Method for extracting soap suds of soapberry by supramolecular solvent

By combining electric field-mediated super-dynamic crushing with supramolecular solvents, oscillating gradient column chromatography, and pneumatic magnetic stirring foaming device, the problems of low extraction rate and unsatisfactory purity of Sapindus mukorossi saponins were solved, achieving efficient and economical extraction and purification.

CN116173548BActive Publication Date: 2026-06-30SHENZHEN SHINESKY BIOLOGICAL TECH CO LTD +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
SHENZHEN SHINESKY BIOLOGICAL TECH CO LTD
Filing Date
2023-01-06
Publication Date
2026-06-30

AI Technical Summary

Technical Problem

The current technology for the extraction and purification of Sapindus mukorossi saponins has not been studied in depth, and there are problems such as large solvent loss, long cycle, low extraction rate and unsatisfactory purity.

Method used

A method of treating composite supramolecular solvents by electric field-mediated super-dynamic crushing, combined with an oscillating gradient column chromatography and a gas magnetic stirring foaming device, was used to extract and purify Sapindus mukorossi saponins.

Benefits of technology

It improves the extraction rate and purity of Sapindus mukorossi saponins in a short period of time, making it suitable for large-scale industrial production, reducing solvent and time costs, and is pollution-free.

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Abstract

This invention provides a method for extracting Sapindus mukorossi saponins using a supramolecular solvent, relating to the field of plant component extraction technology. The method includes the following steps: (1) dissolving the amphiphilic compound in ethanol or acetonitrile, adding water, vortexing, centrifuging, and collecting the upper layer to obtain the supramolecular solvent; (2) drying and pulverizing Sapindus mukorossi, adding the supramolecular solvent and cellulase, and extracting crude saponins using electric field-mediated super-dynamic crushing technology; (3) adsorbing the crude saponins onto a column using resin under oscillation; after washing, eluting with an aqueous ethanol solution under oscillation gradient, and drying to obtain Sapindus mukorossi saponin powder; (4) dissolving the powder in water and transferring it to a gas magnetic stirring foaming device to collect the foam, defoaming with ultrasound to obtain a refined saponin aqueous solution, and evaporating and concentrating to obtain Sapindus mukorossi saponin refined powder. This invention uses an electric field-mediated super-dynamic crushing composite supramolecular solvent, supplemented by oscillation gradient column method and gas magnetic stirring foaming device, which can extract Sapindus mukorossi saponins with higher purity in a short time.
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Description

Technical Field

[0001] This invention relates to the field of plant component extraction technology, and in particular to a method for extracting Sapindus mukorossi saponins using supramolecular solvents. Background Technology

[0002] Soapberry (Sapindus mukorossi Gaertn.), also known as oil soapberry, is a subtropical plant. In traditional Chinese culture, soapberry extract is often used to wash hair and body. The Compendium of Materia Medica records the use of soapberry extract to wash hair to remove dandruff and to wash the face to whiten and remove blemishes.

[0003] Sapindus mukorossi saponins are one of the important active ingredients in Sapindus mukorossi, mainly found in the fruit. They are natural nonionic surfactants with good foaming and detergency properties; Sapindus mukorossi saponins are also excellent pesticide emulsifiers. Pharmacological studies have shown that the saponin components contained in the Sapindus mukorossi pericarp have various biological activities, including antibacterial effects and inhibition of breast cancer.

[0004] Sapindus mukorossi saponins are an important component of the Sapindus mukorossi pericarp, mainly including three types: oleanane-type saponins, dammarane-type saponins, and triterpenoid saponins. Sapindus mukorossi pericarp is rich in saponins and aglycones, making it an excellent natural nonionic surfactant. It effectively promotes the leaching and removal of heavy metals from soil, exhibiting excellent decomposition effects. Most importantly, it leaves no harmful residues and has low skin sensitivity, making it a high-quality raw material for skincare products, shampoos, and various biological detergents.

[0005] From an environmental perspective, Sapindus mukorossi saponins are a natural surfactant that can be 100% decomposed, causing no pollution to the environment and adapting to various extreme conditions. As a high-performance natural surfactant, Sapindus mukorossi saponins are clearly superior to other detergents on the market in terms of ecological protection, and also offer significant economic and social benefits.

