Method for extracting and separating multiple active components in rhizoma polygonati

Abstract

The invention relates to the technical field of active component extraction of rhizoma polygonati, in particular to a method for extracting and separating multiple active components in rhizoma polygonati, which comprises the following steps: step 1, raw material preparation: removing silt from rhizoma polygonati rhizome, cleaning, drying the cleaned rhizoma polygonati to constant weight, and grinding the dried rhizoma polygonati in a grinding centrifugal device; step 2, component extraction: performing ultrasonic-assisted pretreatment on the rhizoma polygonati; extracting flavonoid compounds in rhizoma polygonati by adopting an alcohol extraction method; extracting polysaccharide components in rhizoma polygonati by adopting an alcohol precipitation method; step 3, separation and purification: purifying the polysaccharide by using anion exchange column chromatography; and the flavonoid compounds are purified by using a macroporous resin adsorption method. According to the method disclosed by the invention, ultrasonic waves are utilized for pretreatment, so that the penetrating power of cell membranes is increased, and therefore, active substances in cells can easily permeate, and the purity and the quality of various active components in the finally extracted rhizoma polygonati are improved.

Description

Technical Field

[0001] The invention relates to the technical field of extracting active components of polygonatum, and in particular to a method for extracting and separating multiple active components in polygonatum. Background Art

[0002] Polygonatum sibiricum is a perennial herb, mainly distributed in mountain forests. The rhizome of Polygonatum sibiricum is often used for medicinal purposes. Polygonatum sibiricum contains a variety of active ingredients, including polysaccharides, flavonoids, sterols, etc. The active ingredients in Polygonatum sibiricum have a variety of pharmacological effects, such as antioxidant, anti-inflammatory, immunomodulatory, and anti-tumor. With the increasing demand for natural medicines and healthy foods, Polygonatum sibiricum has attracted much attention as an important medicinal plant.

[0003] In the prior art, when pre-treating polygonatum, a nine-steaming and nine-drying method is usually used, aiming to change the medicinal properties of polygonatum and improve its efficacy through multiple steaming and drying. However, during the steaming process, although polygonatum does not come into direct contact with water, the water vapor may bring out the volatile components on the surface of polygonatum, causing a certain degree of loss.

[0004] In summary, how to solve the problems of low efficiency and easy destruction of the active ingredients of Polygonatum sibiricum in the existing nine-steaming and nine-drying processing method has become a difficult problem that needs to be solved urgently in this field. Therefore, it is necessary to propose a method for extracting and separating multiple active ingredients in Polygonatum sibiricum. Summary of the invention

[0005] In order to solve the above problems, the present invention provides a method for extracting and separating multiple active ingredients in Polygonatum sibiricum, which uses ultrasonic pretreatment to increase the penetration ability of cell membranes and thus facilitate the infiltration of active substances in cells, thereby improving the purity and quality of the multiple active ingredients in Polygonatum sibiricum finally extracted.

[0006] In order to achieve the above object, the technical scheme of the present invention is as follows: A method for extracting and separating multiple active ingredients in polygonatum sibiricum, comprising the following steps:

[0007] Step 1, raw material preparation: remove the sand from the rhizome of polygonatum and wash it, dry the washed polygonatum to constant weight, put the dried polygonatum into a grinding centrifugal device for grinding, collect the polygonatum powder after grinding and store it in a dry and dark place;

[0008] Step 2, component extraction: using ultrasound to assist in pretreatment of polygonatum; using alcohol extraction to extract flavonoids from polygonatum; using alcohol precipitation to extract polysaccharide components from polygonatum;

[0009] Step 3, separation and purification: polysaccharide purification is carried out by anion exchange column chromatography; flavonoid compound purification is carried out by macroporous resin adsorption method;

[0010] Step 4, post-processing: freeze-dry the purified polysaccharides and flavonoids using a freeze dryer, and package and store the dried products.

[0011] Further, in step 1, the polygonatum drying method comprises the following steps:

[0012] S101, placing the washed polygonatum in a vacuum drying oven at 55-60° C. and drying for 1-2 hours to remove surface moisture;

[0013] S102, taking out the polygonatum after the surface moisture is dried and slicing;

[0014] S103, placing the sliced ​​Polygonatum sibiricum in a vacuum drying oven again at 55-60° C. and drying to constant weight.

[0015] Furthermore, in step one, the polygonatum sibiricum grinding method is: the dried flaky polygonatum sibiricum is placed in a grinding centrifugal device for repeated grinding, and after grinding, the polygonatum sibiricum particles are sieved with 60-80 mesh, and the sieved polygonatum sibiricum particles are stirred and crushed again to obtain polygonatum sibiricum powder.

