Preparation method and application of water-soluble paris extract

Abstract

This invention discloses a method for preparing and applying a water-soluble Paris polyphylla extract. The preparation method includes the following steps: alcohol extraction of Paris polyphylla raw material; dissolving the obtained Paris polyphylla extract, cyclodextrin, and chelating agent in pure water until homogeneous; subjecting the resulting system to inclusion under stirring to obtain an inclusion solution; ultrafiltration of the inclusion solution; adding cellulose to the ultrafiltrate; stirring to dissolve; filtering again; and spray drying to obtain the water-soluble Paris polyphylla extract. This invention uses cyclodextrin to form a "water-soluble inclusion complex" from the alcohol-extracted Paris polyphylla extract. Further addition of cellulose to adjust the mixture results in a white powdery water-soluble Paris polyphylla extract with a high inclusion rate and excellent water solubility. The water-soluble Paris polyphylla extract prepared by this invention solves the water solubility problem of the active ingredient Paris saponins, and can be widely used in cosmetics, possessing a very broad market prospect.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to a method for preparing and applying a water-soluble Paris polyphylla extract. Background Technology

[0002] Paris polyphylla is a plant belonging to the Liliaceae family, specifically Paris yunnanensis. Paris polyphylla Smith var. yunnanensis (Franch.) Hand. -Mazz. or Paris polyphylla Paris polyphylla The dried rhizome of *Smith var. chinensis* (Franch.) Hara is bitter in taste and slightly cold in nature. It enters the liver meridian and has the effects of clearing heat and detoxifying, reducing swelling and relieving pain, and cooling the liver and calming the nerves. As a traditional Chinese medicinal plant, the medicinal value of *Paris polyphylla* has been recorded in classics such as *Compendium of Materia Medica* and *Yunnan Materia Medica*. Modern pharmacological research has further confirmed that its active ingredients have significant potential for cosmetic applications, providing a high-quality natural raw material for the research and development of functional cosmetics.

[0003] The main active ingredients of Paris polyphylla are saponins (including saponins I, II, VI, and VII), flavonoids, polysaccharides, amino acids, and trace elements, among which saponins are the key substances for exerting the core efficacy. Paris saponins belong to the steroidal saponin class of compounds and have anti-inflammatory and soothing effects on the skin, making them suitable for sensitive skin care products. Although Paris saponins possess excellent cosmetic efficacy potential, they are almost insoluble in water, resulting in poor solubility in water-based cosmetic formulations, easy precipitation, and affecting the uniformity of product texture. Paris saponins are also susceptible to light, heat, and oxygen, leading to oxidative decomposition and reducing the stability of product efficacy.

[0004] Existing technologies have provided various methods for alcohol extraction of Paris polyphylla saponins, including those described in patent documents CN118490600A and CN117338681A. Although the above methods have achieved efficient extraction of Paris polyphylla saponins, the obtained Paris polyphylla saponins are all alcohol-soluble, and the problems of water solubility and water stability of Paris polyphylla saponins have not been solved.

[0005] Based on the aforementioned technical bottlenecks and the urgent need for water-soluble formulations in the cosmetics industry, there is a pressing need to develop a highly soluble and stable water-soluble system for Paris polyphylla saponins. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the purpose of this invention is to provide a method for preparing water-soluble Paris polyphylla extract and its application.

[0007] The objective of this invention is achieved through the following technical solution: In a first aspect, the present invention provides a method for preparing a water-soluble Paris polyphylla extract, comprising the following steps: A. After crushing the raw material of Paris polyphylla, it is extracted with alcohol. The resulting extract is concentrated under reduced pressure for the first time and decolorized, and then concentrated under reduced pressure for the second time. The alcohol-free concentrate is dried to obtain Paris polyphylla extract. B. After dissolving the Paris polyphylla extract, cyclodextrin, and chelating agent in pure water until homogeneous, the resulting system is incorporated under stirring conditions to obtain an incorporation solution. C. The inclusion solution was subjected to ultrafiltration, and cellulose was added to the ultrafiltrate. After stirring and dissolving, the solution was filtered and spray-dried to obtain water-soluble Paris polyphylla extract. The ingredients, cyclodextrin, chelating agent and cellulose are, by weight, 4-30 parts, 50-86 parts, 1-3 parts and 6-26 parts, respectively. The mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-80.

[0008] As a preferred embodiment, the mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-40.

[0009] As a preferred embodiment, in step B, the cyclodextrin includes at least one of hydroxypropyl-β-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, and α-cyclodextrin.

[0010] As a preferred embodiment, in step B, the chelating agent is EDTA-2Na. In this invention, the added chelating agent functions to chelate metal ions and inhibit oxidation. If the amount of EDTA disodium added is too low, too many unchelated metal ions will remain in the system, interfering with its stability. Conversely, the content of EDTA disodium should generally not be too high, as unchelated EDTA disodium is easily absorbed transdermally, irritating the skin. The amount of chelating agent used in this invention is the optimal safe concentration that maintains system stability.

[0011] As a preferred embodiment, in step B, the solids content of the system is 14-18%. The solids content is adjusted by adding water.

