in small amount. The majority is beta-type structure, and the minority is alpha-type structure. The alpha-type polysaccharide has no pharmacological activity (drug effect). The polysaccharide chain has high branching density or high pharmacological activity of the polysaccharide chain.

The ganoderan can be divided into three types according to the source, which are sporophore polysaccharide, fermentation broth polysaccharide and mycelium polysaccharide. The extraction method is determined by the extraction part and the existence form of the ganoderma lucidum polysaccharide. The prior methods for extracting the ganoderma lucidum polysaccharide mainly comprise a hot water extraction method, an ultrasonic assisted water extraction method, an alkali extraction method, an enzyme method, a microwave extraction method and the like.

The polysaccharide is extracted by a traditional hot water extraction method in industrial production, and according to the principle that the polysaccharide is easy to dissolve in water, the optimal extraction conditions for extracting the ganoderma lucidum polysaccharide by a hot water method are as follows: extracting for 120min at the extraction temperature of 90 ℃ and the liquid-material ratio of 15: 1. the boiling water extraction method is adopted to extract the ganoderma lucidum polysaccharide, and the obtained extraction solution has high viscosity, is not beneficial to filtration and is difficult to centrifuge, thereby causing unstable influence on yield. Although the hot water extraction method is simple and convenient to operate, the development of the ganoderma lucidum industry is limited by high extraction temperature, long time, high energy consumption, low yield and the like.

The enzyme extraction method is a mild extraction method, and the enzyme extraction method utilizes the damage effect of enzyme on cell structures to degrade cell walls, so that intracellular polysaccharide is quickly dissolved out, and the yield of ganoderma lucidum polysaccharide can be improved. The optimal conditions for extracting the polysaccharide by the cellulase are as follows: the enzyme adding amount is 0.5%, the enzymolysis temperature is 55 ℃, the enzymolysis time is 80min, the pH value is 5.0, and the polysaccharide content is 196.50 mg/mL. The polysaccharide content is 211.21mg/mL by adopting a cellulose and ethanol precipitation method for extraction. The extraction rate of the ganoderma lucidum polysaccharide is obviously improved. The extraction rate of the wall-broken spore is compared with that of the non-wall-broken spore by adopting an enzyme method, and the enzyme wall-broken method is found to have the highest extraction rate, probably because more soluble polysaccharide is degraded by enzymolysis, but the cost is higher.

The microwave extraction method is characterized in that water molecules in cells absorb heat by microwaves to rapidly raise the temperature in the cells, so that vaporization effect is generated in the cells, cell membranes and cell walls are damaged, and hollow cracks are generated, and substances in the cells are easily contacted with a solvent due to the generation of the hollow cracks, so that the substances in the cells are dissolved out. Microwave pretreatment is used for extracting the ganoderan, and the result shows that the extraction time of the method is shortened by 60min and the extraction rate is improved by 34.2% compared with the traditional method. Microwave radiation can increase the reaction rate and reduce the reaction time.

The ultrasonic-assisted extraction method has the advantages that the ultrasonic-assisted extraction method has high-frequency vibration and special effects of cavitation, crushing, stirring and the like generated by the ultrasonic, has destructive power on cells of medicinal materials, and can accelerate the effective components of the medicaments to enter a solvent, enlarge the pore diameter of a dialysis membrane and release intracellular polysaccharide as soon as possible, so that the extraction rate is improved, the extraction time is shortened, the solvent is saved, and the low-temperature extraction is favorable for protecting the effective components.

However, the above extraction method is simple, and there is room for improvement in extraction rate.

Disclosure of Invention

The invention aims to provide a device and a process for extracting ganoderma lucidum polysaccharide. The ganoderma lucidum polysaccharide is refined, and the extraction rate and the purity of the ganoderma lucidum polysaccharide are improved.

The purpose of the invention can be realized by the following technical scheme:

the invention provides a ganoderma lucidum polysaccharide extraction device which comprises a water supply source, a water heater, a water extraction container, a prefilter, a dielectrophoresis separator, a storage tank, a concentration container and an alcohol precipitation container which are sequentially connected through pipelines according to the flowing direction of fluid; an ultrasonic generator and a microwave generator are arranged in the water extraction container.

As a preferable technical scheme, the water supply source is also respectively connected with the pre-filter and the dielectrophoresis separator, and the pre-filter and the dielectrophoresis separator are also connected with the water extraction container through the residue return pipe, so that the separated residue is flushed into the water extraction container for water extraction again and is used for equipment cleaning.

As a preferable technical scheme, a first valve is arranged at an outlet of the water supply source which leads to the prefilter and the dielectrophoresis separator, a second valve is arranged on a pipeline of the dielectrophoresis separator which leads to the storage tank, and a third valve and a fourth valve are respectively arranged on a residue return pipe of the prefilter and the dielectrophoresis separator which lead to the water extraction container.

As a preferred technical scheme, the pre-filter adopts a centrifugal filter for filtering large solid particles before the fluid enters the dielectrophoresis separator.

As a preferred technical scheme, the device also comprises a power supply for supplying power, and the power supply is connected with the ultrasonic generator, the water heater, the microwave generator, the dielectrophoresis separator and the concentration container through cables.

As the preferred technical scheme, the dielectrophoresis separator comprises a vertical cylindrical container, electrodes, an inlet porous plate, an outlet porous plate and a plurality of high-dielectric constant medium rods; the top end and the bottom end of the vertical cylindrical container are sealed by a flange plate, a fluid inlet is arranged on the flange plate at the top end, and a fluid outlet is arranged on the flange plate at the bottom end; the electrodes are arranged in the vertical cylindrical container along the central axis of the vertical cylindrical container and are connected with a power supply, and the electrodes and the vertical cylindrical container have opposite polarities, so that an electromagnetic field is generated between the electrodes and the vertical cylindrical container; a plurality of high dielectric constant dielectric rods are vertically arranged and surround the periphery of the electrode, and the inlet porous plate and the outlet porous plate are respectively arranged at two ends of the high dielectric constant dielectric rods and are respectively separated from the flange plates at the top end and the bottom end of the vertically arranged cylindrical container by gaps.