[0016] Further, in step 2, the ultrasonic-assisted pretreatment includes the following steps:

[0017] S201, weigh 1-2 g of polygonatum sibiricum powder and place it in a beaker, and add distilled water at a material-liquid ratio of 10-40 mL / g;

[0018] S202, placing the beaker into an ultrasonic instrument, setting the extraction temperature to 40-80°C, the extraction time to 20-40 min, and the ultrasonic power to 100-300 W, and starting the ultrasonic instrument;

[0019] S203, cooling the liquid obtained in the ultrasonic instrument to room temperature, and filtering with gauze to obtain a pretreatment solution.

[0020] Further, in step 2, the alcohol extraction method comprises the following steps:

[0021] S301, concentrating the pre-treated solution under reduced pressure to obtain a concentrated solution;

[0022] S302, adding 15-30 mL of 50-90% ethanol extraction solvent to the concentrated solution, stirring and refluxing at 50-90° C. for 1-2 hours;

[0023] S303, after the stirred reflux solution is cooled, it is placed in a grinding centrifugal device, the speed is set to 3000-4000 r / min, centrifuged for 10-20 min, and the supernatant is collected;

[0024] S304, filtering the supernatant with an organic filter membrane of 0.22-0.45 μm, and concentrating the filtered liquid by rotary evaporation to obtain a crude extract of polygonatum flavonoids in a volumetric flask.

[0025] Further, in step 2, the alcohol precipitation method comprises the following steps:

[0026] S401, stirring the concentrated solution and adding 4 to 10 times the volume of 70% to 95% ethanol solution, and letting the alcohol precipitation stand for 12 to 24 hours;

[0027] S402, placing the solution after standing still in a grinding centrifugal device, setting the speed to 3000-4000 r / min, and centrifuging for 10-20 minutes to obtain a precipitate;

[0028] S403, adding distilled water to the precipitate to dissolve it, heating to evaporate the ethanol, and freeze-drying after evaporation to obtain crude polygonatum polysaccharide.

[0029] Further, in step three, the anion exchange column chromatography method comprises the following steps:

[0030] S501, weigh 100-200 mg of crude polygonatum polysaccharide, and dissolve it in 10-20 mL of deionized water;

[0031] S502, filtering with a 0.22-0.45 μm organic filter membrane, and loading the sample on a DEAE-Sepharose Fast Flow gel chromatography column at a flow rate of 1.0-2.0 mL / min;

[0032] S503, washing the crude Polygonatum cyrtonema polysaccharide with deionized water, 0.1 mol / L and 0.5 mol / L NaCl solutions in a gradient manner, and collecting the eluate;

[0033] S504, the eluate is concentrated by rotary evaporation and dialyzed with running water for 24 to 48 hours to obtain purified polygonatum sibiricum polysaccharide.

[0034] Further, in step 3, the macroporous resin adsorption method comprises the following steps:

[0035] S601, weigh 10-20 g of DM-130 macroporous adsorption resin, and load it into a 3 cm×50 cm chromatography column by wet method;

[0036] S602, 30-60 mL of a crude extract of polygonatum flavonoids with a concentration of 0.5-2.5 mg / mL is loaded at a volume flow rate of 1.0-2.0 mL / min, the adsorption time is 12-24 h, the adsorption temperature is 15-35° C., and the effluent is collected;

[0037] S603, after all the effluent has flowed out, 30-60 mL of distilled water is used to wash away water-soluble impurities, 70-80% ethanol solution is added for elution, the eluate is collected, and the eluate is concentrated by rotary evaporation to obtain a purified solution of polygonatum flavonoids.

[0038] Furthermore, the grinding centrifugal device comprises a mixing barrel, a plurality of support rods are fixedly connected to the bottom of the mixing barrel, and a grinding assembly for grinding materials and a stirring assembly for stirring materials are respectively arranged in the mixing barrel;

[0039] The grinding assembly includes a double-headed motor, which is electrically connected to a controller. The controller is used to control the opening and closing of the double-headed motor and the speed of the operation according to the degree of grinding of the material. A connecting plate is fixedly connected to the inner wall of the mixing barrel, and the double-headed motor is fixedly connected to the bottom of the connecting plate. The output shaft on the double-headed motor passes through the connecting plate and is coaxially fixedly connected to a rotating disk. The rotating disk is hinged with a "ヘ"-shaped hinged rod along its circumference; the end of the hinged rod away from the rotating disk is hinged with a grinding plate.