[0006] However, current research on the extraction and purification of Sapindus mukorossi saponins is still in its early stages, with limited in-depth studies and drawbacks such as significant solvent loss, long extraction cycles, low extraction rates, and unsatisfactory purity. Therefore, finding an efficient and economical purification method is a key issue that urgently needs to be addressed for Sapindus mukorossi saponins. Summary of the Invention

[0007] To address the aforementioned problems in existing technologies, this invention provides a method for extracting Sapindus mukorossi saponins using supramolecular solvents. This invention employs an electric field-mediated super-dynamic fragmentation process using a composite supramolecular solvent, supplemented by an oscillating gradient column chromatography method and a gas-magnetic stirring foaming device, enabling the extraction of Sapindus mukorossi saponins with higher purity in a short time.

[0008] The technical solution of the present invention is as follows:

[0009] A method for extracting saponins from Sapindus mukorossi using supramolecular solvents includes the following steps:

[0010] (1) Dissolve the amphiphilic compound in ethanol or acetonitrile, add water to form aggregates, then vortex and centrifuge, take the upper layer to obtain the supramolecular solvent.

[0011] (2) Dry the fruit and / or peel of Sapindus mukorossi and pulverize them into powder. Add supramolecular solvent and cellulase, mix well, extract using electric field-mediated super-powered crushing technology, then perform ultrasonic treatment, and obtain crude saponins after centrifugation, filtration, evaporation and concentration.

[0012] (3) The crude saponins were adsorbed onto the column by shaking using D101c type resin; after the adsorption was completed, the resin was washed, and finally the eluent was eluted by shaking gradient with an aqueous ethanol solution. The eluent was dried to obtain Sapindus mukorossi saponin powder.

[0013] (4) Dissolve the above Sapindus mukorossi saponin dry powder in water, transfer it to a gas magnetic stirring foaming device to collect foam, and then obtain a refined saponin aqueous solution after ultrasonic defoaming. Finally, obtain Sapindus mukorossi saponin refined powder by evaporation and concentration.

[0014] Preferably, the amphiphilic compound in step (1) is octanoic acid.

[0015] Preferably, the mass percentage of each raw material in step (1) is: 2-5% amphiphilic compound, 15-30% ethanol or acetonitrile, and the remainder is water.

[0016] Further, the centrifugation speed in step (1) is 6000-10000 r / min, and the centrifugation time is 10-15 minutes.

[0017] Preferably, in step (2), the soapberry fruit and / or pericarp are pulverized into a powder of 20-120 mesh.

[0018] Preferably, the solid-liquid ratio of the powder to the supramolecular solvent in step (2) is 1:10-25 g / mL, and the mass of the cellulase is 1-2% of the total mass of this step.

[0019] Preferably, the electric field-mediated super-dynamic crushing technology in step (2) is achieved by applying an electric field to the outside of the flash extractor, wherein the rotation speed of the flash extractor is 8000-12000 r / min and the time is 20s-80s; the magnitude of the electric field is 300-700 V / cm.

[0020] Furthermore, the ultrasonic time in step (2) is 10 min to 30 min; the extraction rate of crude saponins obtained by centrifugation, filtration, evaporation and concentration can reach 92% to 97%.

[0021] Preferably, in step (3), when using D101c type resin to adsorb crude saponins onto the column by shaking, the crude saponins are first dissolved in water to adjust the pH to 7-9. During adsorption, 150-250 mL of D101c type resin corresponds to 250-350 mL of extract. After shaking the column, the resin is washed with water or an aqueous solution with a concentration of 10%-30% ethanol for 2-4 bv, and then eluted with a 2-4 bv aqueous solution with a concentration of 60%-90% ethanol by shaking gradient, and the eluent is collected.

[0022] Further, step (3) drying yields a dry powder with a soapberry saponin purity of 70% to 80%.

[0023] Preferably, when the Sapindus mukorossi saponin powder in step (4) is dissolved in water, the material-to-liquid ratio is 1:20 to 1:40, and 0.5 to 1 wt% activated carbon is added at the same time.

[0024] Preferably, the gas-magnetic stirring bubbling device in step (4) is a bubbling device with a magnetic stirring device added, wherein air, carbon dioxide, or nitrogen is introduced into the bubbling device at a flow rate of 2-5 m / s. 3 / h, rotation speed is 500~2000r / min.

[0025] Preferably, the ultrasonic defoaming in step (4) refers to the foam being discharged through the foam outlet to the ultrasonic foam collector for defoaming; the ultrasonic foam collector is an ultrasonic device added to the defoaming equipment.

