A self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi*.

By mixing the shells of *Xanthoceras sorbifolium* with extracts or raw materials of *Xanthoceras sorbifolium*, the problem of boiling over during the concentration of *Xanthoceras sorbifolium* saponins was solved, improving the concentration efficiency and yield, making it suitable for industrial applications.

CN117562945BActive Publication Date: 2025-10-31HANDAN COLLEGE
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Patent Information

Application Number
CN202311564513.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-22
Publication Date
2025-10-31
Estimated Expiration
2043-11-22

AI Technical Summary

Technical Problem

The existing concentration process of Sapindus mukorossi saponins is prone to boiling, resulting in low yield and long concentration cycle. In addition, traditional methods require the addition of defoamers, which affects the efficacy or increases the complexity of the process.

Method used

By mixing the shell of *Xanthoceras sorbifolium* with extracts or raw materials from *Xanthoceras sorbifolium* in a certain proportion, and taking advantage of their similarity and differences in non-saponin components, a self-defoaming concentration is achieved, avoiding boiling and improving concentration efficiency.

Benefits of technology

It significantly improves the concentration efficiency of total saponins from Xanthoceras sorbifolium, reduces losses, shortens concentration time, and maintains the quality and efficacy of saponins. No additional defoamer is required, making it suitable for industrial applications.

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Abstract

This invention relates to the field of natural product extraction technology, specifically disclosing a self-defoaming extraction and concentration method for total saponins from *Xanthoceras sorbifolium*. The self-defoaming extraction and concentration method provided by this invention utilizes the homology and similarity of saponin components between *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood, as well as the differences in non-saponin components. The method involves concentrating the extracts from *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood in a specific ratio, or mixing the shells and wood in a specific ratio before extraction. This achieves self-defoaming concentration without any boiling over during the entire concentration process, significantly improving the concentration efficiency of total saponins from *Xanthoceras sorbifolium* and effectively reducing the loss of total saponins during concentration. The total saponin content of the extracted material can reach over 60%. Without adding external defoaming agents and without affecting the quality and efficacy of the saponins, the concentration time is significantly reduced, showing great promise for industrialization.
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Description

Technical Field

[0001] This invention relates to the field of natural product extraction technology, and in particular to a self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi*. Background Technology

[0002] *Xanthoceras sorbifolia* Bunge, belonging to the Sapindaceae family and the *Xanthoceras* genus, is a relatively rare woody oilseed crop in my country. The shell and wood of *Xanthoceras sorbifolia* contain various active ingredients such as triterpenoid saponins, flavonoids, and coumarins, and are commonly used in traditional Chinese medicine in many parts of my country. Since the 1980s, the analysis of the components and evaluation of the efficacy of *Xanthoceras sorbifolia* have been a research hotspot in the field of natural products. Triterpenoids are the most frequently reported components in the shell and wood of *Xanthoceras sorbifolia*, with their parent nuclei mainly being oleanane-type pentacyclic triterpenoids, especially saniculagenin C-type compounds. These compounds possess various biological activities such as improving learning and memory, anti-cancer, and anti-inflammatory effects, and may even be candidate compounds for the prevention and treatment of Alzheimer's disease.

[0003] Existing techniques for separating and purifying saponins from *Xanthoceras sorbifolium* mainly include organic solvent extraction, silica gel column chromatography, and macroporous adsorption resin methods, all of which require a concentration stage. However, saponins possess lipophilic aglycones and hydrophilic sugar groups, exhibiting surfactant-like properties. Therefore, during concentration, the saponin solution, subjected to mechanical forces, forms a large amount of persistent foam that does not disappear with heating. As concentration progresses, the foam accumulates, and especially under vacuum concentration conditions, it is prone to sudden boiling, causing a large amount of saponin to overflow from the system, significantly reducing the saponin yield. Furthermore, to avoid boiling, constant monitoring and repeated interruptions are necessary, resulting in concentration times exceeding 10 hours per liter of extract. Therefore, stable concentration of saponin solutions remains a challenging technical problem in the industry.