[0040] A plurality of slide grooves are provided on the top of the connecting plate, and a slider which slides in cooperation with the slide grooves is fixedly connected to the bottom of the grinding plate; the side of the grinding plate away from the double-headed motor is arc-shaped and contacts the inner wall of the mixing barrel; a screen is fixedly connected to the bottom of the connecting plate, and a centrifugal barrel is coaxially fixedly connected to the top of the rotating disk, and the centrifugal barrel rotates in cooperation with the grinding plate; a top cover is detachably connected to the top of the mixing barrel and the centrifugal barrel; a rotating shaft is coaxially fixedly connected to the output shaft on the double-headed motor, and one end of the rotating shaft which is away from the double-headed motor passes through the rotating disk and the bottom of the centrifugal barrel and extends to the inside of the centrifugal barrel; a plurality of cutting knives are fixedly connected to the rotating shaft inside the centrifugal barrel, and a plurality of openings are provided on the upper part of the side wall of the centrifugal barrel, and baffles are detachably connected to the outside of the openings.

[0041] Furthermore, the stirring assembly includes a stirring shaft, which is coaxially fixedly connected to the lower output shaft of the double-headed motor; a plurality of stirring teeth are fixedly connected to the stirring shaft;

[0042] A pressure sensor and a temperature sensor are fixedly connected to the inner wall of the mixing barrel, and a controller is used to receive signals from the pressure sensor and the temperature sensor; an air pump and a thermal energy regulator are fixedly connected to the outer wall of the mixing barrel, and output ends of the air pump and the thermal energy regulator are both connected to the interior of the mixing barrel, and the controller is used to control the operation of the air pump and the thermal energy regulator according to the pressure and temperature information inside the mixing barrel.

[0043] The above scheme has the following beneficial effects:

[0044] 1. This solution is driven by a double-headed motor. The cutting knife is used to crush the material first. After crushing, the material is thrown into the mixing barrel by centrifugal force and then ground to improve the efficiency of material grinding. The double-headed motor drives the hinged rod and the grinding plate to reciprocate to achieve uniform and efficient grinding of the material, so that the cell wall is broken and more active ingredients are released. The arc contact between the grinding plate and the inner wall of the mixing barrel and the cooperation between the slider and the chute ensure the stability and flexibility of the grinding process. After grinding, the material can be continuously stirred by the stirring teeth; then, the centrifugal barrel can effectively separate these active ingredients to improve the efficiency and purity of the extraction. By integrating multiple functions such as grinding, stirring, crushing and centrifugation, efficient processing of Polygonatum odoratum raw materials is achieved. The top of the mixing barrel and the centrifugal barrel are both equipped with a detachable top cover to facilitate the delivery and removal of materials. Integrating multiple functions in one, it can complete multiple processing steps at one time, greatly improving the processing efficiency, which is suitable for large-scale operations in the factory and further improving production efficiency and capacity.

[0045] The built-in pressure sensor and temperature sensor can monitor the working status inside the mixing barrel in real time to ensure that the extraction process is carried out under optimal conditions. By setting the respective thresholds and the intelligent control of the controller, the working status of the air pump and the thermal regulator can be automatically adjusted to maintain a stable internal environment, thereby protecting and improving the activity of the active ingredients in polygonatum. Accurate control of extraction conditions helps to reduce the loss of active ingredients during the extraction process. By optimizing the parameters of grinding, stirring and centrifugation, and accurately controlling the internal pressure and temperature, the various active ingredients in polygonatum can be effectively retained and the quality of the extract can be improved.

[0046] 2. This scheme uses ultrasound to assist in the pretreatment of Polygonatum sibiricum. Ultrasound is used to change the cell pressure difference of the herb, thereby destroying its cell wall and cell membrane structure, increasing the penetration ability of the cell membrane, and thus facilitating the exudation of active substances in the cell, thereby improving the efficiency of the subsequent extraction steps. At the same time, the ultrasonic method also has the effects of shaking and stirring, which can make the flavonoids in Polygonatum sibiricum continuously and uniformly dissolved in the extraction solvent. In addition, the ultrasonic method also brings about a heat transfer effect, which keeps the extraction process within a certain temperature range, improves the extraction efficiency of flavonoids to a certain extent, and shortens the extraction time. Because some impurities are removed during the pretreatment process and the extraction conditions are optimized, the purity and quality of the various active ingredients in the Polygonatum sibiricum finally extracted are improved.

[0047] 3. This scheme further enriches and purifies the target components through the selective dissolution and precipitation of organic solvents such as ethanol. The combination of multiple methods such as pretreatment of Polygonatum sibiricum and extraction of Polygonatum sibiricum activity by alcohol extraction and alcohol precipitation achieves efficient extraction of active ingredients in Polygonatum sibiricum. By finely adjusting key parameters such as temperature, time, solvent concentration and material ratio, the extraction process can be accurately controlled to ensure that flavonoids and polysaccharides are efficiently extracted. This refined operation not only improves the extraction efficiency, but also ensures the quality stability of the extract, reduces resource waste, and improves resource utilization efficiency. By optimizing the process flow and equipment configuration, continuous and automated production can be achieved, production efficiency can be improved, and market demand can be met; due to the efficiency and stability of the method, this scheme is suitable for large-scale industrial production.

