CN113069492A - Production technology for ultrasonic-assisted continuous countercurrent extraction of sapindus saponin - Google Patents
Production technology for ultrasonic-assisted continuous countercurrent extraction of sapindus saponin Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
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- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses a production technology for ultrasonic-assisted continuous countercurrent extraction of soapberry saponin liquid, belongs to the technical field of medicine, chemical engineering and daily chemicals, relates to efficient and rapid extraction and separation of effective components of Chinese herbal medicine plants, and has remarkable effects in the aspects of saving time, reducing consumption and stabilizing product quality. The method is characterized by comprising the following steps of pretreatment of soapberry fruits, continuous feeding, countercurrent extraction of an extraction solvent and the fruits, preliminary filtration of an extracting solution, horizontal snail centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration, and centrifugal spin-drying discharge of pomace. The extraction solvent includes water, but is not limited to water; the extraction temperature of the soapberry fruits in the continuous extraction device is between room temperature and 95 ℃, and the treatment time is between 30 and 480 minutes; the mass ratio of the fruit to the extraction solvent is 1: 3-20, the ultrasonic frequency is 20000-100000 Hz, and the intensity is adjustable.
Description
Technical Field
The invention belongs to the technical field of medicine, chemical industry and daily chemicals, relates to efficient and rapid extraction and separation of effective components of Chinese herbal medicine plants, and has remarkable effects on time saving, consumption reduction and product quality stabilization.
Technical Field
Sapindus delavayi is a deciduous tree of Sapindaceae and Sapindaceae, and is distributed in the south of Huaihe river in China. Plant seeds are used for medicinal purposes (insect repellent); the seed oil can be used for preparing hardened oil; the peel can replace soap, can generate abundant foam, and has strong detergency mainly derived from soapberry saponin. The saponin is an excellent natural surfactant, and is especially suitable for washing fruits and vegetables, tableware, high-grade silk, pure wool fabrics and infant products, and daily chemicals such as toothpaste and the like. In addition, the sapindus saponin also has strong bacteriostatic and mosquito-repelling effects, is a good pesticide emulsifier, and also has good killing effect on cotton aphids, red spiders, sweet potato leaf beetles and the like.
The fructus Sapindi Mukouossi extract also contains bioactive components with antibacterial, antiinflammatory and natural nutrition regulating effects, has effects of removing dandruff and relieving itching, and can be used for treating tinea pedis and tinea cruris. Various medical books in ancient China have detailed records on the cleaning and medical effects of the soapberry, and the compendium of materia medica describes that the soapberry has the efficacies of clearing heat, eliminating phlegm, removing food retention, killing parasites, dispelling wind, improving eyesight, washing face, removing speckles and the like.
Relatively few reports are made at home and abroad on the extraction and separation technology of the sapindus saponin. At present, the extraction method of the soapberry saponin mainly comprises an ethanol extraction-solvent extraction separation process, and a light yellow soapberry saponin crude product can be obtained; however, the method has the disadvantages of large solvent consumption, complex process, high production cost and limited market responsiveness of the product. Also, a water extraction process is reported to obtain an aqueous solution product with the content of effective substances of 15 to 28 percent; the batch operation of feeding and discharging is labor-consuming and time-consuming, the impurity removal and concentration processes are difficult, and the efficiency is low.
In recent years, the technology of extracting the effective components of the traditional Chinese medicine by using an ultrasonic auxiliary means is gradually popularized and manufactured, and the technologies such as ultrafiltration membrane filtration, reverse osmosis membrane concentration and the like are also applied to the procedures of water treatment, target object purification and the like. However, the series combination of the saponin and the saponin is not reported to be applied to the extraction and production of the sapindus saponin.
Disclosure of Invention
The invention provides a production technology for ultrasonic-assisted continuous countercurrent extraction of soapberry saponin, and aims to solve the problems of high solvent consumption, long time consumption, complex process operation, high product cost, unstable quality, damaged heat-sensitive substances, limited resource waste and the like in the existing extraction production process of soapberry saponin.
The invention adopts the following scheme to solve the technical problems, including but not limited to the following procedures of pretreatment of soapberry fruits, continuous feeding, countercurrent extraction of an extraction solvent and the fruits, preliminary filtration of an extracting solution, horizontal spiral centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and centrifugal drying discharge of fruit residues.