[0004] Currently, some literature reports the addition of cyclodextrin or fatty acid glycerides to saponin extracts to reduce foaming during concentration. However, adding cyclodextrin reduces the content of active ingredients, and adding fatty acid glycerides for defoaming requires subsequent removal of the fatty acid glycerides from the system, increasing the complexity of the process. Therefore, it is necessary to provide a novel extraction and concentration method for Sapindus mukorossi saponins to improve saponin yield and extraction efficiency. Summary of the Invention

[0005] To address the problems of easy boiling, low yield, and long concentration cycle in existing methods for extracting and concentrating saponins from *Xanthoceras sorbifolium*, this invention provides a self-defoaming extraction and concentration method for total saponins from *Xanthoceras sorbifolium*. This method primarily involves concentrating extracts from *Xanthoceras sorbifolium* shells and wood, or by extracting and concentrating a mixture of these raw materials. This effectively avoids boiling, improves extraction efficiency, reduces saponin concentration loss, and eliminates the need for external defoamers, thus preserving the quality and efficacy of the saponins. It shows great promise for industrial application.

[0006] To solve the above-mentioned technical problems, the technical solution provided by the present invention is as follows:

[0007] A self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi* includes the following steps:

[0008] The total saponins of *Sapindus mukorossi* were obtained by concentrating the mixed extract of *Sapindus mukorossi* shell and *Sapindus mukorossi* wood.

[0009] Among them, the volume ratio of *Xanthoceras sorbifolium* shell extract to *Xanthoceras sorbifolium* wood extract is ≤5:2, or the mass ratio of *Xanthoceras sorbifolium* shell to *Xanthoceras sorbifolium* wood is ≤5:2.

[0010] Under laboratory conditions, vacuum concentration of 1000 mL of non-saponin extract can generally be completed in just 0.5-1 hour without the need for supervision. However, under the same conditions, concentrating 1000 mL of saponin extract requires constant supervision due to severe boiling and overflow, and repeated interruptions are necessary to prevent further boiling, resulting in a concentration time of over 10 hours. Furthermore, as the extraction purification process progresses, the saponin content gradually increases, and the concentration difficulty increases rapidly accordingly.

[0011] To address the aforementioned problems, the present invention provides a self-defoaming extraction and concentration method for total saponins from *Xanthoceras sorbifolium*. This method utilizes the homology and similarity of saponin components between *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood, as well as the differences in non-saponin components. The extracts from *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood are combined and concentrated in a specific ratio, or the shells and wood are mixed in a specific ratio before extraction. This achieves self-defoaming concentration without any boiling issues during the entire concentration process, significantly improving the concentration efficiency of total saponins from *Xanthoceras sorbifolium* and effectively reducing the loss of total saponins during concentration. The total saponin content of the extracted material can reach over 60%. Without adding external defoaming agents and without affecting the quality and efficacy of the saponins, the concentration time is significantly reduced, demonstrating extremely high industrialization potential.

[0012] During their research and development, the inventors discovered that the total saponin content in *Xanthoceras sorbifolium* is relatively low, and its extract contains a certain amount of lipids. These lipids can act as defoamers in the *Xanthoceras sorbifolium* shell extract, exhibiting excellent defoaming effects even in the purified saponin solution after purification using macroporous adsorption resin. Furthermore, analysis has shown that the saponin components of *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood are homologous derivatives, not affecting the quality and efficacy of the total saponins. Therefore, mixing the extracts of *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood, or mixing *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood raw materials in a specific ratio, can avoid boiling over during the concentration process, facilitating the concentration of the total saponin extract and purified solution, significantly improving the production efficiency of total saponins, and eliminating the need for external defoamers or modifications to traditional saponin production lines, thus demonstrating high application potential.

[0013] As a specific embodiment of the present invention, the self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi* specifically includes the following steps:

[0014] Step a: Dry and pulverize the shell of *Xanthoceras sorbifolium*, add an alcohol-water solution, and extract to obtain *Xanthoceras sorbifolium* shell extract;

[0015] Step b: Dry and pulverize the *Xanthoceras sorbifolium* wood, add an alcohol-water solution, and extract to obtain *Xanthoceras sorbifolium* wood extract;

[0016] Step c: Mix the extracts from the shells of *Xanthoceras sorbifolium* and the extracts from *Xanthoceras sorbifolium* in a certain proportion, and concentrate under vacuum to obtain crude total saponins from *Xanthoceras sorbifolium*.