[0048] 4. This scheme uses column chromatography separation when separating and purifying the components of Polygonatum odoratum. The principle is that the speed of diffusion into the gel voids varies according to the size and appearance of the compounds in the solution, so that separation can be achieved. When the polysaccharide solution passes through the chromatography column, substances with larger mass are blocked outside the gel voids due to their larger volume and can quickly pass through the chromatography column. Therefore, they have a short retention time in the column and are the first to flow out of the column. On the contrary, substances with small molecular weight can enter the interior of the gel. Due to the obstruction of the movement speed, they have a longer retention time and are finally eluted, thereby achieving the separation and purification of the active ingredients.

[0049] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] Figure 1 The present invention is a schematic diagram of a method for extracting and separating multiple active ingredients from polygonatum.

[0051] Figure 2 It is an axonometric view of an embodiment of a grinding centrifugal device of the present invention.

[0052] Figure 3 It is an axonometric view of an embodiment of a grinding assembly of the present invention.

[0053] Figure 4 It is a side cross-sectional view of an embodiment of a grinding centrifuge device of the present invention.

[0054] Figure 5 For the embodiment of the present invention Figure 4 Enlarged view of part A.

[0055] The figure marks in the drawings of the specification include: 1. stirring barrel; 2. support rod; 3. double-headed motor; 4. connecting plate; 5. rotating disk; 6. hinged rod; 7. grinding plate; 8. centrifugal barrel; 9. top cover; 10. stirring shaft; 11. stirring teeth; 12. air pump; 13. thermal energy regulator; 14. sieve; 15. cutting knife. DETAILED DESCRIPTION

[0056] The following is further described in detail through specific implementation methods:

[0057] Embodiment 1:

[0058] As attached Figure 1 As shown: A method for extracting and separating multiple active ingredients in polygonatum, comprising the following steps:

[0059] Step 1, raw material preparation: remove mud and sand from the rhizome of Polygonatum sibiricum and wash it, dry the washed Polygonatum sibiricum to constant weight, put the dried flake Polygonatum sibiricum into a grinding centrifugal device for repeated grinding, pass through a 60-mesh sieve after grinding, stir and crush the sieved Polygonatum sibiricum particles again to obtain Polygonatum sibiricum powder; collect the Polygonatum sibiricum powder after grinding and store it in a dry and dark place.

[0060] Wherein, the polygonatum drying method comprises the following steps:

[0061] S101, place the washed Polygonatum in a vacuum drying oven at 60°C for 1 hour to remove surface moisture; S102, take out the Polygonatum after the surface moisture is dried and slice it; S103, place the sliced ​​Polygonatum in a vacuum drying oven again at 60°C to dry until constant weight.

[0062] Step 2, component extraction: pre-treating the polygonatum sibiricum with the aid of ultrasound; the ultrasonic-assisted pre-treatment includes the following steps:

[0063] S201. Weigh 2 g of polygonatum powder and place it in a beaker, and add distilled water at a solid-liquid ratio of 40 mL / g; S202. Place the beaker in an ultrasonic instrument, set the extraction temperature to 80°C, the extraction time to 40 min, and the ultrasonic power to 250 W, and start the ultrasonic instrument; S203. Cool the liquid obtained in the ultrasonic instrument to room temperature, and filter it with gauze to obtain a pretreatment solution.

[0064] The flavonoid compounds in polygonatum are extracted by alcohol extraction; the alcohol extraction method comprises the following steps:

[0065] S301. Concentrate the pretreated solution under reduced pressure to obtain a concentrated solution; S302. Add 30 mL of 80% ethanol extraction solvent to the concentrated solution, and stir and reflux at 90°C for 2 hours; S303. After the stirred and refluxed solution is cooled, put it into a grinding centrifuge, set the speed to 3000 r / min, centrifuge for 20 minutes, and collect the supernatant; S304. Filter the supernatant with a 0.45 μm organic filter membrane, and after filtration, perform rotary evaporation and concentration to a fixed volume in a volumetric flask to obtain a crude extract of polygonatum flavonoids.