The invention has the following beneficial effects:
1. the fruits and the extraction water adopt a continuous feeding mode, so that the labor and time are saved, the operation is convenient, and the working efficiency is high;
2. the cavitation effect of ultrasonic high-frequency vibration is utilized to effectively break the structural barriers of the fruits and improve the extraction rate of the sapindus saponin;
3. the solid phase and the liquid phase realize reverse flow and full contact in the device, effectively increase the concentration difference (mass transfer driving force) of the soapnut saponin in the whole extraction process, strengthen the mass transfer efficiency, greatly improve the extraction effect of the soapnut saponin and greatly shorten the extraction time reaching a certain extraction rate;
4. except water and filtration and centrifugal operation, other chemical substances and chemical treatment processes are not used, so that the active ingredients in the soapberry fruit are prevented from being denatured and damaged, and the full naturalness and the original biological activity of the soapberry saponin extracting solution are maintained;
5. the extracted pomace is centrifugally dried for discharging, so that the soapberry saponin is fully recovered, other complicated steps of bagging, disassembling a filter frame and cleaning a filter bag for solid matter filtering treatment are avoided, continuous operation can be realized, and the working efficiency is high.
Description of the drawings:
FIG. 1 is a schematic view of an ultrasonic-assisted, continuous countercurrent extraction apparatus, wherein,
1-propeller conveying motor; 2-a charging motor; 3-soapberry fruit; 4-fruit propulsion propeller; 5-ultrasonic energy converter; 6-hot water for extraction; 7-a residue lifting mechanism; 8, recovering the extracting solution by using a centrifugal machine; 9-extraction device support; 10-extracting solution.
In the device, the soapberry fruit and the extracted residues are pushed from left to right, and the water and the extracting solution flow from right to left; the two move in opposite directions and contact with each other to generate mass transfer extraction.
Fig. 2 is a schematic view of a propeller impeller pushing sapindus fruit, wherein,
1-flow direction of extract (water); 2-propeller blade; 3-extraction pipeline; 4-liquid passing hole; 5-central shaft of propeller; 6-the trend of the fruit (dregs); 7-fruit pomace; 8-soapberry fruit.
The specific implementation mode is as follows:
the technical solution of the present invention is further illustrated by the following examples.
Example 1
Removing impurities such as foreign matters, pedicels and twigs from newly picked fresh fructus Sapindi Mukouossi, sieving to remove dust such as soil, and washing with cold water (spraying) to clean; and (3) fracturing the soapberry by using a proper stainless steel plate to generate certain cracks and fissures on the surface of the soapberry. Starting an ultrasonic energy converter of the continuous extraction device to generate ultrasonic waves; simultaneously starting a hot water delivery pump, and adding hot water preheated to 95 ℃ into the extraction pipeline from a liquid adding port at the other end of the continuous extraction device; adding fresh soapberry fruits into a feeding hopper of a continuous extraction device, and starting a motor of a material conveying threaded impeller to slowly push the soapberry fruits forward to an extraction pipeline; ultrasonic-assisted continuous countercurrent extraction of sapindus saponin is started when fresh sapindus fruits are contacted and mixed with hot water.
Controlling the running speed of a motor of the material conveying threaded turbine wheel to ensure that the retention time of the fresh soapberry fruits in the extraction pipeline is 3 hours; controlling the output flow of the hot water delivery pump to ensure that the ratio of the weight of the fresh soapberry fruits to the amount of the hot water pumped in is 1: 5. Starting a liquid outlet vacuum pump, and pumping the extract through a filtering (fluff) cloth bag in the filtering tank to discharge the extract out of the extraction device. Starting a fruit residue lifter near the liquid feeding end of the continuous extraction device, continuously lifting and guiding extracted fruit residues into a central inlet of the three-foot type centrifugal filter, and further recovering the extracting solution in the residues by using the action of centrifugal force.