[0017] Preferably, in step a, the particle size of the crushed *Vernicia fordii* shell is 40 mesh to 200 mesh.

[0018] Preferably, in step b, the length of the crushed *Sapindus mukorossi* wood is 0.5cm to 20cm.

[0019] Preferably, in steps a and b, the alcohol-water solution is a mixed solution of short-chain alcohol and water, wherein the volume fraction of the short-chain alcohol in the alcohol-water solution is 63% to 78%.

[0020] Preferably, in steps a and b, the ratio of material to liquid is 1g:(6-13)mL.

[0021] Specifically, in steps a and b, the aqueous solution is an aqueous solution of methanol or an aqueous solution of ethanol.

[0022] Preferably, in steps a and b, the extraction temperature is 65℃~85℃, the extraction time is 1h~3h, and the number of extractions is 2~5.

[0023] The optimal extraction scheme can not only ensure the full dissolution of the active ingredients, but also improve the extraction efficiency.

[0024] Preferably, in step c, the vacuum concentration conditions are: vacuum degree 0.07MPa~0.1MPa, vacuum concentration temperature 70℃~90℃, and vacuum concentration stirring speed 45r / min~75r / min.

[0025] Specifically, in step c, the mixed extract of *Vernicia fordii* shell and *Vernicia fordii* wood is concentrated to a water content of less than 15%.

[0026] During the experiment, it was found that the method of combining and concentrating the extracts of *Vernicia fordii* shell and *Vernicia fordii* wood provided by this invention can achieve no boiling over during the entire concentration process, thus improving the safety and efficiency of the concentration process.

[0027] Preferably, step c further includes: refining the concentrated liquid through a macroporous adsorption resin to obtain total saponins from *Sapindus mukorossi*.

[0028] For example, the macroporous adsorption resin is AB-8 macroporous adsorption resin.

[0029] The total saponin extract of *Xanthoceras sorbifolium* obtained by the extraction method provided by this invention will not experience boiling even when the saponin purified by macroporous adsorption resin is concentrated, thus solving the technical problem of low efficiency and low yield of total saponins in existing *Xanthoceras sorbifolium* concentration production.

[0030] In another specific embodiment of the present invention, the self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi* specifically includes the following steps:

[0031] Step a: Dry and pulverize the *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood separately to obtain *Xanthoceras sorbifolium* shell powder and *Xanthoceras sorbifolium* wood powder.

[0032] Step b: Mix the crushed shells and crushed wood of *Sapindus mukorossi* in a certain proportion, add an alcohol-water solution, and extract to obtain total saponin extract of *Sapindus mukorossi*.

[0033] Step c: Vacuum concentrate the extract of total saponins from *Xanthoceras sorbifolium* to obtain crude total saponins from *Xanthoceras sorbifolium*.

[0034] Preferably, in step a, the particle size of the crushed *Vernicia fordii* shell is 40 mesh to 200 mesh.

[0035] Preferably, in step a, the length of the *Sapindus mukorossi* wood shreds is 0.5cm to 20cm.

[0036] Preferably, in step b, the alcohol-water solution is a mixed solution of short-chain alcohol and water, wherein the volume fraction of the short-chain alcohol in the alcohol-water solution is 63% to 78%.

[0037] Preferably, in step b, the ratio of material to liquid is 1g:(6-13)mL.

[0038] Preferably, in step b, the aqueous solution is an aqueous solution of methanol or an aqueous solution of ethanol.

[0039] Preferably, in step b, the extraction temperature is 65℃~85℃, the extraction time is 1h~3h, and the number of extractions is 2~5.

[0040] The optimal extraction scheme can not only ensure the full dissolution of the active ingredients, but also improve the extraction efficiency.

[0041] Preferably, in step c, the vacuum concentration conditions are: vacuum degree 0.07MPa~0.1MPa, vacuum concentration temperature 70℃~90℃, and vacuum concentration stirring speed 45r / min~75r / min.

[0042] Specifically, in step c, the total saponin extract of *Sapindus mukorossi* is concentrated to a water content of less than 15%.