[0066] The polysaccharide components in Polygonatum sibiricum are extracted by alcohol precipitation method. The alcohol precipitation method includes the following steps:

[0067] S401. Stir the concentrated solution and add 10 times the volume of 95% ethanol solution, and let it stand for 24 hours; S402. Put the solution after standing into a grinding centrifuge and set the speed to 4000r / min. Centrifuge for 10 minutes to obtain a precipitate; S403. Add distilled water to the precipitate to dissolve it, heat to evaporate the ethanol, and freeze-dry after evaporation to obtain crude polygonatum polysaccharide.

[0068] Step 3, separation and purification: polysaccharide purification is performed using anion exchange column chromatography; anion exchange column chromatography includes the following steps:

[0069] S501. Weigh 100 mg of crude polygonatum polysaccharide and dissolve it in 10 mL of deionized water; S502. Filter with a 0.45 μm organic filter membrane and load the sample on a DEAE-Sepharose Fast Flow gel chromatography column at a flow rate of 2.0 mL / min; S503. Rinse the crude polygonatum polysaccharide with deionized water, 0.1 mol / L and 0.5 mol / L NaCl solutions in a gradient manner and collect the eluate; S504. Concentrate the eluate by rotary evaporation and dialyze it with running water for 48 hours to obtain purified polygonatum polysaccharide.

[0070] The flavonoids are purified by macroporous resin adsorption method; the macroporous resin adsorption method includes the following steps:

[0071] S601. Weigh 20 g of DM-130 macroporous adsorption resin and load it into a 3 cm×50 cm chromatography column using a wet method; S602. Load 60 mL of 2.0 mg / mL crude extract of polygonatum flavonoids at a volume flow rate of 2.0 mL / min, with an adsorption time of 12 h and an adsorption temperature of 35°C, and collect the effluent; S603. After all the effluent has flowed out, wash away water-soluble impurities with 60 mL of distilled water, add 80% ethanol solution for elution, collect the eluate, and concentrate the eluate by rotary evaporation to obtain a purified solution of polygonatum flavonoids.

[0072] Step 4, post-processing: freeze-dry the purified polysaccharides and flavonoids using a freeze dryer, and package and store the dried products.

[0073] Embodiment 2:

[0074] As attached Figure 2-Figure 5 As shown, the difference from the above embodiment is that the grinding centrifugal device includes a mixing barrel 1, a plurality of support rods 2 are bolted to the bottom of the mixing barrel 1, and a grinding component for grinding materials and a stirring component for stirring materials are respectively arranged in the mixing barrel 1.

[0075] The grinding assembly includes a double-headed motor 3, which is electrically connected to a controller. The controller is used to control the opening and closing and the speed of the double-headed motor 3 according to the degree of grinding required for the material; the inner wall of the mixing barrel 1 is bolted fixedly connected to a connecting plate 4, and the double-headed motor 3 is bolted fixedly connected to the bottom of the connecting plate 4; the output shaft of the double-headed motor 3 passes through the connecting plate 4 and is coaxially sleeved with a rotating disk 5, and the rotating disk 5 is hingedly connected to a "ヘ"-shaped hinged rod 6 along its circumference; a grinding plate 7 is hingedly connected to the end of the hinged rod 6 away from the rotating disk 5.

[0076] A plurality of slide grooves are provided on the top of the connecting plate 4, and a slider that slides in cooperation with the slide grooves is bolted to the bottom of the grinding plate 7; the side of the grinding plate 7 away from the double-headed motor 3 is arc-shaped and contacts the inner wall of the mixing barrel 1; a screen 14 is bolted to the bottom of the connecting plate 4, and a centrifugal barrel 8 is coaxially bolted to the top of the rotating disk 5, and the centrifugal barrel 8 rotates in cooperation with the grinding plate 7; the tops of the mixing barrel 1 and the centrifugal barrel 8 are both detachably threaded with a top cover 9; a rotating shaft is coaxially bolted to the top of the output shaft on the double-headed motor 3, and one end of the rotating shaft away from the double-headed motor 3 passes through the rotating disk 5 and the bottom of the centrifugal barrel 8 and extends to the interior of the centrifugal barrel 8, and a plurality of cutting knives 15 are bolted to the rotating shaft inside the centrifugal barrel 8, and a plurality of openings are provided on the upper part of the side wall of the centrifugal barrel 8, and a baffle is detachably connected to the outside of the openings.

[0077] The stirring assembly includes a stirring shaft 10, which is coaxially bolted to the lower output shaft of the double-head motor 3; a plurality of stirring teeth 11 are bolted to the stirring shaft 10; a pressure sensor and a temperature sensor are bolted to the inner wall of the stirring barrel 1, and a controller is used to receive signals from the pressure sensor and the temperature sensor; an air pump 12 and a thermal energy regulator 13 are bolted to the outer wall of the stirring barrel 1, and the output ends of the air pump 12 and the thermal energy regulator 13 are both connected to the inside of the stirring barrel 1, and the controller is used to control the operation of the air pump 12 and the thermal energy regulator 13 according to the pressure and temperature information inside the stirring barrel 1.