[0012] As a preferred embodiment, in step B, the inclusion process involves stirring at a speed of 2000–10000 r / min and in a constant-temperature water bath at 50–60°C for 1.5–2.5 h. The solid content refers to the total mass percentage of the Paris polyphylla extract and cyclodextrin in the system. If the stirring speed used for inclusion is below 2000 r / min, the water solubility stability of the inclusion complex will be significantly reduced. However, when the stirring speed is within the range of 2000–10000 r / min, the prepared inclusion complex exhibits good water solubility stability.

[0013] As a preferred embodiment, in step C, the cellulose is selected from at least one of hydroxypropyl methylcellulose (HPMC), hydroxyethyl cellulose (HEC), and hydroxypropyl carboxymethyl cellulose (HPCMC).

[0014] As a further preferred option, the cellulose is hydroxypropyl methylcellulose.

[0015] As a preferred embodiment, the cellulose is 10 to 18 parts by weight; more preferably 12 to 15 parts by weight.

[0016] As a preferred embodiment, in step C, the ultrafiltration uses an ultrafiltration membrane with a molecular weight cutoff of 20–100 kDa (operating pressure 0.1–0.2 MPa, temperature 30–35°C). Ultrafiltration can remove unencapsulated macromolecular impurities (such as residual polysaccharides and resin fragments), and the removal rate of macromolecular impurities in the collected ultrafiltrate is ≥95%, which can reduce the risk of skin irritation.

[0017] As a preferred embodiment, in step C, the filtration uses a 0.1–0.22 μm nylon membrane.

[0018] As a preferred embodiment, in step A, the solvent used for the alcohol extraction is at least one of ethanol and methanol; reflux extraction is performed 2 to 4 times, with each extraction lasting 1 to 2 hours.

[0019] As a preferred embodiment, in step A, the decolorization uses at least one of LX-94 anion exchange resin, acidic alumina, and activated carbon. More preferably, the decolorization uses LX-94 anion exchange resin.

[0020] As a preferred option, in step C, the water content of the obtained water-soluble Paris polyphylla extract is ≤5%, which facilitates the storage of cosmetic raw materials.

[0021] Secondly, the present invention provides a water-soluble Paris polyphylla extract prepared according to the aforementioned method, wherein the water-soluble Paris polyphylla extract comprises Paris polyphylla extract, cyclodextrin, chelating agent and cellulose.

[0022] Thirdly, the present invention provides an application of water-soluble Paris polyphylla extract in the preparation of cosmetics.

[0023] Compared with the prior art, the present invention has the following beneficial effects: 1) In this invention, the Paris polyphylla extract prepared by alcohol extraction is encapsulated with cyclodextrin to form a "water-soluble inclusion complex". After further adding cellulose, the resulting white powdery water-soluble Paris polyphylla extract has a high inclusion rate and very good water solubility (the aqueous solution prepared by dissolving in water is clear and transparent).

[0024] 2) By further optimizing the addition ratio of cyclodextrin, the type and addition ratio of cellulose, this invention can further improve the total saponin content of Paris polyphylla extract (reaching over 0.95%) and inclusion rate (reaching over 90%), exhibiting excellent water solubility stability (the aqueous solution prepared by dissolving in water remains clear and transparent after 3 months) and compatibility (the mixed solution prepared by dissolving in water and other solvents remains clear and transparent after 3 months, with no precipitation). Furthermore, the prepared water-soluble Paris polyphylla extract has been verified to have excellent soothing effects such as reducing redness and relieving skin discomfort.

[0025] 3) The water-soluble Paris polyphylla extract prepared by this invention solves the water solubility problem of its active ingredient, Paris saponin, and can be widely used in cosmetics, with a very broad market prospect. Attached Figure Description

[0026] Other features, objects, and advantages of the present invention will become more apparent from the following detailed description of non-limiting embodiments with reference to the accompanying drawings: Figure 1 Photographs of the state of the dissolution system for the water-saturated dissolution of the Paris polyphylla extract obtained in Example 3; Figure 2 The results of HPLC analysis were obtained after filtering the water-saturated dissolution system of the Paris polyphylla extract obtained in Example 3. Figure 3 A photograph of step 1 of Example 7, which involves mixing to form an encapsulation mixture; Figure 4 Comparative photographs of the inclusion solution (left glass) obtained in step 1 of Example 7 and the ultrafiltrate (right glass bottle) obtained in step 2; Figure 5 The results of HPLC analysis of the ultrafiltrate obtained in step 2 of Example 7; Figure 6 This is a flowchart illustrating the preparation process of the water-soluble Paris polyphylla extract of the present invention. Figure 7 These are photographs of the sample solutions from Examples 4-17 in the stability study after three months of storage. Figure 8 Photographs of the sample solutions of Examples 18 (left) and 19 (right) on the second day after preparation in the stability study; Figure 9 Photographs of sample solutions from Examples 4-17 after three months of storage during compatibility testing (with 0.5% GPL and 4% glycerol added); Figure 10 Photographs of sample solutions from Examples 4-17 after three months of storage (with 0.5% GPL and 4% ethanol added) during compatibility testing; Figure 11Photographs of sample solutions from Examples 4-17 (with 0.5% GPL and 4% 1,3-propanediol added) after three months of storage for compatibility testing; Figure 12 The results of clinical redness reduction tests were conducted on test samples Y7, Y8, Y9, Y10, and Y11; Figure 13 The results of lactic acid stinging test were performed on test samples Y7, Y8, Y9, Y10, and Y11. Detailed Implementation

[0027] The present invention will now be described in detail with reference to specific embodiments. These embodiments will help those skilled in the art to further understand the present invention, but do not limit the invention in any way. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention. These all fall within the scope of protection of the present invention.