[0043] Preferably, step c further includes: refining the concentrated liquid through a macroporous adsorption resin to obtain total saponins from *Sapindus mukorossi*.

[0044] For example, the macroporous adsorption resin is AB-8 macroporous adsorption resin.

[0045] The total saponin extract of *Xanthoceras sorbifolium* obtained by the extraction method provided by this invention will not experience boiling over when concentrated. Even when the saponin purified solution after purification by macroporous adsorption resin is concentrated, boiling over will still not occur, thus solving the technical problems of low efficiency and low yield of total saponins in existing *Xanthoceras sorbifolium* concentration production.

[0046] The extraction and concentration method for total saponins from *Xanthoceras sorbifolium* provided by this invention can avoid the problem of boiling during the concentration process of the extract, improve the concentration efficiency, and does not affect the quality and efficacy of the total saponins. It completely solves the problems of long production cycle and low production efficiency of traditional *Xanthoceras sorbifolium* total saponins, and has extremely high promotion value. Detailed Implementation

[0047] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0048] To better illustrate the present invention, further examples are provided below.

[0049] The method used to detect the total saponin content of *Cinnamomum camphora* in the following examples and comparative examples is the vanillin-perchloric acid ultraviolet colorimetric method.

[0050] Example 1

[0051] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0052] Step 1: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 40-60 mesh material, add 800mL of 70% ethanol aqueous solution, extract in a 70℃ water bath for 1h, filter through a 300 mesh filter cloth, separate the residue and filtrate, repeat the extraction 3 times, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0053] Step 2: Crush the *Xanthoceras sorbifolium* wood, sieve it, take 100g of material with a thickness of 0.5-5cm, add 800mL of 70% ethanol aqueous solution, and extract in a 70℃ water bath for 1h. Pass it through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction 3 times, combine the filtrates, and obtain *Xanthoceras sorbifolium* wood extract.

[0054] Step 3: Take 500mL of *Xanthoceras sorbifolium* shell extract and 200mL of *Xanthoceras sorbifolium* wood extract, combine them, add the combined extract to a rotary flask, and concentrate it under a vacuum of 0.1MPa at 90℃ in a water bath with a stirring speed of 75r / min until there is no alcohol smell. There should be no bumping during the concentration process. The concentration time is 23min.

[0055] Step 4: The above concentrated solution was purified by AB-8 macroporous adsorption resin, eluted with 70% ethanol aqueous solution, and then concentrated and dried. The concentration was carried out under a vacuum of 0.1 MPa, in a water bath at 90°C, and with a stirring speed of 75 r / min until there was no alcohol odor and no bumping. The total saponin content was found to be 68%.

[0056] Example 2

[0057] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0058] Step 1: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 50-80 mesh material, add 1000mL of 65% ethanol aqueous solution, and extract in a 65℃ water bath for 1.5h. Pass it through a 300 mesh filter cloth to separate the residue and filtrate. Repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0059] Step 2: Crush the *Xanthoceras sorbifolium* wood, sieve it, take 100g of material with a thickness of 16-20cm, add 1000mL of 65% ethanol aqueous solution, and extract in a 65℃ water bath for 1.5h. Pass it through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* wood extract.

[0060] Step 3: Take 1000mL of *Xanthoceras sorbifolium* shell extract and 500mL of *Xanthoceras sorbifolium* wood extract, combine them, add the combined extract to a rotary flask, and concentrate it at 85℃ in a water bath under a vacuum of 0.07MPa and a stirring speed of 67r / min until there is no alcohol smell. There is no bumping during the concentration process. The total concentration time is 52min.

[0061] Step 4: The above concentrate was purified by AB-8 macroporous adsorption resin, eluted with 75% ethanol aqueous solution, and then concentrated and dried. The concentration was carried out under a vacuum of 0.07 MPa, in a water bath at 85°C, and with a stirring speed of 67 r / min until there was no alcohol odor and no bumping. The total saponin content was found to be 69%.