[0026] Furthermore, the refined saponin aqueous solution obtained in step (4) can be concentrated by evaporation to obtain Sapindus mukorossi saponin powder with a purity of about 90% to 98%.

[0027] The concentration of the above-mentioned aqueous solution of ethanol is a volume concentration.

[0028] The beneficial technical effects of this invention are as follows:

[0029] 1. This invention is the first to utilize an electric field-mediated super-dynamic crushing method for processing composite supramolecular solvents, screening out a superior supramolecular solvent suitable for industrial extraction of Sapindus mukorossi saponins. The extraction time is shorter and the extraction rate is higher, which can increase the extraction rate of Sapindus mukorossi saponins to about 95% in a short time. Moreover, the screened supramolecular solvent is safe and pollution-free, and is suitable for large-scale industrial production.

[0030] 2. This invention is the first to optimize the traditional macroporous resin purification method by using a combination of oscillating gradient and elution. Specifically, the column pass is made by using a combination of oscillating gradient and elution during the macroporous resin purification process, which significantly increases the single-pass purification effect of the crude extract and allows the purity of Sapindus saponins to reach about 75%.

[0031] 3. This invention is the first to use a gas-magnetic stirring foaming device and an ultrasonic defoamer to refine Sapindus mukorossi saponins. The combined effect of gas introduction and magnetic stirring allows for faster foam generation of Sapindus mukorossi saponins, and the refined saponin foam can be quickly defoamed under ultrasonic treatment. Finally, the refined Sapindus mukorossi saponin powder is obtained through evaporation and concentration, achieving a purity of approximately 95%. This method is simple to operate, saves solvent and time costs, and is safe and pollution-free. Attached Figure Description

[0032] Figure 1 The diagram shows the equipment structure of the electric field-mediated super-powered crushing technology. The correspondence between the names of the components and the numbers in the attached figures is as follows: 1-Power supply; 2-Stirring motor; 3-Stirring head; 4-External electric field. Detailed Implementation

[0033] The present invention will now be described in detail with reference to the accompanying drawings and embodiments. Obviously, the described embodiments are merely some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0034] In the following embodiments, the device for the electric field-mediated super-dynamic crushing technology is based on the KM1-JHBE-50T flash extractor from Beijing Haifuda Technology Co., Ltd., with an external electric field applied. Parameters are adjusted to ensure the extract is stirred and crushed within a uniform electric field. The structure is as follows: Figure 1 As shown. The device includes the flash extractor itself, such as its own stirring motor 2 and stirring head 3; an external electric field 4 is set outside the flash extractor, which is powered by the power supply 1.

[0035] In the following embodiments, the gas magnetic stirring foaming device adds a magnetic stirring device during the bubbling process, wherein the magnetic stirrer is a 79-1 constant temperature magnetic stirrer from Changzhou Juhui Instrument Manufacturing Co., Ltd.; the ultrasonic defoaming refers to adding an ultrasonic device during the defoaming process, wherein the ultrasonic device is a P360-15T ultrasonic cleaner from Kunshan Ouhua Ultrasonic Technology Co., Ltd., with an ultrasonic power of 40KHZ. The structure of the above-mentioned bubbling and defoaming devices refers to the equipment structure provided in CN111249766A "A foam generating and collecting device and a method for extracting total saponins", namely the layout and structure of the foam generating tower, the foam collecting tower, and the gas control system.

[0036] Example 1: Selection of solvent for extracting Sapindus mukorossi saponins

[0037] (1) Pulverization: Dry and pulverize the soapberry into 60-mesh powder.

[0038] (2) Add extraction solvent: Weigh 100g of Sapindus mukorossi powder into three portions, and add water, ethanol and supramolecular solvent (5% octanoic acid, 25% ethanol and 70% water) respectively according to the solid-liquid ratio of 1:15g / mL to obtain extracts 1, 2 and 3.

[0039] (3) Enzymatic hydrolysis: Add 2% cellulase to extracts 1, 2 and 3 respectively, mix well and set aside.

[0040] (4) Extraction: Using the traditional method, the enzymatically hydrolyzed extracts 1, 2, and 3 were stirred and heated to 70°C, and kept at this temperature for 2 hours. After the extraction, the liquid was filtered through a filter cloth. The corresponding solvent was then added to the residue, stirred, and heated to 70°C, and kept at this temperature for 2 hours. After the extraction, the extracts were combined.