[0028] In a specific embodiment of the present invention, a method for preparing a water-soluble Paris polyphylla extract is provided, comprising the following steps: (1) pulverizing Paris polyphylla raw material and then extracting it with alcohol, and then performing a first vacuum concentration and decolorization of the resulting extract, followed by a second vacuum concentration, and drying the resulting alcohol-free concentrate to obtain Paris polyphylla extract; (2) Weigh out each component by weight as follows: 4-30 parts of Paris polyphylla extract, 50-86 parts of cyclodextrin, 1-3 parts of chelating agent and 6-26 parts of cellulose. (3) After weighing the Paris polyphylla extract, cyclodextrin and chelating agent and dissolving them evenly in pure water, the resulting system with a solid content of 14-18% is subjected to inclusion in a constant temperature water bath at 50-60 ℃ for 1.5-2.5 h at a stirring speed of 2000-10000 r / min to obtain the inclusion solution. (4) The inclusion solution is ultrafiltered, and the weighed cellulose is added to the ultrafiltrate. After stirring and dissolving, the solution is filtered and spray-dried to obtain water-soluble Paris polyphylla extract.

[0029] In one specific embodiment, the total saponin content of Paris polyphylla extract obtained in step (1) is more than 20%. In step (2), the weight parts of Paris polyphylla extract are preferably 4.4 to 28.2 parts, more preferably 4.4 to 10.5 parts, and most preferably 10.5 parts.

[0030] In one specific embodiment, the cyclodextrin includes at least one selected from hydroxypropyl-β-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, and α-cyclodextrin. Previous experiments have shown that the inclusion effect of different types of cyclodextrin is comparable, and these are not listed individually in the embodiments of this invention. The preferred weight percentage of the cyclodextrin is 56.3–80.1 parts, more preferably 74–80.1 parts, and most preferably 74 parts.

[0031] In one specific embodiment, the mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-80. This ratio significantly improves the inclusion rate. More preferably, the mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-40, resulting in a water-soluble Paris polyphylla extract with a total saponin content of 1.8% or higher. Most preferably, the mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-35, resulting in the highest total saponin content in the water-soluble Paris polyphylla extract, reaching 2% or higher, exhibiting the best redness-reducing effect and lactic acid sting-reducing effect.

[0032] In one specific embodiment, the chelating agent is EDTA-2Na.

[0033] In one specific embodiment, the cellulose is selected from at least one of hydroxypropyl methylcellulose (HPMC), hydroxyethyl cellulose (HEC), and hydroxypropyl carboxymethyl cellulose (HPCMC). More preferably, hydroxypropyl methylcellulose is used, as the water-soluble Paris polyphylla extract prepared using it exhibits the best water solubility stability and compatibility.

[0034] In one specific embodiment, the weight parts of hydroxypropyl methylcellulose are preferably 10 to 18 parts. More preferably, they are 12 to 15 parts, as this content improves the water solubility stability and compatibility of the prepared water-soluble Paris polyphylla extract. Most preferably, the weight parts of hydroxypropyl methylcellulose are 13.5 parts, resulting in the best water solubility stability and compatibility of the prepared water-soluble Paris polyphylla extract.

[0035] In step (4) above, this application uses a 100KD ultrafiltration membrane to treat the inclusion solution, the purpose of which is to remove unincluded, water-insoluble saponin precipitates from the system. Since the saponin compounds in Paris polyphylla extract have extremely poor water solubility and are easily precipitated in aqueous solvents, and the particle size of the precipitate is usually much larger than the filtration pore size corresponding to the 100KD ultrafiltration membrane, step (4) uses a 100KD ultrafiltration membrane to remove saponin precipitates.

[0036] In this invention, all the Chinese herbal raw materials and reagents used in the experiments were provided by our company and / or purchased from the market.

[0037] The method for detecting the total saponin content of Paris polyphylla used in the embodiments of the present invention refers to the "Technical Guidelines for Testing and Evaluation of Physicochemical and Hygienic Indicators of Health Food (2020 Edition)" - Total Saponin Determination.

[0038] It should be noted that existing literature uses the ratio of total saponins before and after inclusion to represent the inclusion effect of saponin compounds. For example, the inclusion rate defined in Literature 1 is the ratio of the content of ginsenosides in the inclusion compound to the content of ginsenosides before inclusion. Literature 2 defines the inclusion rate as (content of ginsenoside Rg3 measured in the inclusion compound) / (amount of ginsenoside Rg3 added before inclusion) × 100%. Both literatures used spectrophotometry and liquid chromatography to determine the total saponins in the inclusion compound solution, respectively, as the content of saponins measured in the inclusion compound, without considering the content of trace amounts of dissolved free saponins.

[0039] Reference 1: Qin Feng, Chen Yuyong, Zhu Shanyuan, Huang Wenqiang. Preparation process of β-cyclodextrin inclusion complex of total saponins of Panax notoginseng [J]. Hubei Agricultural Sciences, 2013, 52(22):5564-5566; Reference 2: Zhang Naixian, Ai Li, Dong Yingjie, Sun Xiaojuan, Li Xiaoyi, Zou Xiaofeng. Preparation and characterization of ginsenoside Rg3 hydroxypropyl-β-cyclodextrin inclusion complex [J]. Journal of Shenyang Pharmaceutical University, 2017, 34(12):1033-1037 Considering that Paris polyphylla saponins are almost insoluble in water, the free form of Paris polyphylla saponins dissolved in the inclusion solution has a very small impact on the final inclusion effect. Therefore, the method described in the literature is adopted. When detecting the content, the separation of free saponins is not considered. The inclusion rate is defined directly by the mass ratio of total saponins before and after inclusion.

