Compound pearl ancient-method polymer and preparation method thereof

Abstract

The invention relates to the technical field of cosmetics, and discloses a compound pearl ancient-method polymer and a preparation method thereof.The compound pearl ancient-method polymer comprises water, a mint extract, a radix rehmanniae extract, a feverfew extract and nano pearl powder. The preparation method comprises the following steps: extracting white chrysanthemum through a carbon dioxide supercritical fluid to obtain a volatile component, extracting and concentrating mint leaves into extract through a gradient percolation method, preparing pearl into nano pearl powder with the particle size of less than 100nm through a biological enzymolysis process, and mixing the extract and deionized water in stages under the protection of inert gas. Through trehalose modification on the surface of the nano pearl powder and a staged mixing process, the component stability of the compound pearl ancient-method polymer is improved, the degradation rate of effective components can be as low as 4%, trehalose modification provides additional protection for the nano pearl powder, and the staged mixing process ensures that all the components are uniformly mixed under the protection of inert gas; and oxidation and degradation of the components are reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and specifically to a compound pearl ancient method polymer and a preparation method thereof. Background Art

[0002] As a traditional Chinese medicine and beauty raw material, pearls have a long application history. Its main components include various amino acids, minerals and bioactive substances, and have effects such as antioxidant, anti-inflammatory, and repairing skin barrier. However, traditional pearl preparations have problems such as low component extraction efficiency, poor bioavailability, and insufficient stability, which limit their wide application in the fields of modern medicine and cosmetics.

[0003] Currently, most pearl preparations on the market are still prepared by traditional processes. The pearl powder prepared by traditional processes is prone to degradation during storage, resulting in loss of active ingredients; while the particle size of ordinary pearl powder is relatively large, making it difficult to effectively penetrate the skin cutin layer, which limits its application in skin care. In addition, the surface modification of pearl powder in the prior art is insufficient, and its biological activity has not been fully exerted. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the present invention provides a compound pearl ancient method polymer and a preparation method thereof, which solve the problems of low extraction efficiency, poor bioavailability and insufficient component stability of traditional pearl preparations.

[0005] To achieve the above objectives, the present invention is realized through the following technical solutions: A compound pearl ancient method polymer, comprising the following substances in mass percentages: 30%-65% water, 5%-l5% mint extract, 8%-25% rehmannia root extract, 7%-22% white chrysanthemum extract, 3%-15% nano pearl powder.

[0006] By adopting the above technical solutions: through the trehalose modification on the surface of nano pearl powder and the staged mixing process, the component stability of the compound pearl ancient method polymer is significantly improved. The accelerated test shows that the degradation rate of active ingredients can be as low as 4%, far lower than 15% of the traditional process. The trehalose modification provides additional protection for nano pearl powder, while the staged mixing process ensures that each component is uniformly mixed under the protection of inert gas, reducing the oxidation and degradation of components.

[0007] Preferably, the mass percentages of each component are: 49% water, 15% mint extract, 18% rehmannia root extract, 10% white chrysanthemum extract, 8% nano pearl powder.

[0008] Preferably, the surface of the nano pearl powder is modified with trehalose, and the addition amount of the modifier is 1%-3% of the mass of the pearl powder.

[0009] Preferably, a method for preparing a compound pearl ancient method polymer, which is used for the compound pearl ancient method polymer described above, the method comprising the following steps: S1. After slicing the rehmannia root, extract the active ingredients by using a low-temperature ultrasonic extraction technique; S2. Obtain the volatile components from the white chrysanthemum by supercritical carbon dioxide fluid extraction; S3. Extract and concentrate the peppermint leaves into an extract by gradient percolation; S4. Prepare nano pearl powder with a particle size less than 100 nm from pearls by a biological enzymolysis process; S5. Mix the above extracts with deionized water in stages under the protection of an inert gas. First, add the rehmannia root extract and stir evenly for 20 - 40 minutes, then add the white chrysanthemum extract and react at a constant temperature of 50 - 60 °C for 1 - 2 hours, and finally add the peppermint extract and nano pearl powder in sequence for homogenization treatment.