[0062] Example 3

[0063] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0064] Step 1: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 60-100 mesh material, add 600mL of 70% ethanol aqueous solution, extract in a 75℃ water bath for 1h, filter through a 300 mesh filter cloth, separate the residue and filtrate, repeat the extraction 3 times, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0065] Step 2: Crush the *Xanthoceras sorbifolium* wood, sieve it, take 100g of material with a thickness of 10-20cm, add 600mL of 70% ethanol aqueous solution, and extract in a 75℃ water bath for 1h. Pass it through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction 3 times, combine the filtrates, and obtain *Xanthoceras sorbifolium* wood extract.

[0066] Step 3: Take 600mL of *Xanthoceras sorbifolium* shell extract and 400mL of *Xanthoceras sorbifolium* wood extract, combine them, add the combined extract to a rotary flask, and concentrate under a vacuum of 0.08MPa at 90℃ in a water bath with a stirring speed of 63r / min until there is no alcohol odor. There should be no bumping during the concentration process. The concentration time is 34min.

[0067] Example 4

[0068] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0069] Step 1: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 100-200 mesh material, add 1300mL of 73% ethanol aqueous solution, extract in an 85℃ water bath for 1h, filter through a 300 mesh filter cloth, separate the residue and filtrate, repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0070] Step 2: Crush the *Xanthoceras sorbifolium* wood, sieve it, take 100g of material with a thickness of 5-15cm, add 1300mL of 73% ethanol aqueous solution, extract in an 85℃ water bath for 1h, filter through a 300-mesh filter cloth, separate the residue and filtrate, repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* wood extract.

[0071] Step 3: Take 500mL of *Xanthoceras sorbifolium* shell extract and 500mL of *Xanthoceras sorbifolium* wood extract, combine them, add the combined extract to a rotary flask, and concentrate it under a vacuum of 0.09MPa at 70℃ in a water bath with a stirring speed of 55r / min until there is no alcohol smell. There should be no bumping during the concentration process. The concentration time is 35min.

[0072] Step 4: The above concentrate was purified by AB-8 macroporous adsorption resin, eluted with 75% ethanol aqueous solution, and then concentrated and dried. The concentration was carried out under a vacuum of 0.09 MPa, in a water bath at 70°C, and with a stirring speed of 55 r / min until there was no alcohol odor and no bumping. The total saponin content was found to be 63%.

[0073] Example 5

[0074] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0075] Step a: Crush the shell of *Xanthoceras sorbifolium*, sieve it, and take 50g of 100-200 mesh material; crush the *Xanthoceras sorbifolium* wood, sieve it, and take 50g of 0.5-10cm material. Mix them evenly, add 1300mL of 63% ethanol aqueous solution, and extract in a water bath at 85℃ for 1h. Filter through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction twice, combine the filtrates, and obtain the total saponin extract of *Xanthoceras sorbifolium*.

[0076] Step b: Add the total saponin extract of Xanthoceras sorbifolium obtained above into a rotary flask, and concentrate it under vacuum of 0.09 MPa, water bath temperature of 77℃ and stirring speed of 45 r / min until there is no alcohol odor and no bumping phenomenon. The total concentration time is 73 min.

[0077] Step c: The above concentrate was purified by AB-8 macroporous adsorption resin, eluted with 75% ethanol aqueous solution, concentrated and dried. The concentration was carried out under a vacuum of 0.09 MPa, in a water bath at 77°C, and with a stirring speed of 45 r / min until there was no alcohol odor and no bumping. The total saponin content was found to be 64%.

[0078] Example 6

[0079] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0080] Step a: Crush the shell of *Xanthoceras sorbifolium*, sieve it, and take 30g of 60-100 mesh material; crush the *Xanthoceras sorbifolium* wood, sieve it, and take 20g of 5-20cm material. Mix them evenly, add 300mL of 78% methanol aqueous solution, and extract in a water bath at 75℃ for 1h. Filter through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction 3 times, combine the filtrates, and obtain the total saponin extract of *Xanthoceras sorbifolium*.

[0081] Step b: Add the total saponin extract of Xanthoceras sorbifolium obtained above into a rotary flask, and concentrate it under vacuum of 0.08 MPa, water bath temperature of 90℃, and stirring speed of 56 r / min until there is no alcohol odor and no bumping phenomenon. The concentration time is 26 min.