[0040] The method for calculating the inclusion rate of total saponins from Paris polyphylla according to the present invention is as follows: Inclusion rate = (mass of total saponins from Paris polyphylla in the inclusion complex) / (mass of total saponins from Paris polyphylla before inclusion) × 100%; wherein, the mass of total saponins from Paris polyphylla in the inclusion complex is calculated as: mass of water-soluble Paris polyphylla extract × content of total saponins from Paris polyphylla extract, and considering the operability of the detection, the mass of water-soluble Paris polyphylla extract obtained by spray drying is used for calculation; the mass of total saponins from Paris polyphylla before inclusion is calculated as: amount of Paris polyphylla extract added × content of total saponins from Paris polyphylla extract.

[0041] The raw material used in the embodiments of the present invention is the commercially available Chinese medicinal herb, Yunnan Paris polyphylla (Paris polyphylla var. yunnanensis). Paris polyphylla Smith var. yunnanensis (Franch.) Hand.-MazzThe total saponin content of Paris polyphylla was 2.9%. The CAS number of the hydroxypropyl-β-cyclodextrin used was 128446-33-3; the CAS number of EDTA-2Na was 6381-92-6; hydroxypropyl methylcellulose, hydroxyethyl cellulose, and hydroxypropyl carboxymethyl cellulose were all purchased from Sigma-Aldrich.

[0042] Example 1 This embodiment provides a method for preparing Paris polyphylla extract, the specific steps of which are as follows: 1. Take 100 g of Paris polyphylla raw material, crush it through a 20-mesh sieve to obtain Paris polyphylla powder. First extraction: add 8 Bv of 90% ethanol and reflux for 1.5 h; second extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; third extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; combine the three extracts, cool the extract and pass it through a 0.8 μm polypropylene membrane to obtain the total extract; 2. The total extract was concentrated under reduced pressure at 50–70 °C and -0.08–-0.09 MPa, and ethanol was recovered until the ethanol concentration of the concentrate was 80%. The volume of the concentrate was 400 mL, and the primary concentrate was obtained. 3. Pass the primary concentrate into 35 g of acid- and alkali-treated LX-94 anion exchange resin at a flow rate of 1–2 Bv / h, then wash with 1 Bv of 80% ethanol, and collect the decolorizing solution and the wash solution. 4. The decolorized solution was concentrated and dried under reduced pressure at 50-70 ℃ and -0.08--0.09 MPa to obtain 9.5 g of Paris polyphylla extract with a total saponin content of 22.7%.

[0043] Example 2 This embodiment provides a method for preparing Paris polyphylla extract, the specific steps of which are as follows: 1. Take 100 g of Paris polyphylla raw material, crush it through a 20-mesh sieve to obtain Paris polyphylla powder. First extraction: add 8 Bv of 90% ethanol and reflux for 1.5 h; second extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; third extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; combine the three extracts, cool the extract and pass it through a 0.8 μm polypropylene membrane to obtain the total extract; 2. The total extract was concentrated under reduced pressure at 50–70 °C and -0.08–-0.09 MPa, and ethanol was recovered until the ethanol concentration of the concentrate was 80%. The volume of the concentrate was 400 mL, and the primary concentrate was obtained. 3. Pass the primary concentrate into 25 g of acidic alumina at a flow rate of 1-2 Bv / h, then wash with 1 Bv of 80% ethanol, and collect the decolorizing solution and the washing solution. 4. The decolorized solution was concentrated and dried under reduced pressure at 50-70℃ and -0.08--0.09 MPa to obtain 8.5g of Paris polyphylla extract with a total saponin content of 23.1%.

[0044] Example 3 This embodiment provides a method for preparing Paris polyphylla extract, the specific steps of which are as follows: 1. Take 100 g of Paris polyphylla raw material, crush it through a 20-mesh sieve to obtain Paris polyphylla powder. First extraction: add 8 Bv of 90% ethanol and reflux for 1.5 h; second extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; third extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; combine the three extracts, cool the extract and pass it through a 0.8 μm polypropylene membrane to obtain the total extract; 2. The total extract was concentrated under reduced pressure at 50–70℃ and -0.08–-0.09 MPa, and ethanol was recovered until the ethanol concentration of the concentrate was 80%. The volume of the concentrate was 400 mL, and the primary concentrate was obtained. 3. Add 2.0 g of 300-mesh wood-based decolorizing activated carbon to the primary concentrate, stir at 60 ℃ for 1.0 h, and then filter through a 0.8 μm nylon membrane to obtain the decolorized solution; 4. The decolorized solution was concentrated and dried under reduced pressure at 50-70℃ and -0.08--0.09MPa to obtain 8.6 g of Paris polyphylla extract with a total saponin content of 20.5%.