[0041] (5) Centrifugal drying: Extracts 1, 2 and 3 were centrifuged at 4200 r / min for 10 min, and then concentrated and freeze-dried under reduced pressure to obtain crude saponins 1, 2 and 3.

[0042] Results: Comparison of the saponin content of crude saponins 1, 2, and 3 with that in the original Sapindus mukorossi powder revealed that the extraction rates of saponins from crude saponins 1, 2, and 3 were 51.97%, 57.32%, and 67.84%, respectively. This indicates that using supramolecular solvents as extraction solutions can increase the extraction rate of Sapindus mukorossi saponins.

[0043] Example 2: Screening of supramolecular solvents

[0044] In this embodiment, octanoic acid, nonanoic acid, and decanoic acid were used as amphiphiles to compare the extraction effects of supramolecular solvents formed by protic solvent ethanol and aprotic solvent acetonitrile on Sapindus mukorossi saponins.

[0045] First, the amphiphilic compound is dissolved in ethanol or acetonitrile, then water is added to form aggregates. The aggregates are then vortexed and centrifuged at 8000 r / min for 15 minutes. The supernatant is taken as the supramolecular solvent.

[0046] Then, following the steps of Example 1 above and the formulation in Table 1 below, Sapindus mukorossi saponins were extracted to obtain crude saponins 4-9 in sequence.

[0047] Table 1 Screening of supramolecular solvents

[0048]

[0049] Test results: The extraction rates of crude saponins 4-9 and the original Sapindus mukorossi powder were 67.84%, 71.32%, 65.44%, 69.96%, 61.88%, and 63.57%, respectively.

[0050] This indicates that the supramolecular solvent formed by octanoic acid as an amphiphilic and aprotic solvent, acetonitrile, provides the best extraction effect for Sapindus mukorossi saponins. However, due to the toxicity of acetonitrile, which is not conducive to industrial production, and the fact that the extraction effect of ethanol / water as a solvent is not significantly different from that of acetonitrile, octanoic acid / ethanol was ultimately selected as the superior supramolecular solvent for the extraction of Sapindus mukorossi saponins.

[0051] Example 3: Determination of supramolecular solvent

[0052] Using octanoic acid / ethanol as the extraction solvent for Sapindus mukorossi saponins, the supramolecular solvent ratio was determined according to the formulation in Table 2. Other experimental methods were the same as in Examples 1 and 2. The extraction rate test results are shown in Table 3.

[0053] Table 2 Determination of supramolecular solvents

[0054]

[0055]

[0056] Table 3 Extraction effects of different proportions of supramolecular solvents

[0057] Sample number 10 11 12 13 14 15 Extraction rate 63.12% 68.13% 66.89% 62.45% 64.78% 66.23%

[0058] A comparison of the saponin content in crude saponins 10-15 and the original Sapindus mukorossi powder revealed that the extraction effect of 70% water solvent was generally better than that of 80% water solvent. Furthermore, the extraction effect of octanoic acid in the range of 2-6% showed a trend of first increasing and then decreasing. Therefore, 4% octanoic acid-26% ethanol-70% water was finally selected as the best extraction solvent for Sapindus mukorossi saponins.

[0059] Example 4: Comparison of different methods for extracting saponins from Sapindus mukorossi

[0060] Based on Experiments 1-3 above, the extraction solvent was determined to be a supramolecular solvent of 4% n-octanoic acid - 26% ethanol - 70% water. The super-dynamic disruption technique involved extracting the enzymatically hydrolyzed extract at 10000 r / min for 30 s.

[0061] The traditional heating and stirring extraction method involves stirring the enzymatically hydrolyzed extract and heating it to 70°C, holding it at that temperature for 2 hours, and then filtering the liquid through a filter cloth. The corresponding solvent is then added to the residue, stirred, and heated to 70°C, held at that temperature for 2 hours, and the extracts are then combined.

[0062] The effect of an applied electric field of 500 V / cm on the extraction rate of Sapindus mukorossi saponins was also investigated. Other experimental methods were the same as in Examples 1 and 2. The extraction rates are shown in Table 5.

[0063] Table 4 Different extraction methods of Sapindus mukorossi saponins

[0064]

[0065]

[0066] Table 5. Extraction effects of different extraction methods

[0067] Sample number 16 17 18 19 Extraction rate 68.13% 73.11% 89.74% 93.41%

[0068] A comparison of the saponin content in crude saponins 16-19 and the original Sapindus mukorossi powder revealed that the super-dynamic crushing technology significantly increased the extraction rate of Sapindus mukorossi saponins compared with the traditional heating and stirring extraction method. Furthermore, the external electric field also had a certain promoting effect on the extraction effect. Therefore, the electric field-mediated super-dynamic crushing technology was ultimately selected as the extraction method for Sapindus mukorossi saponins.