[0082] Example 7

[0083] This embodiment provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, comprising the following steps:

[0084] Step a: Crush the shell of *Xanthoceras sorbifolium*, sieve it, and take 10g of 40-200 mesh material; crush the *Xanthoceras sorbifolium* wood, sieve it, and take 100g of 0.5-20cm material. Mix them evenly, add 1000mL of 67% ethanol aqueous solution, and extract in a water bath at 65℃ for 1.5h. Filter through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction 3 times, combine the filtrates, and obtain the total saponin extract of *Xanthoceras sorbifolium*.

[0085] Step b: Add the total saponin extract of Xanthoceras sorbifolium obtained above into a rotary flask, and concentrate it under vacuum of 0.07 MPa, water bath temperature of 83℃ and stirring speed of 53 r / min until there is no alcohol odor and no bumping phenomenon. The total concentration time is 82 min.

[0086] Step c: The above concentrate was purified by AB-8 macroporous adsorption resin, eluted with 75% ethanol aqueous solution, concentrated and dried. The concentration was carried out under a vacuum of 0.07 MPa, in a water bath at 83°C, and with a stirring speed of 53 r / min until there was no alcohol odor and no bumping. The total saponin content was found to be 61%.

[0087] Comparative Example 1

[0088] This comparative example provides a method for extracting and concentrating total saponins from *Sapindus mukorossi*, comprising the following steps:

[0089] Step a: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 50-80 mesh material, add 1000mL of 65% ethanol aqueous solution, extract in a 65℃ water bath for 1.5h, filter through a 300 mesh filter cloth, separate the residue and filtrate, repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0090] Step b: Add 1000 mL of Xanthoceras sorbifolium shell extract to a rotary flask, and concentrate it at 85°C in a water bath under a vacuum of 0.07 MPa and a stirring speed of 67 r / min until there is no alcohol smell. During the concentration process, there is severe boiling, and the pressure is released once every 3-8 minutes on average. The concentration time is more than 15 hours.

[0091] Comparative Example 2

[0092] This comparative example provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, which differs from Example 2 only in the volume ratio of *Xanthoceras sorbifolium* shell extract to *Xanthoceras sorbifolium* wood extract. The specific steps include:

[0093] Step 1: Crush the shell of *Xanthoceras sorbifolium*, sieve it, take 100g of 50-80 mesh material, add 1000mL of 65% ethanol aqueous solution, and extract in a 65℃ water bath for 1.5h. Pass it through a 300 mesh filter cloth to separate the residue and filtrate. Repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* shell extract.

[0094] Step 2: Crush the *Xanthoceras sorbifolium* wood, sieve it, take 100g of material with a thickness of 16-20cm, add 1000mL of 65% ethanol aqueous solution, and extract in a 65℃ water bath for 1.5h. Pass it through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction twice, combine the filtrates, and obtain *Xanthoceras sorbifolium* wood extract.

[0095] Step 3: Take 1000mL of *Xanthoceras sorbifolium* shell extract and 350mL of *Xanthoceras sorbifolium* wood extract, combine them, add the combined extract to a rotary flask, and concentrate under vacuum of 0.07MPa at 85℃ in a water bath with a stirring speed of 67r / min until there is no alcohol smell. During the concentration process, there is severe boiling, and the gas is released and pressure is relieved every 3-8 minutes on average. The concentration time is more than 13 hours.

[0096] Comparative Example 3

[0097] This comparative example provides a method for extracting and concentrating total saponins from *Xanthoceras sorbifolium*, which differs from Example 6 only in the mass ratio of *Xanthoceras sorbifolium* shell to *Xanthoceras sorbifolium* wood. The specific steps include:

[0098] Step a: Crush the shell of *Xanthoceras sorbifolium*, sieve it, and take 60g of 60-100 mesh material; crush the *Xanthoceras sorbifolium* wood, sieve it, and take 20g of 5-20cm material. Mix them evenly, add 480mL of 78% ethanol aqueous solution, and extract in a water bath at 75℃ for 1h. Filter through a 300-mesh filter cloth to separate the residue and filtrate. Repeat the extraction 3 times, combine the filtrates, and obtain the total saponin extract of *Xanthoceras sorbifolium*.