As the preferred technical scheme, a first pump is arranged on a pipeline of the water extraction container, which leads to the prefilter, a second pump is arranged on a pipeline of the storage tank, which leads to the concentration container, and a third pump is arranged on a pipeline of the concentration container, which leads to the alcohol precipitation container.

The second aspect of the invention provides an extraction process of ganoderma lucidum polysaccharide, which adopts the extraction device and comprises the following steps:

s1: putting the ganoderma lucidum spores into a water extraction container for hot water immersion and boiling, and using an ultrasonic generator and a microwave generator for assistance;

s2: after the digestion is finished, the feed liquid is prefiltered by a prefilter to obtain coarse liquid, the coarse liquid enters a dielectrophoresis separator for solid-liquid separation to obtain ganoderma lucidum polysaccharide clear liquid, and the ganoderma lucidum polysaccharide clear liquid is stored in a storage tank;

s3: cleaning solid residues in the prefilter and the dielectrophoresis separator by using clear water in a water supply source, and flowing into a water extraction container through a residue return pipe;

s4: repeating steps S1 and S2;

s5: conveying the ganoderma lucidum polysaccharide clear liquid in the storage tank to a concentrator for concentration to obtain a concentrated ganoderma lucidum polysaccharide solution;

s6: and (3) conveying the concentrated ganoderma lucidum polysaccharide solution to an alcohol precipitation container, and performing alcohol precipitation to obtain the high-purity ganoderma lucidum polysaccharide.

In a preferable technical scheme, in step S1, the ultrasonic power is 320W, the microwave power is 284W, the liquid-material ratio is 11.6mL:1g, and the temperature is 55 ℃.

Preferably, in step S1, the time for the hot water to soak is 40 min.

The whole process from ganoderma spore powder to ganoderma polysaccharide obtaining comprises water extraction, solid-liquid separation, concentration and alcohol precipitation.

Wherein the water extraction utilizes microwave-ultrasonic cooperative auxiliary method, the high frequency vibration of ultrasonic wave has destructive power to the cells of the medicinal material by utilizing the crushing and stirring effects, the dialysis membrane diameter is enlarged, and the polysaccharide in the cells can be accelerated to enter the solvent, thereby improving the efficiency and shortening the extraction time. Microwave is utilized to enable water molecules in cells to absorb heat so as to enable the temperature in the cells to rise rapidly, vaporization effect is generated in the cells, cell membranes and cell walls are damaged, so that cavity cracks occur, substances in the cells are easy to contact with a solvent due to the cavity cracks, the substances in the cells are dissolved out, and rapid dissolution of ganoderma lucidum polysaccharide is promoted.

The solid-liquid separation part comprises a prefilter and a dielectrophoresis separator. The pre-filtration section employs centrifugal filtration for filtering large solid particles before the fluid enters the dielectrophoretic separator. Dielectrophoresis, also known as dielectrophoresis, is a phenomenon in which an object having a low dielectric constant is subjected to a force in a non-uniform electric field. The dielectric force is independent of whether the object is charged or not, and is dependent on the size and the electrical property of the object, the electrical property of the surrounding medium, the field intensity of an external electric field, the field intensity change rate and the frequency. The solid impurities in the mixed liquor of the extraction residues of the wall-broken ganoderma lucidum spore powder are left by utilizing the dielectrophoresis principle, and the solution containing the ganoderma lucidum polysaccharide is delivered into a storage container. And powering off the dielectrophoresis separator to stop generating an electromagnetic field, feeding clear water into the container, and cleaning the solid ganoderma spore powder into the water extraction container by the clear water through the channel to carry out secondary water extraction.

Compared with the prior art, the method utilizes a microwave-ultrasonic cooperative auxiliary method, and utilizes the combination of prefiltering and dielectrophoresis separation for solid-liquid separation, further re-extracts the filtered residues, optimizes the extraction process, effectively improves the extraction rate of the ganoderma lucidum polysaccharide, and obtains the ganoderma lucidum polysaccharide with higher purity.

Drawings

FIG. 1 is a schematic connection diagram of the extraction apparatus of the present invention.

Fig. 2 is a schematic diagram of power connection of the extraction device of the present invention.

FIG. 3 is a schematic front sectional view of a dielectrophoretic separator of the invention.

Figure 4 is a schematic cross-sectional view of a dielectrophoretic separator of the invention.

FIG. 5 is a schematic view of the high dielectric constant media rods of the dielectrophoretic separator of the invention.

In the figure, 10 is a water extraction container, 11 is an ultrasonic generator, 12 is a first pump, 13 is a water heater, 14 is a microwave generator, 20 is a prefilter, 21 is a third valve, 30 is a dielectrophoresis separator, 31 is a second valve, 32 is a fourth valve, 301 is a vertically-arranged cylindrical container, 302 is an electrode, 303 is an inlet porous disk, 304 is an outlet porous disk, 305 is a high-permittivity medium rod, 306 is a flange plate, 307 is a fluid inlet, 308 is a fluid outlet, 40 is a storage tank, 41 is a second pump, 50 is a concentration container, 51 is a third pump, 60 is a container, 70 is a water supply source, 71 is a first valve, and 80 is a power supply.

Detailed Description

The invention is described in detail below with reference to the figures and specific embodiments.