[0069] Example 5: Optimization of the extraction method of Sapindus mukorossi saponins

[0070] (1) Sample pretreatment: Weigh 3 portions of 100g Sapindus mukorossi powder according to the method in Example 1 above, add supramolecular solvent, and after enzymatic hydrolysis, obtain extracts 20, 21 and 22.

[0071] (2) Electric field-mediated super-powered crushing and extraction: The extract was then placed in an electric field-mediated super-powered crusher and extracted for 20s, 40s and 60s under the conditions of 10000r / min and an applied electric field.

[0072] (3) Centrifugal drying: The saponin content of extracts 20, 21 and 22 was measured after centrifugation and drying according to the conditions of Examples 1-5 above.

[0073] Results: Comparison of crude saponins 20, 21 and 22 with the saponin content in the original Sapindus mukorossi powder revealed that their saponin extraction rates were 92.94%, 94.67% and 95.32%, respectively.

[0074] This indicates that the combination of electric field-mediated super-dynamic fragmentation technology and supramolecular solvent can increase the extraction rate of Sapindus mukorossi saponins, and the extraction rate increases with the increase of extraction time, but the increasing trend slows down after 40s. Therefore, 50s was finally selected as the optimal extraction time.

[0075] Example 6: Selection of Resin for Purification of Sapindus mukorossi Saponins

[0076] Four portions of crude saponin powder were weighed, dissolved in water, and the pH was adjusted to 8. AB-8, LX-100B, D101c, and LX-T28 resins were used, with 300 mL of extract for every 200 mL of resin. The extract was added to a chromatography column packed with macroporous adsorption resin. After adsorption, the resin was washed with water / 10% ethanol / 30% ethanol for 3 bv, and then isocratically eluted with 70% ethanol aqueous solution for 3 bv. The collected solution was evaporated and concentrated to obtain saponins 1, 2, 3, and 4.

[0077] Results: The purities of saponins 1, 2, 3, and 4 were found to be 55.76%, 62.74%, 72.16%, and 51.55%, respectively. This indicates that the D101c type macroporous resin is more suitable for the purification of Sapindus mukorossi saponins.

[0078] Example 7: Selection of elution method during the purification of Sapindus mukorossi saponins

[0079] Based on Example 6 above, D101c type macroporous resin was selected to purify Sapindus mukorossi saponins, and the effects of isocratic elution, gradient elution, and shaking isocratic / gradient elution on the purification method of Sapindus mukorossi saponins were investigated. Isocratic elution was performed using 3 bv of 70% ethanol aqueous solution, and gradient elution was performed using 6 bv of 35%–85% ethanol aqueous solution. The test results are shown in Table 7.

[0080] Table 6 Different elution methods

[0081] Sample number Washing method Will it fluctuate? 5 Isocratic elution no 6 Isocratic elution yes 7 Gradient elution no 8 Gradient elution yes

[0082] Table 7 Purification effects of different elution methods

[0083] Sample number 5 6 7 8 purity 62.13% 66.21% 72.16% 77.43%

[0084] Purity tests on saponins 5–8 revealed that using an elution method combining oscillation gradients significantly improved the purification effect of D101c macroporous resin on Sapindus mukorossi saponins.

[0085] Example 8: Optimization of Sapindus mukorossi saponin purification method

[0086] The gradient elution conditions of Example 7 were further optimized by dissolving the crude saponin powder in water and adjusting the pH to 7, 8, and 9; and using a D101c resin:extract ratio of 3:7, 2:3, and 1:1. The collected liquid from each column volume was analyzed by HPLC to determine the most suitable elution system.

[0087] The results showed that pH = 7-9 had little effect on the purification effect of D101c macroporous resin. When the resin:extract ratio was 2:3, the adsorption capacity was better and basically reached saturation.

[0088] Meanwhile, Sapindus saponins are mainly found in the collection solution of 75%–85% ethanol aqueous solution. Therefore, through trial and error, it was finally determined that the sample loading should be performed at pH 7–9, with a resin:extract ratio of 2:3. During desorption, a gradient elution of 60%–90% ethanol aqueous solution for 3 bv was used, which resulted in a shorter elution time. After evaporation and concentration, Sapindus saponin powder with a purity of about 80% could be obtained.