And (3) sequentially carrying out horizontal spiral centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and other processes on the extracting solution discharged from the extracting device to obtain the bright yellow extracting solution with the soapberry total saponin content of 11.3 mg/mL. The dry residue is thrown off by centrifugation and discharged out of the centrifugal filter intermittently. The extraction rate of the soapberry fruit saponin is 79.3 percent.
Example 2
Taking the dried soapberry fruits, removing impurities such as twigs, foreign matters and the like, peeling the peels and the kernels by using a soapberry kernel peeling machine, and screening to remove impurities such as the pedicles, the soil and the like for later use. Starting an ultrasonic energy converter of the continuous extraction device to generate ultrasonic waves; simultaneously starting a hot water delivery pump, and adding hot water preheated to 80 ℃ into the extraction pipeline from a liquid adding port at the other end of the continuous extraction device; adding the dried soapberry peel into a feeding hopper of a continuous extraction device, and starting a motor of a material conveying threaded impeller to slowly push the soapberry peel forward to an extraction pipeline; the soapberry peel is contacted with hot water to carry out ultrasonic-assisted continuous countercurrent extraction of saponin.
Controlling the running speed of a motor of the material conveying threaded turbine wheel to ensure that the retention time of the soapberry peel in the extraction pipeline is 6 hours; controlling the output flow of the hot water delivery pump to ensure that the total weight ratio of the soapberry peel weight to the hot water pumping amount is 1: 8. Starting a liquid outlet vacuum pump, and pumping the extract through a filtering (fluff) cloth bag in the filtering tank to discharge the extract out of the extraction device. Starting a fruit residue lifter near the liquid feeding end of the continuous extraction device, continuously lifting and guiding extracted fruit residues into a central inlet of the three-foot type centrifugal filter, and further recovering the extracting solution in the residues by using the action of centrifugal force.
And (3) sequentially carrying out horizontal spiral centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and other processes on the extracting solution discharged from the extracting device to obtain a light yellow extracting solution with the soapberry total saponin content of 12.6 mg/mL. The dry residue is thrown off by centrifugation and discharged out of the centrifugal filter intermittently. The extraction rate of the sapindus mukorossi fruit saponin is 84.5%.
Example 3
Taking the dried soapberry fruits, removing impurities such as twigs, foreign matters and the like, peeling the peels and the kernels by using a soapberry kernel peeling machine, and screening to remove impurities such as the pedicles, the soil and the like for later use. Starting an ultrasonic energy converter of the continuous extraction device to generate ultrasonic waves; simultaneously starting a hot water delivery pump, and adding hot water preheated to 55 ℃ into the extraction pipeline from a liquid adding port at the other end of the continuous extraction device; adding the dried soapberry peel into a feeding hopper of a continuous extraction device, and starting a motor of a material conveying threaded impeller to slowly push the soapberry fruit forward to an extraction pipeline; contacting fresh fructus Sapindi Mukouossi with hot water, and performing ultrasonic-assisted continuous countercurrent extraction of Sapindus saponin.
Controlling the running speed of a motor of the material conveying threaded turbine wheel to ensure that the retention time of the fresh soapberry fruits in the extraction pipeline is 400 minutes; controlling the output flow of the hot water delivery pump to ensure that the ratio of the weight of the fresh soapberry fruits to the amount of the hot water pumped in is 1: 12. Starting a liquid outlet vacuum pump, and pumping the extract through a filtering (fluff) cloth bag in the filtering tank to discharge the extract out of the extraction device. Starting a fruit residue lifter near the liquid feeding end of the continuous extraction device, continuously lifting and guiding extracted fruit residues into a central inlet of the three-foot type centrifugal filter, and further recovering the extracting solution in the residues by using the action of centrifugal force.
And (3) sequentially carrying out horizontal spiral centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and other processes on the extracting solution discharged from the extracting device to obtain a light yellow extracting solution with the soapberry total saponin content of 10.2 mg/mL. The dry residue is thrown off by centrifugation and discharged out of the centrifugal filter intermittently. The extraction rate of the sapindus mukorossi fruit saponin is 78.5%.
The sequence of the above embodiments is only for convenience of description, and does not represent the superiority and inferiority of the extraction efficiency of the embodiments.