[0010] Preferably, the low-temperature ultrasonic extraction temperature is 35 - 45 °C, the frequency is 28 - 40 kHz, and the extraction time is 30 - 90 minutes.

[0011] Preferably, the supercritical carbon dioxide fluid extraction pressure is 15 - 25 MPa, the temperature is 40 - 50 °C, and the separation kettle pressure is 6 - 10 MPa.

[0012] Preferably, the gradient percolation method uses a 30% - 70% ethanol solution as the solvent, the flow rate is controlled at 2 - 5 mL / min, and after collecting the percolate, it is concentrated under reduced pressure to a relative density of 1.10 - 1.20.

[0013] Preferably, the biological enzymolysis process uses a compound protease and lipase mixed in a ratio of 1:0.5, the enzymolysis pH value is 7.5 - 8.5, the temperature is 37 - 42 °C, and the time is 4 - 8 hours.

[0014] Preferably, the homogenization treatment is carried out in a high-pressure homogenizer, the pressure range is 60 - 100 MPa, and the cyclic treatment is carried out 3 - 5 times.

[0015] Preferably, the final product is sterilized by a microfiltration membrane, the membrane pore size is 0.22 - 0.45 μm, and the operating pressure is 0.1 - 0.3 MPa.

[0016] The present invention provides a compound pearl ancient method polymer and a preparation method thereof. It has the following beneficial effects: 1. Through the trehalose modification on the surface of nano pearl powder and the staged mixing process, the component stability of the compound pearl ancient method polymer is significantly improved. Accelerated tests show that the degradation rate of the active ingredients can be as low as 4%, far lower than 15% of the traditional process. The trehalose modification provides additional protection for the nano pearl powder, while the staged mixing process ensures the uniform mixing of each component under the protection of inert gas, reducing the oxidation and degradation of the components.

[0017] 2. The present invention uses an optimized nanonization technology to prepare nano pearl powder with a particle size less than 100nm, significantly improving the transdermal absorption ability. The transdermal absorption rate of the nano pearl powder can be up to 3.5 times that of the traditional process at most. This improvement mainly benefits from the nanonization treatment and the staged mixing process, making the active ingredients easier to penetrate the skin and improving the bioavailability of the product.

[0018] 3. By high-pressure supercritical fluid extraction of white chrysanthemum and extending the enzymatic hydrolysis time, the antioxidant activity of the compound pearl ancient method polymer is significantly enhanced. Its antioxidant capacity (IC50 = 0.18mg / mL) is significantly better than that of the traditional process (IC50 = 0.50mg / mL). These process improvements effectively increase the content and biological activity of the active ingredients, making the product perform excellently in terms of antioxidant. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a flowchart of the preparation method of a compound pearl ancient method polymer of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0020] The technical solutions of the present invention will be clearly and completely described below in conjunction with the drawings of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0021] Example 1: Basic formula and preparation process I. Technical solution This example provides a compound pearl ancient method polymer, and its mass percentage composition is: water 49%, mint extract 15%, rehmannia extract 18%, white chrysanthemum extract 10%, nano pearl powder 8%, wherein the surface of the nano pearl powder is modified by trehalose, and the addition amount of the modifier is 2% of the mass of the pearl powder.

[0022] II. Preparation method 1. Extraction of rehmannia Low-temperature ultrasonic extraction was adopted, with specific parameters of 40 °C, 35 kHz, and 60 min. After slicing the Rehmannia glutinosa, extraction was carried out, and the yield was increased by 12% compared with the traditional water decoction method. The comparative experiment referred to the "Ultrasonic Extraction Method" in General Principles 2201, Volume IV of the Chinese Pharmacopoeia 2020 Edition. Taking the catalpol content as the index, the extraction efficiency of this method reached 92.5 ± 1.8%, which was significantly improved compared with conventional reflux extraction (80.3 ± 2.1%) (p < 0.05).

[0023] 2. Extraction of Chrysanthemum morifolium Supercritical carbon dioxide fluid extraction was used, with parameter settings of 20 MPa and 45 °C, and the separation kettle pressure of 8 MPa, which increased the retention rate of chlorogenic acid by 15%. According to GB / T 31743-2015 "Technical Specification for Supercritical Fluid Extraction Technology" in the comparative experiment, compared with traditional ethanol extraction, the total flavonoid yield increased by 18.7%, and no solvent residue was detected.

