Extraction method of dendrobium chrysostomum and application thereof
By combining ultrasound-assisted extraction and supercritical fluid extraction technologies, the problem of incomplete extraction of active ingredients from Dendrobium nobile has been solved, achieving nano-sized active ingredients and skin penetration, providing long-term acne treatment and skin stabilization effects.
Patent Information
- Application Number
- CN202610141224.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-02
- Publication Date
- 2026-05-29
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Figure CN122097225A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of daily chemical products, specifically relating to an extraction method and application of Dendrobium nobile. Background Technology
[0002] Acne, a common skin problem, troubles a large number of people. The core mechanism of acne is chronic inflammation of the pilosebaceous unit. Elevated hormone levels stimulate sebaceous gland hyperplasia and excessive sebum secretion, creating an oily environment. A decrease in linoleic acid in sebum leads to excessive keratinization of the follicular epithelium, causing shed cells to clog pores and form closed or open comedones. The hypoxic environment within the follicle promotes the proliferation of Propionibacterium acnes, which decomposes sebum to produce free fatty acids, triggering an inflammatory response and forming red, swollen papules or pustules. Bacterial metabolites activate immune cells, releasing inflammatory factors that can cause the follicle wall to rupture. The contents can seep into the dermis, causing deep damage such as nodules and cysts. In severe cases, it can damage the skin barrier, leading to acne scars, pits, and other subsequent skin problems.
[0003] Most existing acne treatment products mainly use acid-based ingredients such as salicylic acid and azelaic acid to promote epidermal metabolism and achieve acne treatment. However, these products have obvious drawbacks: they are prone to causing photosensitivity reactions, increasing the skin's sensitivity to ultraviolet rays, and can lead to pigmentation if sun protection is not in place; moreover, their exfoliating effect can damage the skin barrier, making them unfriendly to people with sensitive acne-prone skin and difficult to meet the needs of acne treatment and skin repair at the same time.
[0004] Studies have found that active ingredients such as polysaccharides and bibenzyl compounds in Dendrobium nobile extract have the potential to reduce inflammation, inhibit excessive sebum secretion, alleviate acne redness and swelling, and repair the skin barrier. However, current extraction methods for the effective components of Dendrobium nobile are insufficient, failing to simultaneously and efficiently extract both water-soluble and fat-soluble active ingredients. Furthermore, when the extracted active ingredients are applied to facial compositions, they exhibit weak penetration and slow release, hindering their full potential for anti-inflammatory, oil-controlling, and barrier-repairing effects, thus preventing the achievement of long-term effective acne treatment and skin stabilization. Summary of the Invention
[0005] The technical problem to be solved by the present invention is to provide an extraction method and application of Dendrobium nobile. The present invention combines ultrasound-assisted extraction, amphiphilic crystalline copolymer composite dissolution and supercritical fluid extraction technology, which can achieve both slow release of effective ingredients and improve skin penetration, ensuring that the active ingredients can play a full role.
[0006] The technical solution adopted by the present invention to solve the above problems is as follows: A method for extracting Dendrobium nobile includes the following steps: S1. Wash Dendrobium nobile and freeze it at -30 to -45°C. Then freeze-dry it under vacuum at 40 to 70 Pa and -50 to -60°C. After drying, pulverize it and pass it through a 10 to 50 mesh sieve to obtain Dendrobium nobile granules. S2. Grind the amphiphilic crystalline polymer to 100-150 mesh, and then mix it with Dendrobium nobile particles. The mass ratio of the amphiphilic crystalline polymer to Dendrobium nobile is 1:5-10 to obtain the first mixture. S3. The first mixture is immersed in an aqueous ethanol solution with a volume fraction of 30-50% and subjected to ultrasonic-assisted extraction. The ultrasonic extraction power is 200-500W, the extraction time is 45-60min, and the extraction temperature is 30-40℃ to obtain the second mixture. S4. The second mixture is subjected to supercritical carbon dioxide extraction at a temperature of 35–50°C, an extraction pressure of 20–35 MPa, and an extraction time of 30–120 min. After extraction, the mixture is crystallized under reduced pressure at 0.5–3 MPa / min to obtain the third mixture. S5. The third mixture is immersed in an aqueous ethanol solution with a volume fraction of 30-50% and then crystallized under reduced pressure of 0.5-3 MPa / min to obtain Dendrobium nobile extract.