[0089] Example 9: Selection of purification method for Sapindus mukorossi saponins

[0090] To obtain Sapindus saponins with higher purity, the Sapindus saponin powder obtained above was refined using the following three methods.

[0091] n-Butanol extraction method: Dissolve 10g of Sapindus mukorossi saponin powder in 100mL of water, then add 300mL of n-butanol and stir for 30min. After standing and separating the layers, the organic phase is washed twice with 50mL of water each time. Finally, the organic phase is dried to obtain refined saponin 1.

[0092] Preparation of Sapindus mukorossi saponins by foam separation method: A conventional bubble column was used to separate the aqueous solution of Sapindus mukorossi saponins by foam separation at a gas flow rate of 3 m / s. 3 / h; The defoaming method adopts mechanical shearing and stirring, followed by drying to obtain refined saponin 2.

[0093] Preparation of Sapindus mukorossi saponins by an improved foam separation method: Based on the above foam separation method, a magnetic stirring device is added during the bubbling process, and about 1% activated carbon is added at the same time; an ultrasonic device is added during the defoaming process, and then the product is dried to obtain refined saponin 3.

[0094] Results: Compared with the n-butanol extraction method, the foam separation method yielded higher purity samples of Sapindus mukorossi saponins, reaching about 95%. Furthermore, the improved foam separation method, which incorporates pneumatic magnetic stirring and ultrasonic defoaming, reduced the purification time of Sapindus mukorossi saponins by 1 / 3 and increased the yield by 10%.

[0095] Example 10: Preparation method of Sapindus mukorossi saponins by extraction using electric field-mediated super-dynamic fragmentation technology combined with supramolecular solvent.

[0096] Based on Examples 1-9 above, Sapindus mukorossi was dried and pulverized into a 60-mesh powder. A supramolecular solvent (4% n-octanoic acid - 26% ethanol - 70% water) was added at a solid-liquid ratio of 1:20 g / mL, along with 1% cellulase. After mixing, extraction was performed for 50 seconds using electric field-mediated super-dynamic disruption technology at a rotation speed of 8800 r / min and an electric field strength of 500 V / cm. The extract was then sonicated for 20 minutes. After centrifugation, filtration, and evaporation, crude saponins were obtained, with an extraction rate reaching 95.45%.

[0097] The crude saponins were then dissolved in water, and the pH was adjusted to 7. Using D101c type resin, 300 mL of extract was applied for every 200 mL of resin. After vortexing and loading the column, the resin was washed with 20% ethanol aqueous solution for 3 bv, followed by gradient elution with 3 bv of 60% ethanol aqueous solution. The eluent was collected and dried to obtain a dry powder with a saponin content of 74.58%.

[0098] Finally, the above-mentioned Sapindus mukorossi saponin powder was dissolved in water at a ratio of 1:20 g / mL, and 1% activated carbon was added. The mixture was then transferred to a magnetic stirring and bubbling device with a nitrogen flow rate of 3 m / s. 3The process involves rotating the machine at 1400 r / min for 1 hour, then discharging the solution through the foam outlet into an ultrasonic foam collector to obtain a refined saponin aqueous solution. Finally, the solution is concentrated by evaporation to obtain Sapindus mukorossi saponin powder with a purity of 95.47%.

[0099] Example 11: Preparation method of Sapindus mukorossi saponins by extraction using electric field-mediated super-dynamic fragmentation technology combined with supramolecular solvent.

[0100] Based on Examples 1-9 above, Sapindus mukorossi was dried and pulverized into 80-mesh powder. A supramolecular solvent (5% n-octanoic acid - 25% ethanol - 70% water) was added at a solid-liquid ratio of 1:12 g / mL, along with 1.5% cellulase. After mixing, extraction was performed for 30 seconds using electric field-mediated super-dynamic disruption technology at a rotation speed of 11000 r / min and an electric field strength of 600 V / cm. The extract was then sonicated for 10 minutes. After centrifugation, filtration, and evaporation, crude saponins were obtained, with an extraction rate reaching 96.32%.

[0101] The crude saponins were then dissolved in water, and the pH was adjusted to 8. Using D101c type resin, 350 mL of extract was applied for every 250 mL of resin. After vortexing and loading the column, the resin was washed with 3bv of 30% ethanol aqueous solution, followed by gradient elution with 3bv of 90% ethanol aqueous solution. The eluent was collected and dried to obtain a dry powder with a saponin purity of 78.37%.