[0078] The specific implementation process is as follows: when grinding work is required, first open the top cover 9 on the mixing barrel 1 and the centrifugal barrel 8, and put the material into the centrifugal barrel 8. At this time, remove the baffle. Because the output shaft on the double-headed motor 3 passes through the connecting plate 4 and is coaxially sleeved and fixedly connected to the rotating disk 5, and the top of the rotating disk 5 is coaxially bolted and fixedly connected to the centrifugal barrel 8, when the double-headed motor 3 drives the rotating disk 5 to rotate, it can drive the centrifugal barrel 8 to rotate together. Since the top of the output shaft on the double-headed motor 3 is coaxially bolted and fixedly connected to the rotating shaft, and the end of the rotating shaft away from the double-headed motor 3 passes through the internal bolts of the centrifugal barrel 8 and is fixedly connected to a plurality of cutting knives 15, the double-headed motor 3 can also drive the cutting knives 15 to rotate. Since the upper part of the centrifugal barrel 8 has a plurality of openings, the material can be cut and crushed by the cutting knives 15. When the material reaches a certain degree of coarseness, it will be thrown to the openings on the upper part by the centrifugal force of the centrifugal barrel 8, and then thrown out into the mixing barrel 1 through the openings, so as to improve the grinding efficiency.

[0079] At the same time, since the inner wall of the mixing barrel 1 is fixedly connected with a connecting plate 4 by bolts, and a slide groove is opened on the connecting plate 4, and a slider that slides with the slide groove is fixedly connected with bolts at the bottom of the grinding plate 7, the grinding plate 7 can be moved horizontally in the mixing barrel 1 through the slider and the slide groove. Because the bottom of the connecting plate 4 is bolted and fixedly connected with the double-headed motor 3, the output shaft of the double-headed motor 3 passes through the connecting plate 4 and is coaxially bolted and fixedly connected with the rotating disk 5, and the rotating disk 5 is hinged with a plurality of "ヘ"-shaped hinged rods 6 along its circumference, and the ends of the hinged rods 6 away from the rotating disk 5 are hinged with the grinding plate 7, so the hinged rods 6 can be driven to expand outward through the rotating disk 5, and the grinding plate 7 is driven to expand outward together when expanding; on the contrary, when the rotating disk 5 rotates in the reverse direction, the hinged rods 6 can be retracted toward the rotating disk 5, and the grinding plate 7 is driven to retract toward the rotating disk 5 when retracting, and the reciprocating motion of the grinding plate 7 is realized in this way. In this process, when the grinding plate 7 expands outward, the double-headed motor 3 rotates half a circle in the forward direction, and when the grinding plate 7 shrinks inward, the double-headed motor 3 rotates half a circle in the reverse direction. At the same time, the centrifugal barrel 8 will also perform forward and reverse reciprocating motions accordingly, and this process can make the material evenly crushed and cut by the cutting knife 15, thereby improving the efficiency of material grinding.

[0080] by Figure 3 For example, when the double-headed motor 3 drives the rotating disk 5 to rotate clockwise, it can drive the right-side hinged rod 6 to move to the right, thereby driving the right-side grinding plate 7 to expand outward. At this time, the left-side hinged rod 6 also drives the grinding plate 7 to expand outward. In this way, the outward expansion of the grinding plate 7 is achieved; conversely, when the double-headed motor 3 drives the rotating disk 5 to rotate counterclockwise, it can drive the right-side hinged rod 6 to move to the left, thereby driving the right-side grinding plate 7 to shrink inward. At this time, the left-side hinged rod 6 also drives the grinding plate 7 to shrink inward. In this way, the reciprocating motion of the grinding plate 7 is achieved, thereby repeatedly grinding the material.