[0045] A comparison of the results from Examples 1-3 shows that, when extracting 100g of Paris polyphylla raw material, the decolorization effect using wood-based activated carbon was poor, resulting in the lowest total amount of total saponins (1.76 g); the decolorization using acidic alumina resulted in significant losses, leading to the lowest total amount of Paris polyphylla extract; while the decolorization using LX-94 anion exchange resin was the most effective, yielding the highest total amount of Paris polyphylla extract and the highest total amount of total saponins (2.16 g).

[0046] The Paris polyphylla extract obtained in Example 3 was dissolved in water to achieve a water saturation state, as shown in the figure. Figure 1 As shown, after thorough stirring, the water-saturated solution system of the Paris polyphylla extract remained turbid and contained a large amount of precipitate, indicating that the Paris polyphylla extract obtained in Example 3 is poorly soluble in water. The solution system was filtered and then analyzed by HPLC. The analytical conditions and methods for HPLC were referenced from the determination method of total saponins in Paris polyphylla in the 2025 edition of the Chinese Pharmacopoeia.

[0047] HPLC detection results are as follows Figure 2 As shown, the peak at 3-4 min is the solvent peak, and the peak at 12-32 min corresponds to the Paris saponin peak. The test results show that almost all of the Paris saponins were removed during the filtration process, and the content of Paris saponins dissolved in water was extremely low.

[0048] Example 4 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract (the preparation process is as follows). Figure 6 (As shown), the specific steps are as follows: 1. Take 2.0 kg of Paris polyphylla raw material, crush it through a 20-mesh sieve to obtain Paris polyphylla powder. First extraction: add 8 Bv of 90% ethanol and reflux for 1.5 h; second extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; third extraction: add 6 Bv of 90% ethanol and reflux for 1.5 h; combine the three extracts, cool the extract and pass it through a 0.8 μm polypropylene membrane to obtain the total extract; 2. The total extract was concentrated under reduced pressure at 50–70℃ and -0.08–-0.09 MPa, and ethanol was recovered until the ethanol concentration of the concentrate was 80%. The volume of the concentrate was 8000 mL, and the primary concentrate was obtained. 3. The primary concentrate was passed through 670 g of acid- and alkali-treated LX-94 anion exchange resin at a flow rate of 1–2 Bv / h, followed by washing with 1 Bv of 80% ethanol. The decolorized solution and the washing solution were collected. The decolorized solution was then concentrated and dried under reduced pressure at 50–70℃ and -0.08–-0.09 MPa to obtain 190.0 g of Paris polyphylla extract with a total saponin content of 22.5%. 4. Take 28.2 g of the above Paris polyphylla extract (6.34 g of total saponins), 56.3 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (to obtain a solid content of 15.3%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 5. Pass the inclusion solution through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 6. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 7. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 90.2g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.34%, and the inclusion rate is 33.29%.

[0049] Example 5 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 16.9 g of the Paris polyphylla extract (3.8 g of total Paris polyphylla saponins), 67.6 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 16.9%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ inlet and 85℃ outlet to obtain 93.2g of white powdery water-soluble Paris polyphylla extract. (The water-soluble Paris polyphylla extract comprises Paris polyphylla extract, cyclodextrin, chelating agent and cellulose), the total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.27%, and the inclusion rate is 55.67%.

[0050] Example 6 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 14.1 g of the Paris polyphylla extract (3.17 g of total Paris polyphylla saponins), 70.4 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 15.0%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution is passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.0g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.23%, and the inclusion rate is 66.12%.

[0051] Example 7 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (to obtain a solid content of 15.0%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.7g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.25%, and the inclusion rate is 90.29%.

[0052] Figure 3 The image shown is of step 1, where the mixture is stirred to form the encapsulation. Figure 4 The glass on the left shows the inclusion solution obtained in step 1. Figure 4 The glass bottle on the right shows the ultrafiltrate obtained in step 2. From Figure 3 and Figure 4 As can be seen, the unencapsulated saponins cannot dissolve in the inclusion solution, making the inclusion solution turbid. However, after the treatment in step 2, the undissolved saponins in the inclusion solution are removed, thus restoring the solution to clarity.

[0053] The ultrafiltrate obtained in step 2 above was subjected to HPLC analysis. The analytical conditions and methods for HPLC were in accordance with the determination method of total saponins in Paris polyphylla, Chinese Pharmacopoeia 2025 edition. The detection results are as follows: Figure 5 As shown, the peak of Paris polyphylla saponins corresponds to 12-32 min, proving that inclusion greatly improves the solubility of Paris polyphylla saponins in the aqueous phase.

[0054] Example 8 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 8.4 g of Paris polyphylla extract (1.9 g of total Paris polyphylla saponins), 76.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 15.3%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain an inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170°C for air intake and 85°C for air outlet to obtain 94.8g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 1.80%, and the inclusion rate is 89.81%.

[0055] Example 9 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 6.5 g of the Paris polyphylla extract (1.46 g of total Paris polyphylla saponins), 78.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 15.5%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.2g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 1.38%, and the inclusion rate is 89.0%.

[0056] Example 10 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 5.3 g of Paris polyphylla extract (1.19 g of total Paris polyphylla saponins), 79.2 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 14.6%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain an inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain a white powdery water-soluble Paris polyphylla extract 94.9 (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponins of Paris polyphylla in the water-soluble Paris polyphylla extract are 1.13% and the inclusion rate is 90.11%.