[0099] Step b: Add 1000 mL of total saponin extract from *Sapindus mukorossi* to a rotary flask and concentrate it under vacuum of 0.08 MPa, water bath temperature of 90℃, and stirring speed of 56 r / min until there is no alcohol odor and no bumping. The concentration time is more than 10 hours.

[0100] In summary, the method of extracting total saponins from *Xanthoceras sorbifolium* by mixing its shell extract and wood extract in a certain proportion, or by mixing the shell and wood in a certain proportion, can effectively avoid the problem of boiling over during subsequent vacuum concentration, significantly improve the concentration efficiency of total saponins from *Xanthoceras sorbifolium*, and does not require the addition of external defoaming agents or changes to the traditional extraction process and equipment for total saponins from *Xanthoceras sorbifolium*. This method is more suitable for industrial production applications and has extremely high practical value.

[0101] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions or improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi*, characterized in that, Includes the following steps: Step a: Dry and pulverize the shell of *Xanthoceras sorbifolium*, add an alcohol-water solution, and extract to obtain *Xanthoceras sorbifolium* shell extract; Step b: Dry and pulverize the *Xanthoceras sorbifolium* wood, add an alcohol-water solution, and extract to obtain *Xanthoceras sorbifolium* wood extract; Step c: Mix the extract of *Xanthoceras sorbifolium* shell and extract of *Xanthoceras sorbifolium* in a certain proportion, concentrate under vacuum, and refine the concentrate through macroporous adsorption resin to obtain total saponins of *Xanthoceras sorbifolium*. In step a, the particle size of the crushed *Vernicia fordii* shell is 40-200 mesh; the length of the crushed *Vernicia fordii* wood is 0.5-20 cm; and the volume ratio of *Vernicia fordii* shell extract to *Vernicia fordii* wood extract is ≤5:

2. In steps a and b, the alcohol-water solution is a methanol-water solution or an ethanol-water solution, wherein the volume fraction of alcohol in the alcohol-water solution is 63%~78%; in steps a and b, the material-to-liquid ratio is 1g:(6~13)mL; in steps a and b, the extraction temperature is 65℃~85℃, the extraction time is 1h~3h, and the extraction is performed 2~5 times. In step c, the conditions for vacuum concentration are: vacuum degree 0.07MPa~0.1MPa, vacuum concentration temperature 70℃~90℃, and vacuum concentration stirring speed 45r / min~75r / min.

2. A self-defoaming extraction and concentration method for total saponins from *Sapindus mukorossi*, characterized in that, Specifically, the steps include the following: Step a: Dry and pulverize the *Xanthoceras sorbifolium* shell and *Xanthoceras sorbifolium* wood separately to obtain *Xanthoceras sorbifolium* shell powder and *Xanthoceras sorbifolium* wood powder. Step b: Mix the crushed shells and crushed wood of *Sapindus mukorossi* in a certain proportion, add an alcohol-water solution, and extract to obtain total saponin extract of *Sapindus mukorossi*. Step c: Vacuum concentrate the extract of total saponins from *Xanthoceras sorbifolium*, and then refine the concentrate through a macroporous adsorption resin to obtain total saponins from *Xanthoceras sorbifolium*. In step a, the mass ratio of *Vernicia fordii* shell to *Vernicia fordii* wood is ≤5:2; the particle size of the crushed *Vernicia fordii* shell is 40 mesh to 200 mesh; and the length of the crushed *Vernicia fordii* wood is 0.5 cm to 20 cm. In step b, the alcohol-water solution is a methanol-water solution or an ethanol-water solution, wherein the volume fraction of alcohol in the alcohol-water solution is 63%~78%; the material-to-liquid ratio for extraction is 1g:(6~13)mL; the extraction temperature is 65℃~85℃, the extraction time is 1h~3h, and the number of extractions is 2~5 times. In step c, the conditions for vacuum concentration are: vacuum degree 0.07MPa~0.1MPa, vacuum concentration temperature 70℃~90℃, and vacuum concentration stirring speed 45r / min~75r / min.

Citation Information

Patent Citations

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