Comparative example 1
Taking the dried Sapindus mukorossi Gaertn, removing impurities such as twigs and foreign matters, peeling peel and kernel with a Sapindus mukorossi kernel peeling machine, removing impurities such as pedicles and soil, sieving with a 20-mesh standard sieve, and collecting the undersize fraction for use.
Taking 10kg of the sieved dried soapberry peel, pouring into an extraction kettle, adding 100kg of hot water preheated to 95 ℃ into the extraction kettle, starting mechanical stirring immediately to ensure that the soapberry peel is fully contacted with the hot water, introducing steam through a jacket to maintain the temperature of the feed liquid at 95 ℃, and carrying out water boiling extraction on saponin.
Continuously stirring, controlling the temperature of the feed liquid at 95 +/-2 ℃, and maintaining the state for 4 hours to perform water boiling extraction. And stopping stirring after the extraction time reaches 4 hours, opening a discharging ball valve at the bottom of the kettle, and introducing the extracted pulp residues and the extracting solution into a filtering (down) cloth bag for primary filtering. Then taking out the filter bag and the residues, putting the filter bag and the residues into a three-foot centrifugal filter, starting a motor of the centrifugal filter, and recovering the extracting solution in the residues by using the action of centrifugal force.
Collecting the primarily filtered extract and filtrate obtained by centrifugal drying recovery by a centrifuge, and sequentially carrying out horizontal snail centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and other processes to obtain 102kg of light yellow soapberry saponin extract, wherein the content of soapberry total saponin is 8.9 mg/mL. The total extraction rate of the soapberry fruit saponin is 66.4%.
Comparative example 2
Removing impurities such as foreign matters, pedicels and twigs from freshly picked fresh fructus Sapindi Mukouossi, sieving to remove dust such as soil, and washing with cold water (spraying) to clean; and (3) fracturing the soapberry by using a proper stainless steel plate to generate certain cracks and splits on the surface of the soapberry. Pouring 8kg of the fresh soapberry fruits into a cleaning tank of an ultrasonic cleaning machine; then 96kg of hot water preheated to 65 ℃ is added into the cleaning tank, and the motor is started to generate ultrasonic waves for ultrasonic-assisted extraction. And intermittently introducing steam, and maintaining the temperature of the feed liquid at 65 ℃.
Continuously generating ultrasonic waves, and controlling the temperature of the feed liquid at 65 +/-2 ℃. When the state is maintained for 5 hours, the ultrasonic energy converter is closed, and the extracted pulp residue and the extracting solution are transferred into a filtering (down) cloth bag together for primary filtering from the cleaning tank by using a plastic ladle or a spoon. Then taking out the filter bag and the residues, putting the filter bag and the residues into a three-foot centrifugal filter, starting a motor of the centrifugal filter, and recovering the extracting solution in the residues by using the action of centrifugal force.
Collecting the primarily filtered extract and filtrate obtained by centrifugal drying and recovering by a centrifuge, and sequentially carrying out horizontal snail centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration and other processes to obtain yellowish soapberry saponin extract 99kg, wherein the soapberry total saponin content is 7.5 mg/mL. The total extraction rate of the soapberry fruit saponin is 59.9%.
Comparing the extraction processes and efficiencies of the 3 embodiments and 2 comparative examples, it can be seen that, by adopting the technical scheme of the present invention, the beneficial effects of the above 5 aspects can be achieved: labor and time are saved, the operation is convenient, and the working efficiency is high; the extraction rate of the soapberry saponin is improved; the extraction time for reaching a certain extraction rate can be greatly shortened; can maintain the natural property and original bioactivity of the sapindus saponin extract.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A production technology for ultrasonic-assisted continuous countercurrent extraction of sapindus saponin comprises the steps of pretreatment of sapindus fruits, continuous feeding, countercurrent extraction of an extraction solvent and the fruits, preliminary filtration of an extracting solution, horizontal spiral centrifugal separation, ultrafiltration membrane filtration, reverse osmosis membrane concentration, and centrifugal spin-drying and discharging of fruit residues.
2. The ultrasonic-assisted continuous countercurrent extraction production technology of sapindus saponin as claimed in claim 1, wherein the extraction solvent includes water, but is not limited to water, the extraction temperature of sapindus fruit in the continuous extraction device is room temperature-95 ℃, the treatment time is 30-480 minutes, and the mass ratio of fruit to extraction solvent is 1: 3-20, the ultrasonic frequency is 20000-100000 Hz, and the intensity is adjustable.
3. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein the pretreatment of soapberry fruit comprises the following steps.
1) Removing foreign matter, pedicel, and twig from picked or purchased fructus Sapindi Mukouossi, sieving to remove dust such as mud, washing with cold water (or sprinkling), and air drying.
2) When the fresh fruit extraction process is adopted, the soapberry fruit is fractured by a mechanical means, so that certain cracks and crazes are generated on the surface of the peel for later use.
3) When the dry fruit extraction process is adopted, a soapberry kernel stripping device is used for stripping and separating peel and kernel of the soapberry, the peel (flesh) is reserved, and the kernel can be used for other purposes.
4) When the dry fruit extraction process is adopted, the pulp can be subjected to necessary crushing treatment, and the crushing can be avoided.
4. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein the continuous feeding is to continuously feed soapberry fruit into the extraction pipe or trough through a hopper at the material inlet of the continuous extraction device, and to continuously feed the extraction solvent (such as water) into the extraction pipe or trough through an infusion pump at the other end of the continuous extraction device.
5. The ultrasonic-assisted continuous countercurrent extraction production technology for soapberry saponin according to claim 1, wherein the solvent and fruit are added at different ports of the continuous extraction device according to the feeding method of claim 4, the fruit is slowly moved from the material inlet to the other end of the device by propelling a spiral vortex blade or a mechanical rotating device, the solvent and the extracting solution slowly flow from a high position to a low position by an intentionally-arranged inclination in the horizontal direction of the continuous extraction device, the fruit and the solvent are fully contacted in the process of countercurrent movement, and the dissolution, extraction and extraction of soapberry saponin are realized, and the countercurrent continuous extraction can be arranged in the device in a whole-segment straight line (circumference) manner or in a segmented or turning manner.
6. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein the primary filtration of the extraction liquid is achieved by the mechanical action of centrifugal pump or vacuum pump near the material inlet of the continuous extraction device to make the extraction liquid exit the extraction device and enter and pass through the filtering (fluff) cloth bag arranged in the filtering tank.
7. The ultrasonic-assisted continuous countercurrent extraction production technology of sapindus saponin as claimed in claim 1, wherein the horizontal decanter centrifugation is to introduce the extract filtered by the filter tank cloth bag into a horizontal decanter centrifuge, and to throw the extract from the outer ring of the double-layer tube in the center of the centrifuge to the inner wall of the container in the centrifuge by the centrifugal force provided by the rotating helical blades, wherein the object with large mass is attached to the wall of the container, and the sapindus saponin and the solvent with small mass are gathered at the center of the horizontal decanter centrifuge, and overflow flows out of the horizontal decanter centrifuge from the inner tube of the double-layer tube, thereby realizing further separation.
8. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein said ultrafiltration membrane filtration is to filter the extract after centrifugation with an ultrafiltration (nanofiltration) membrane with cut-off molecular weight of more than 3000 daltons (or pore size of 1000nm) to remove macromolecular substances (such as protein, starch and polysaccharide).
9. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein said reverse osmosis membrane concentration is performed by using reverse osmosis membrane concentration device to perform reverse osmosis treatment on the extract filtered by ultrafiltration membrane to remove water molecules and obtain concentration, so that the content of soapberry total saponin is increased to meet the requirement of product quality standard.
10. The ultrasonic-assisted continuous countercurrent extraction production technology of soapberry saponin as claimed in claim 1, wherein the centrifugal spin-drying and discharging step of the fruit residues comprises the steps of arranging a hopper type lifting mechanism at the solvent feeding end of the continuous extraction device, continuously lifting and guiding the extracted fruit residues pushed by a spiral vortex blade or a mechanical rotation device into the central inlet of a three-foot type centrifugal filter, further recovering the extraction liquid in the residues by the action of centrifugal force, and intermittently discharging the residues subjected to centrifugal spin-drying out from the centrifugal filter, thereby realizing the continuous operation and production of solid materials and extraction liquid materials.
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