[0057] Example 11 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 4.4 g of the Paris polyphylla extract (1 g of total Paris polyphylla saponins), 80.1 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 17.4%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain an inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.75g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 0.95%, and the inclusion rate is 90.01%.

[0058] Example 12 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract (total saponins 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na obtained in step 3 of Example 4 above, add pure water and dissolve evenly (to obtain a solid content of 14.8%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxyethyl cellulose (HEC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.65g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponins of Paris polyphylla in the water-soluble Paris polyphylla extract contain 2.21% and the inclusion rate is 88.63%.

[0059] Example 13 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (to obtain a solid content of 14.7%). Then, start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution is passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl carboxymethyl cellulose (HPCMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.5g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.19%, and the inclusion rate is 87.69%.

[0060] Example 14 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (so that the solid content of the obtained system is 14.9%). Start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 6.2 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 88.0g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.18%, and the inclusion rate is 81.29%.

[0061] Example 15 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (so that the solid content of the obtained system is 15.1%). Start stirring to carry out inclusion, stirring speed: 2000 r / min, temperature: 55℃, time: 2.0 h, to obtain the inclusion solution; 2. The inclusion solution was passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 8.6 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 90.14g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.25%, and the inclusion rate is 85.94%.

[0062] Example 16 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (so that the solid content of the obtained system is 14.8%). Start stirring to carry out inclusion at a stirring speed of 2000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 21.4 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170°C for air intake and 85°C for air outlet to obtain 101.5g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.02%, and the inclusion rate is 86.88%.

[0063] Example 17 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (so that the solid content of the obtained system is 15.1%). Start stirring to carry out inclusion, stirring speed: 2000 r / min, temperature: 55℃, time: 2.0 h, to obtain the inclusion solution; 2. The inclusion solution was passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 26.0 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 106.0g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 1.92%, and the inclusion rate is 86.24%.

[0064] Example 18 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, 2.0 g of EDTA-2Na, and 13.5 g of hydroxypropyl methylcellulose (HPMC). Add pure water to dissolve evenly (so that the solid content of the obtained system is 15.0%), start stirring to carry out inclusion, stirring speed: 2000 r / min, temperature: 55℃, time: 2.0 h, to obtain the inclusion solution; 2. The inclusion solution was passed through a 100 kDa ultrafiltration membrane to obtain the ultrafiltrate; 3. Spray drying at 170℃ for air intake and 85℃ for air outlet to obtain 94.0g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 1.87%, and the inclusion rate is 74.48%.

[0065] Example 19 This embodiment provides a method for preparing a water-soluble Paris polyphylla extract, the specific steps of which are as follows: 1. Take 10.5 g of the Paris polyphylla extract obtained in step 3 of Example 4 (total saponins of Paris polyphylla 2.36 g), 74.0 g of hydroxypropyl-β-cyclodextrin, and 2.0 g of EDTA-2Na, add pure water and dissolve evenly (to obtain a solid content of 14.7%). Then, start stirring to carry out inclusion at a stirring speed of 1000 r / min, a temperature of 55℃, and a time of 2.0 h to obtain the inclusion solution. 2. The inclusion solution was passed through a 100 KD ultrafiltration membrane to obtain the ultrafiltrate; 3. Add 13.5 g of hydroxypropyl methylcellulose (HPMC) to the ultrafiltrate, stir and dissolve at room temperature, and pass through a 0.22 μm nylon membrane to obtain the prepared solution; 4. Spray dry at 170℃ for air intake and 85℃ for air outlet to obtain 94.7g of white powdery water-soluble Paris polyphylla extract (the water-soluble Paris polyphylla extract consists of Paris polyphylla extract, cyclodextrin, chelating agent and cellulose). The total saponin content of Paris polyphylla in the water-soluble Paris polyphylla extract is 2.12%, and the inclusion rate is 85.07%.

[0066] The amount of each raw material added in the preparation methods of Examples 4-19 above is shown in Table 1. The total saponin content and inclusion rate of the obtained water-soluble Paris polyphylla extract are summarized in Table 1.

[0067] Table 1 Stability assessment: To examine the stability of the prepared samples, the water-soluble Paris polyphylla extract powder obtained in Examples 4-19 was prepared into a 1% aqueous solution (sample solution). Immediate observation revealed that all sample solutions were clear and transparent. Stability was then assessed by placing the solutions at room temperature. After three months, the sample solutions from Examples 7, 8, 9, 10, and 11 remained clear and transparent; while the sample solutions from Examples 4, 5, 6, 12, 13, 14, 15, 16, and 17 showed varying degrees of turbidity. Photos of the sample solutions from Examples 4-17 after three months of storage are shown below. Figure 7 As shown, Figure 7 The sample vials at the top, from left to right, represent the sample solutions from Examples 7, 8, 9, 10, and 11, respectively. Figure 7 The sample vials at the bottom, from left to right, represent sample solutions from Examples 4, 5, 6, 12, 13, 14, 15, 16, and 17, respectively. This demonstrates that the water-soluble Paris polyphylla extracts prepared in Examples 7-11 exhibit good water solubility and stability.

[0068] The sample solution in Example 18 became turbid on the second day after preparation. Figure 8 (The sample vial on the left in the image) indicates that the cyclodextrin needs to be filtered and clarified after inclusion before HPMC can be added.