[0102] Finally, the above-mentioned Sapindus mukorossi saponin powder was dissolved in water at a ratio of 1:30 g / mL, and 0.8% activated carbon was added simultaneously. The mixture was then transferred to a magnetic stirring and foaming device with an air flow rate of 4 m / s. 3 The process involves rotating the machine at 1200 r / min for 1 hour, then discharging the solution through the foam outlet into an ultrasonic foam collector to obtain a refined saponin aqueous solution. Finally, the solution is concentrated by evaporation to obtain Sapindus mukorossi saponin powder with a purity of 96.82%.

[0103] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. They can be applied to various fields suitable for the present invention. For those skilled in the art, and for those of ordinary skill in the art, various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. Therefore, the present invention is not limited to the specific details without departing from the general concept defined by the claims and their equivalents.

Claims

1. A method for extracting Sapindus mukorossi saponins using a supramolecular solvent, characterized in that, Includes the following steps: (1) Dissolve the amphiphilic compound in ethanol or acetonitrile, add water to form aggregates, then vortex and centrifuge, take the upper phase to obtain the supramolecular solvent. (2) Dry the fruit and / or pericarp of Sapindus mukorossi and pulverize it into powder. Add supramolecular solvent and cellulase, mix well, extract using electric field-mediated super-powered crushing technology, then perform ultrasonic treatment, and obtain crude saponins after centrifugation, filtration, evaporation and concentration. (3) The crude saponins were adsorbed onto the column by shaking using D101c type resin; after the adsorption was completed, the resin was washed, and finally the eluent was eluted by shaking gradient with an aqueous solution of ethanol. The eluent was dried to obtain Sapindus mukorossi saponin powder. (4) Dissolve the above Sapindus mukorossi saponin dry powder in water, transfer it to a gas magnetic stirring foaming device to collect foam, and then obtain a refined saponin aqueous solution after ultrasonic defoaming. Finally, obtain Sapindus mukorossi saponin refined powder by evaporation and concentration. The electric field-mediated super-dynamic crushing technology described in step (2) is achieved by applying an electric field to the outside of a flash extractor, wherein the rotation speed of the flash extractor is 8000~12000 r / min and the time is 20 s~80 s; the magnitude of the electric field is 300~700 V / cm; the flash extractor includes a stirring motor and a stirring head; The gas magnetic stirring bubbling device of step (4) is a magnetic stirring device added in a bubbling device; air, carbon dioxide or nitrogen is introduced into the bubbling device, the flow rate is 2~5 m 3 / h, and the rotating speed is 500~2000 r / min.

2. The method according to claim 1, characterized in that, The amphiphilic compound mentioned in step (1) is octanoic acid.

3. The method according to claim 1, characterized in that, The mass percentages of each raw material mentioned in step (1) are: 2-5% amphiphilic compound, 15-30% ethanol or acetonitrile, and the remainder is water.

4. The method according to claim 1, characterized in that, In step (2), the soapberry fruit and / or pericarp are crushed into powder of 20-120 mesh.

5. The method according to claim 1, characterized in that, In step (2), the solid-liquid ratio of the powder to the supramolecular solvent is 1:10-25 g / mL, and the mass of the cellulase is 1-2% of the total mass of this step.

6. The method according to claim 1, characterized in that, In step (3), when using D101c type resin to adsorb crude saponins onto the column by shaking, first dissolve the crude saponins in water to adjust the pH to 7-9. During adsorption, each 150-250 mL of D101c type resin corresponds to 250-350 mL of extract. After shaking the column, wash the resin with water or an aqueous solution with a concentration of 10%-30% ethanol for 2-4 bv, and then use a 2-4 bv aqueous solution with a concentration of 60%-90% ethanol to elute using a shaking gradient. Collect the eluent.

7. The method according to claim 1, characterized in that, When the Sapindus mukorossi saponin powder in step (4) is dissolved in water, the ratio of material to liquid is 1:20 to 1:40, and 0.5 to 1 wt% activated carbon is added at the same time.

8. The method according to claim 1, characterized in that, Step (4) refers to the process where foam is discharged through the foam outlet to the ultrasonic foam collector for defoaming; the ultrasonic foam collector is an ultrasonic device added to the defoaming equipment.