[0081] Since the connecting plate 4 is in the shape of a strip, and the screen 14 is distributed throughout the interior of the mixing barrel, the connecting plate 4 does not completely cover the screen 14, so the material can fall into the bottom of the mixing barrel 1 through the screen 14 after being ground, because the lower output shaft of the double-headed motor 3 is coaxially bolted and fixedly connected with the mixing shaft 10, and a plurality of stirring teeth 11 are bolted and fixedly connected with the stirring shaft 10, so at this time, the stirring teeth 11 can be driven by the double-headed motor 3 to rotate, thereby further stirring the material; when it is necessary to mix with the solvent, the material and the solvent can be further stirred by the stirring teeth 11. After the material is crushed and ground, the material is taken out. When the material needs to be centrifuged, the top cover 9 on the top of the mixing barrel 1 and the centrifugal barrel 8 is opened to put the material into the centrifugal barrel 8. At this time, the baffle is clamped at the opening on the outside of the centrifugal barrel 8 to prevent the material from being thrown out. Because the rotating disk 5 bolted and fixedly connected to the double-headed motor 3 is also bolted and fixedly connected to the centrifugal barrel 8, the centrifugal barrel 8 can be driven by the double-headed motor 3 to rotate, thereby realizing the centrifugal effect on the material. In this way, multiple functions such as grinding, crushing, stirring and centrifuging of materials can be achieved at the same time, which can further improve efficiency and is suitable for large-scale operations in factories.

[0082] During the operation of the device, the working pressure and temperature inside the stirring barrel 1 are monitored in real time through the pressure sensor and the temperature sensor. By setting the corresponding threshold value, when the controller receives that the internal pressure or temperature is high, the air pump 12 or the thermal energy regulator 13 is turned on to reduce the internal pressure and temperature accordingly. In this way, the material extraction conditions can be accurately controlled, thereby increasing the active ingredients of Polygonatum sibiricum and achieving efficient extraction.

[0083] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A method for extracting and separating multiple active ingredients from Polygonatum sibiricum, characterized in that: The following steps are involved: Step 1, raw material preparation: remove the sand from the rhizome of polygonatum and wash it, dry the washed polygonatum to constant weight, put the dried polygonatum into a grinding centrifugal device for grinding, collect the polygonatum powder after grinding and store it in a dry and dark place; Step 2, component extraction: pre-treating the polygonatum sibiricum with the aid of ultrasound; The flavonoids in polygonatum were extracted by alcohol extraction. The polysaccharide components in polygonatum were extracted by alcohol precipitation method. Step 3, separation and purification: polysaccharide purification is performed using anion exchange column chromatography; Flavonoids were purified using macroporous resin adsorption; Step 4, post-processing: freeze-dry the purified polysaccharides and flavonoids using a freeze dryer, and package and store the dried products.

2. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 1, characterized in that: In step 1, the polygonatum drying method comprises the following steps: S101, placing the washed polygonatum in a vacuum drying oven at 55-60° C. and drying for 1-2 hours to remove surface moisture; S102, taking out the polygonatum after the surface moisture is dried and slicing; S103, placing the sliced ​​Polygonatum sibiricum in a vacuum drying oven again at 55-60° C. and drying to constant weight.

3. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 2, characterized in that: In step one, the polygonatum sibiricum grinding method is: the dried flaky polygonatum sibiricum is placed in a grinding centrifugal device for repeated grinding, and after grinding, the polygonatum sibiricum is sieved with a 60-80 mesh sieve, and the sieved polygonatum sibiricum particles are stirred and crushed again to obtain polygonatum sibiricum powder.

4. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 3, characterized in that: In step 2, the ultrasonic assisted pretreatment includes the following steps: S201, weigh 1-2 g of polygonatum sibiricum powder and place it in a beaker, and add distilled water at a material-liquid ratio of 10-40 mL / g; S202, placing the beaker into an ultrasonic instrument, setting the extraction temperature to 40-80°C, the extraction time to 20-40 min, and the ultrasonic power to 100-300 W, and starting the ultrasonic instrument; S203, cooling the liquid obtained in the ultrasonic instrument to room temperature, and filtering with gauze to obtain a pretreatment solution.

5. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 4, characterized in that: In step 2, the alcohol extraction method comprises the following steps: S301, concentrating the pre-treated solution under reduced pressure to obtain a concentrated solution; S302, adding 15-30 mL of 50-90% ethanol extraction solvent to the concentrated solution, stirring and refluxing at 50-90° C. for 1-2 hours; S303, after the stirred reflux solution is cooled, it is placed in a grinding centrifugal device, the speed is set to 3000-4000 r / min, centrifuged for 10-20 min, and the supernatant is collected; S304, filtering the supernatant with an organic filter membrane of 0.22-0.45 μm, and concentrating the filtered liquid by rotary evaporation to obtain a crude extract of polygonatum flavonoids in a volumetric flask.

6. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 5, characterized in that: In step 2, the alcohol precipitation method comprises the following steps: S401, stirring the concentrated solution and adding 4 to 10 times the volume of 70% to 95% ethanol solution, and letting the alcohol precipitation stand for 12 to 24 hours; S402, placing the solution after standing still in a grinding centrifugal device, setting the speed to 3000-4000 r / min, and centrifuging for 10-20 minutes to obtain a precipitate; S403, adding distilled water to the precipitate to dissolve it, heating to evaporate the ethanol, and freeze-drying after evaporation to obtain crude polygonatum polysaccharide.

7. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 6, characterized in that: In step 3, the anion exchange column chromatography method comprises the following steps: S501, weigh 100-200 mg of crude polygonatum polysaccharide, and dissolve it in 10-20 mL of deionized water; S502, filtering with a 0.22-0.45 μm organic filter membrane, and loading the sample on a DEAE-Sepharose Fast Flow gel chromatography column at a flow rate of 1.0-2.0 mL / min; S503, washing the crude Polygonatum cyrtonema polysaccharide with deionized water, 0.1 mol / L and 0.5 mol / L NaCl solutions in a gradient manner, and collecting the eluate; S504, the eluate is concentrated by rotary evaporation and dialyzed with running water for 24 to 48 hours to obtain purified polygonatum sibiricum polysaccharide.

8. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 7, characterized in that: In step 3, the macroporous resin adsorption method includes the following steps: S601, weigh 10-20 g of DM-130 macroporous adsorption resin, and load it into a 3 cm×50 cm chromatography column by wet method; S602, 30-60 mL of a crude extract of polygonatum flavonoids with a concentration of 0.5-2.5 mg / mL is loaded at a volume flow rate of 1.0-2.0 mL / min, the adsorption time is 12-24 h, the adsorption temperature is 15-35° C., and the effluent is collected; S603, after all the effluent has flowed out, 30-60 mL of distilled water is used to wash away water-soluble impurities, 70-80% ethanol solution is added for elution, the eluate is collected, and the eluate is concentrated by rotary evaporation to obtain a purified solution of polygonatum flavonoids.

9. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 8, characterized in that: The grinding centrifugal device comprises a mixing barrel (1), a plurality of support rods (2) are fixedly connected to the bottom of the mixing barrel (1), and a grinding component for grinding materials and a stirring component for stirring materials are respectively arranged in the mixing barrel (1); The grinding assembly comprises a double-headed motor (3), the double-headed motor (3) is electrically connected to a controller, and the controller is used to control the opening and closing and the speed of the double-headed motor (3) according to the degree of grinding required for the material; a connecting plate (4) is fixedly connected to the inner wall of the mixing barrel (1), and the double-headed motor (3) is fixedly connected to the bottom of the connecting plate (4); an output shaft on the double-headed motor (3) passes through the connecting plate (4) and is coaxially fixedly connected to a rotating disk (5), and the rotating disk (5) is hingedly connected to a "ヘ"-shaped hinged rod (6) along its circumference; a grinding plate (7) is hingedly connected to one end of the hinged rod (6) away from the rotating disk (5); The top of the connecting plate (4) is provided with a plurality of slide grooves, and the bottom of the grinding plate (7) is fixedly connected with a slider that slides with the slide grooves; the side of the grinding plate (7) away from the double-headed motor (3) is arc-shaped and contacts the inner wall of the stirring barrel (1); the bottom of the connecting plate (4) is fixedly connected with a screen (14), and the top of the rotating disk (5) is coaxially fixedly connected with a centrifugal barrel (8), and the centrifugal barrel (8) and the grinding plate (7) are rotatably matched; the top of the stirring barrel (1) and the centrifugal barrel (8) are detachably connected with a top cover (9); the top of the output shaft of the double-headed motor (3) is coaxially fixedly connected with a rotating shaft, and the end of the rotating shaft away from the double-headed motor (3) passes through the rotating disk (5) and the bottom of the centrifugal barrel (8) and extends to the inside of the centrifugal barrel (8); the rotating shaft located inside the centrifugal barrel (8) is fixedly connected with a plurality of cutting knives (15), and the upper part of the side wall of the centrifugal barrel (8) is provided with a plurality of openings, and the outer side of the openings is detachably connected with a baffle.

10. The method for extracting and separating multiple active ingredients in Polygonatum sibiricum according to claim 9, characterized in that: The stirring assembly comprises a stirring shaft (10), which is coaxially fixedly connected to the lower output shaft of the double-headed motor (3); a plurality of stirring teeth (11) are fixedly connected to the stirring shaft (10); The inner wall of the mixing barrel (1) is fixedly connected to a pressure sensor and a temperature sensor, and the controller is used to receive signals from the pressure sensor and the temperature sensor; the outer wall of the mixing barrel (1) is fixedly connected to an air pump (12) and a heat regulator (13), the output ends of the air pump (12) and the heat regulator (13) are both connected to the inside of the mixing barrel (1), and the controller is used to control the operation of the air pump (12) and the heat regulator (13) according to the pressure and temperature information inside the mixing barrel (1).

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