[0069] The sample solution in Example 19 became turbid on the second day after preparation. Figure 8 (The sample bottle on the right in the image) indicates that reducing the stirring speed has little effect on the efficiency of the inclusion complex, but it will significantly reduce the water solubility stability of the inclusion complex.

[0070] Furthermore, the sample solution prepared by the Paris polyphylla extract in step 3 of Example 4 using the same method showed obvious turbidity and crystallization on the same day after preparation (Paris polyphylla saponins are difficult to dissolve in water but easy to dissolve in organic solvents due to their amphiphilic structure containing a steroidal nucleus (hydrophobic) and a sugar chain (polar), thus indicating that the Paris polyphylla extract without inclusion has poor water solubility).

[0071] Compatibility assessment: The water-soluble Paris polyphylla extract powder obtained in Examples 4-17 was prepared into a 1% aqueous solution, diluted to 1.0%, and then 0.5% GPL and 4% glycerol, 0.5% GPL and 4% ethanol, and 0.5% GPL and 4% 1,3-propanediol were added respectively. After being placed at room temperature for three months, the stability was observed. Figure 9 The sample shown contains 0.5% GPL and 4% glycerol. Figure 9 The sample vials at the top, from left to right, represent the sample solutions from Examples 7, 8, 9, 10, and 11, respectively. Figure 9The sample vials below, from left to right, are the sample solutions of Examples 4, 5, 6, 12, 13, 14, 15, 16, and 17, respectively; Figure 10 The sample shown contains 0.5% GPL and 4% ethanol. Figure 10 The sample vials at the top, from left to right, represent the sample solutions from Examples 7, 8, 9, 10, and 11, respectively. Figure 10 The sample vials below, from left to right, are the sample solutions of Examples 4, 5, 6, 12, 13, 14, 15, 16, and 17, respectively; Figure 11 The sample shown contains 0.5% GPL and 4% 1,3-propanediol. Figure 11 The sample vials at the top, from left to right, represent the sample solutions from Examples 7, 8, 9, 10, and 11, respectively. Figure 11 The sample vials at the bottom, from left to right, represent sample solutions from Examples 4, 5, 6, 12, 13, 14, 15, 16, and 17, respectively. After three months of observation, it was found that no precipitation occurred in the solutions prepared for Examples 7-11 after storage for more than three months, while the solutions prepared for Examples 4-6 and Examples 12-17 showed a tendency to become turbid.

[0072] Efficacy test: The water-soluble Paris polyphylla extracts prepared in Examples 7, 8, 9, 10, and 11 were used to prepare test samples with a test solution concentration of 1% using a matrix raw material (an aqueous solution containing 0.3% xanthan gum, labeled Base), and were labeled Y7, Y8, Y9, Y10, and Y11 respectively.

[0073] Clinical redness reduction and lactic acid stinging tests were performed on each test sample and the matrix raw material (labeled Base) control sample. The capsaicin concentration used was 200 μg / mL, and the lactic acid concentration was 10%.

[0074] 1. The specific clinical testing protocol for reducing redness is as follows: 1.1 After cleaning the inner arm, equilibrate for 20 minutes, and mark the test areas for each group with a marker. 3 cm 2 Each test area should be spaced at least 1 cm apart; 1.2 Skin base was tested using a skin color meter (Skin Color Catch, brand: Delfin). Value (i.e., a) value 刺激前 After applying 30 µL of capsaicin for 15 minutes, probe testing was performed. Value (i.e., a) value 刺激后 This is recorded as 0 minutes of repair.

[0075] 1.3 Then apply 25 µL of each test sample or Base control sample to the sample group; do not apply any sample to the irritant group.

[0076] After applying the test sample or base control sample for 30 minutes, the sample group and the stimulus group were tested again using the probe. Value (i.e., a) value 修护后 ), recorded as 30 min of repair.

[0077] 1.4 The specific data analysis methods are as follows: Δa for each sample group and stimulus group The value is calculated using the following formula: Δa value = a value 修护后 -a value 刺激前 Compared to the stimulus group, the Δa of the sample group The rate of change of value is calculated using the following formula: Δa Rate of change of value (%) = (Δa) value 样品组 / Δa value 刺激物组 -1) 100% Paired T-test, α=0.05, compared with the stimulus group (capsaicin), represent P <0.001, represent P <0.01, represent P <0.05, ns represents P >0.05.

[0078] The results of the alleviating effects of test samples Y7, Y8, Y9, Y10, Y11 and the Base control sample on capsaicin-induced skin redness are as follows: Figure 12 As shown. Compared to the capsaicin-stimulating group, the Δa of Y7, Y8, Y9, Y10, and Y11... The rates of change of the values ​​were -50.19%, -50.38%, -30.29%, -21.98%, and -16.93%, respectively, Δa. The value decreased significantly; while the Δa of the Base control sample decreased significantly. The value change rate was 2.42%, which was actually higher than that of the stimulus group.

[0079] 2. The specific testing protocol for clinical lactic acid stinging is as follows: 2.1 Prepare a 10% lactic acid solution in advance using sterile water. Cut the filter paper into 1×1 cm pieces. 2 Filter paper.

[0080] 2.2 After the subjects arrived, they washed their faces and wiped them clean with a washcloth.

[0081] 2.3 After equilibration in a constant temperature and humidity laboratory for 20 minutes, enter the internal testing room. During this period, drinking water, walking around, and touching the face are prohibited.