[0024] 3. Preparation of peppermint extract The gradient percolation method was adopted, using 50% ethanol as the solvent, with the flow rate controlled at 3 mL / min, and concentrated to a relative density of 1.15. At this time, the menthol content reached 85 mg / g.

[0025] 4. Preparation of nano pearl powder Through the biological enzymatic hydrolysis method, the enzyme system ratio was compound protease: lipase = 1:0.5, and the reaction was carried out at pH 8.0 and 40 °C for 6 h. The D50 of the prepared nano pearl powder was 68 nm (measured by a Malvern laser particle size analyzer).

[0026] 4. Mixing and homogenization Under the protection of inert gas, each component was mixed in stages, and then high-pressure homogenization was carried out. The pressure was set at 80 MPa, and homogenization was carried out 4 times. Finally, microfiltration sterilization was carried out using a 0.3 μm membrane.

[0027] III. Verification of technical effects Stability test: According to the ICH Q1A (R2) accelerated test guideline, an accelerated test was carried out at 40 °C and RH 75% for 30 days. The degradation rate of the active ingredient ≤ 5% (determined by HPLC), which was better than the unmodified pearl powder formula (degradation rate ≥ 12%).

[0028] In vitro transdermal experiment: According to the in vitro permeation method of the "Cosmetics Safety and Technology Specifications" (2022 Edition), an experiment was carried out using a Franz diffusion cell. The results showed that the skin penetration amount of nano pearl powder was increased by 3.2 times compared with ordinary pearl powder (p < 0.01).

[0029] IV. Conclusion In this example, by optimizing the extraction process and nanotechnology, the stability and bioavailability of the components were significantly improved, providing a scientific basis for the improvement of subsequent formulations.

[0030] Example 2: Parameter-Optimized Formula I. Technical Solution Adjust the component ratio to: 55% water, 12% mint extract, 20% rehmannia root extract, 8% white chrysanthemum extract, 5% nano pearl powder, and the modification amount of trehalose is 1%.

[0031] II. Process Improvement 1. Rehmannia Root Extraction Optimize the ultrasonic parameters to 38°C, 40 kHz, and 45 min, so that the yield of catalpol is increased by 6% compared with Example 1.

[0032] 2. Homogenization Pressure Adjustment Adopt low-pressure homogenization at 60 MPa and circulate 5 times to make the particle size distribution more uniform, and the PDI (polydispersity index) is 0.21 ± 0.03.

[0033] III. Comparative Experiment 1. Influence of Particle Size Referring to ISO22412:2017 "Dynamic Light Scattering Method", it is found by comparison that the PDI of the low-pressure homogenized product is 27% lower than that of the high-pressure homogenized (100 MPa), indicating better dispersibility.

[0034] 2. Comparison of Modifier Dosage The dissolution rate of 1% trehalose-modified pearl powder in simulated gastric juice reaches 94% in 2 h, while the dissolution rate of the 3% modification group decreases to 82% due to over-dense coating.

[0035] IV. Conclusion In this example, by finely regulating the process parameters, the balance between the solubility and stability of the components is achieved, and the formula performance is further optimized.

[0036] Example 3: High-Activity Component Formula I. Technical Solution The composition is: 45% water, 18% mint extract, 15% rehmannia root extract, 15% white chrysanthemum extract, 7% nano pearl powder, and the modification amount of trehalose is 3%.

[0037] II. Key Processes 1. White Chrysanthemum Extraction Adopt high-pressure supercritical extraction at 25 MPa to make the total flavonoid content reach 120 mg / g, which is 22% higher than that in Example 1.

[0038] 2. Enzymolysis Process Prolong the enzymolysis time to 8 h, so that the proportion of pearl powder peptide segments with a molecular weight < 1 kDa reaches 91% (verified by SDS-PAGE).

[0039] III. Effect Verification 1. Antioxidant experiment The antioxidant experiment was carried out by the DPPH method. The IC50 of the product in this example was 0.18 mg / mL, which was significantly lower than that of the control sample (0.35 mg / mL).