[0082] 2.4 Use a marker to mark an area of ​​about 1 cm square on the same location on both sides of the face (such as the left and right nasolabial grooves).

[0083] 2.5 Apply the sample: Use 50 μL of test sample (sample group) and Base control sample (matrix group) to evenly apply to the marked position (left and right nasolabial folds), and wait 15 min for the skin to absorb the sample.

[0084] 2.6 1×1 cm 2 Place the filter paper onto the sample application area, then add 50 μL of 10% lactic acid solution to the filter paper, and start timing immediately. The total test time is 5 minutes.

[0085] 2.7 Subjective Sensation Assessment: Sensation in each area was assessed and recorded at 2.5 min and 5 min after lactic acid application. Sensation was graded as follows: 0 points: no sensation; 1 point: mild stinging, itching, or burning, but not noticeable; 2 points: moderate stinging, noticeable but tolerable; 3 points: intense, unbearable stinging, burning, or itching.

[0086] 2.8 Calculate the total stinging score: Add the scores of the lactic acid area at the two time points of 2.5 min and 5 min to obtain the total stinging score.

[0087] 2.9 Specific data analysis is as follows: Using the matrix group as a control, the lactic acid stinging score and its rate of change in the sample group were analyzed, where: rate of change = (lactic acid stinging score of sample group / lactic acid stinging score of matrix group - 1). 100% Paired T-test, α=0.05, compared with the base control group, represent P <0.001, represent P <0.01, represent P <0.05, ns represents P >0.05.

[0088] The test results of the effects of samples Y7, Y8, Y9, Y10, and Y11 on alleviating lactic acid-induced skin discomfort are as follows: Figure 13 As shown in the figure. Compared with the Base control group, the changes in lactic acid stinging scores in Y7, Y8, Y9, Y10, and Y11 were -70.54%, -64.89%, -46.12%, -37.23%, and -31.06%, respectively, indicating a significant decrease in lactic acid stinging scores.

[0089] This invention has many specific applications, and the above description is only a preferred embodiment. It should be noted that the above embodiments are for illustrative purposes only and are not intended to limit the scope of protection of this invention. For those skilled in the art, several improvements can be made without departing from the principle of this invention, and these improvements should also be considered within the scope of protection of this invention.

Claims

1. A method for preparing a water-soluble Paris polyphylla extract, characterized in that, Includes the following steps: A. After crushing the raw material of Paris polyphylla, it is extracted with alcohol. The resulting extract is concentrated under reduced pressure for the first time and decolorized, and then concentrated under reduced pressure for the second time. The alcohol-free concentrate is dried to obtain Paris polyphylla extract. B. After dissolving the Paris polyphylla extract, cyclodextrin, and chelating agent in pure water until homogeneous, the resulting system is incorporated under stirring conditions to obtain an incorporation solution. C. The inclusion solution was subjected to ultrafiltration, and cellulose was added to the ultrafiltrate. After stirring and dissolving, the solution was filtered and spray-dried to obtain water-soluble Paris polyphylla extract. The ingredients, cyclodextrin, chelating agent and cellulose are, by weight, 4-30 parts, 50-86 parts, 1-3 parts and 6-26 parts, respectively. The mass ratio of total saponins from Paris polyphylla to cyclodextrin in the Paris polyphylla extract is 1:30-80. The encapsulation process involves stirring at a speed of 2000–10000 r / min and encapsulating in a constant-temperature water bath at 50–60 ℃ for 1.5–2.5 h.

2. The method for preparing the water-soluble Paris polyphylla extract according to claim 1, characterized in that, In step B, the cyclodextrin includes at least one of hydroxypropyl-β-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, and α-cyclodextrin; The chelating agent is EDTA-2Na.

3. The method for preparing the water-soluble Paris polyphylla extract according to claim 1, characterized in that, In step B, the solids content of the system is 14-18%.

4. The method for preparing the water-soluble Paris polyphylla extract according to claim 1, characterized in that, In step C, the cellulose is selected from at least one of hydroxypropyl methylcellulose, hydroxyethylcellulose, and hydroxypropyl carboxymethylcellulose.

5. The method for preparing the water-soluble Paris polyphylla extract according to claim 1 or 4, characterized in that, The cellulose is present in parts by weight of 10 to 18.

6. The method for preparing the water-soluble Paris polyphylla extract according to claim 1 or 4, characterized in that, In step C, the ultrafiltration uses an ultrafiltration membrane with a molecular weight cutoff of 20–100 kDa; the filtration uses a 0.1–0.22 μm nylon membrane.

7. The method for preparing the water-soluble Paris polyphylla extract according to claim 1, characterized in that, In step A, the solvent used for the alcohol extraction is at least one of ethanol and methanol; reflux extraction is performed 2 to 4 times, with each extraction lasting 1 to 2 hours.

8. The method for preparing the water-soluble Paris polyphylla extract according to claim 1, characterized in that, In step A, the decolorization process uses at least one of LX-94 anion exchange resin, acidic alumina, and activated carbon.

9. A water-soluble Paris polyphylla extract prepared according to any one of claims 1-8, characterized in that, The water-soluble Paris polyphylla extract comprises Paris polyphylla extract, cyclodextrin, chelating agent and cellulose.

10. The use of a water-soluble Paris polyphylla extract prepared according to any one of claims 1-8 or the water-soluble Paris polyphylla extract according to claim 9 in the preparation of cosmetics.

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