[0040] 2. Cell experiment The cell experiment was carried out using the HaCaT model. The amount of collagen synthesis promoted by pearl powder peptides was increased by 40% compared with the non-enzymatic hydrolysis group (detected by ELISA).

[0041] IV. Conclusion In this example, by strengthening the extraction and degradation processes of active ingredients, the antioxidant and skin repair functions of the product were significantly improved, meeting the requirements for highly active products.

[0042] V. Comprehensive comparative analysis Summary: Each example was superior to the traditional process in terms of component stability, transdermal absorption rate, and antioxidant activity. Example 3 showed the best performance in terms of degradation rate (≤4%) and antioxidant activity (IC50 was 0.18 mg / mL), and at the same time had the highest transdermal absorption rate (3.5 times). Examples 1 and 2 were also superior to the traditional process in all indicators, but their comprehensive performance was slightly lower than that of Example 3.

[0043] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A compound pearl ancient method polymer, characterized in that It consists of the following substances by mass percentage: 30%-65% water, 5%-20% mint extract, 8%-25% rehmannia root extract, 7%-22% white chrysanthemum extract, and 3%-15% nano pearl powder.

2. The compound pearl ancient method polymer according to claim 1, wherein The mass percentage of each component is: 49% water, 15% mint extract, 18% rehmannia root extract, 10% white chrysanthemum extract, and 8% nano pearl powder.

3. A compound pearl ancient method polymer according to claim 1, characterized in that: The surface of the nano pearl powder is modified with trehalose, and the addition amount of the modifier is 1%-3% of the mass of the pearl powder.

4. A preparation method of a compound pearl ancient polymer, characterized in that, For a compound pearl ancient method polymer according to any one of claims 1-2, the method comprises the following steps: S1. Cut the rehmannia root into slices and extract the active ingredients by low-temperature ultrasonic extraction technology; S2. Obtain the volatile components from the white chrysanthemum by supercritical carbon dioxide fluid extraction; S3. Extract and concentrate the mint leaves into an extract by gradient percolation method; S4. Prepare nano pearl powder with a particle size less than 100 nm from pearls by biological enzymatic hydrolysis process; S5. Mix the above extracts with deionized water in stages under the protection of inert gas. First, add the rehmannia root extract and stir evenly for 20-40 minutes, then add the white chrysanthemum extract and react at a constant temperature of 50-60 °C for 1-2 hours, and finally add the mint extract and nano pearl powder in sequence for homogenization treatment.

5. The preparation method of a compound pearl ancient method polymer according to claim 4, characterized in that: The low-temperature ultrasonic extraction temperature is 35-45 °C, the frequency is 28-40 kHz, and the extraction time is 30-90 minutes.

6. The preparation method of a compound pearl ancient polymer according to claim 4, characterized in that: The pressure of the supercritical carbon dioxide fluid extraction is 15-25 MPa, the temperature is 40-50 °C, and the pressure of the separation kettle is 6-10 MPa.

7. The preparation method of a compound pearl ancient method polymer according to claim 4, characterized in that: The gradient percolation method uses a 30%-70% ethanol solution as the solvent, the flow rate is controlled at 2-5 mL / min, and after collecting the percolate, it is concentrated under reduced pressure to a relative density of 1.10-1.

20.

8. The preparation method of a compound pearl ancient method polymer according to claim 4, characterized in that: The biological enzymatic hydrolysis process uses a composite protease and lipase mixed in a ratio of 1:0.5, the enzymatic hydrolysis pH value is 7.5-8.5, the temperature is 37-42 °C, and the time is 4-8 hours.

9. The preparation method of a compound pearl ancient polymer according to claim 4, characterized in that: The homogenization treatment is carried out in a high-pressure homogenizer, and the pressure range is 60-100 MPa, and the cycle treatment is carried out 3-5 times.

10. The preparation method of a compound pearl ancient polymer according to claim 4, characterized in that: The final product is sterilized by a microfiltration membrane, the membrane pore size is 0.22-0.45 μm, and the operating pressure is 0.1-0.3 MPa.

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