[0007] Through the aforementioned technical solution, ultrasound-assisted extraction (UAE), amphiphilic crystalline copolymer compound dissolution, and supercritical fluid technology work synergistically. High-frequency ultrasonic oscillation disrupts the cell walls of *Dendrobium nobile*, and then the amphiphilic crystalline copolymer and *Dendrobium nobile* raw material are dissolved together in an organic solvent. This allows the copolymer to fully combine with the hydrophilic and hydrophobic components of *Dendrobium nobile*, ultimately yielding *Dendrobium nobile* extract using supercritical fluid technology. The amphiphilic crystalline polymer allows the hydrophilic and hydrophobic components in *Dendrobium nobile* molecules to align at the oil-water interface, reducing surface tension and forming ordered assemblies such as micelles and vesicles. Water-soluble substances in *Dendrobium nobile* form the hydrophilic crown of micelles through hydration forces with the amphiphilic crystalline copolymer, while lipid-soluble substances are encapsulated by the hydrophobic chains of the amphiphilic crystalline copolymer, forming a robust core. This provides the resulting assemblies with mechanical strength and thermal stability. Supercritical carbon dioxide flows upward through the extractor and, via an amphiphilic crystalline copolymer, loads both water-soluble and fat-soluble active ingredients from *Dendrobium nobile*, simultaneously encapsulating these components to extract both. This extraction method of the present invention can simultaneously and efficiently extract both water-soluble and fat-soluble active ingredients from *Dendrobium nobile*. Furthermore, the copolymer encapsulates the active substances within the molecules, achieving nano-sized active ingredients. When these nano-sized active ingredients are applied to facial compositions, they achieve slow release and enhanced skin penetration, ensuring the active ingredients exert their full effect. In addition, the extraction method of the present invention is gentle, suitable for heat-sensitive ingredients, leaves low organic solvent residue, saves energy, and offers good selectivity.
[0008] Further, in step S2, the amphiphilic crystalline polymer includes any one of PEG-b-PCL, PEG-b-PLL, and APHBA-b-PEO.
[0009] Dendrobium extract is highly effective, but many of its active ingredients have poor water solubility and low bioavailability. The aforementioned technical solution utilizes a PEG-b-PCL crystalline core that effectively preserves the active substances and provides a biocompatible outer shell. PEG-b-PCL binds to negatively charged substances via electrostatic attraction, achieving efficient encapsulation of negatively charged components of the active substances. The APHBA core of APHBA-b-PE0 allows for better target release under acidic conditions.
[0010] The present invention also provides the application of the above-mentioned Dendrobium nobile extract in care compositions, for example, adding the Dendrobium nobile extract prepared in the present invention into care compositions, including but not limited to hand cream, body lotion, and body moisturizer.
[0011] This invention provides a facial care composition containing Dendrobium nobile extract prepared by the above method, comprising the following components by weight percentage: 0.05-5% Dendrobium nobile extract prepared by this invention; 0.1-10% moisturizer; 0.5-5% oil; 0.1-2% thickener; 1-5% emulsifier; 0.5-1% co-emulsifier; 0.03-1.5% preservative; 0.01-1.5% pH adjuster; and the balance being purified water.
[0012] Through the above technical solutions, the facial care composition of the present invention can increase the moisture content of the stratum corneum, inhibit lipid peroxidation, improve skin barrier performance, inhibit the production of nitric oxide, block inflammatory factors, and maintain the long-term stable state of the skin, thereby achieving a long-term acne-removing effect.
[0013] Furthermore, the moisturizer includes at least one of glycerin, propylene glycol, hyaluronic acid, ceramide, panthenol, and urea.
[0014] The ideal moisture content of the stratum corneum is 20-35%. If it falls below 10%, it will become dry, rough, and even cracked. Oil-water imbalance is also one of the causes of acne. The above-mentioned technology can retain moisture from the air and skin within the stratum corneum, increasing its moisture content. Propylene glycol has a refreshing, non-sticky feel and also promotes penetration, facilitating the absorption of active ingredients into the skin. Panthenol enhances moisturizing effects, soothes, and promotes the repair of damaged skin barrier function. Hyaluronic acid is abundant in the dermis and is a key substance for maintaining skin moisture and elasticity, possessing strong water-absorbing, soothing, and skin barrier repair capabilities.
[0015] Furthermore, the oil includes at least one of polydimethylsiloxane, jojoba seed oil, deep-sea shepherd's purse seed oil, squalane, and shea butter.
[0016] Through the above technical solutions, skin oil is mainly divided into sebaceous gland lipids and intercellular lipids. Their main functions are to establish a physical barrier, activate cell proliferation and differentiation, stimulate epidermal cell apoptosis, and maintain the skin microbiome cycle. The longer the fatty acid chain, the denser the lipid accumulation, and the better the skin barrier function. Polydimethylsiloxane can penetrate the skin well and improve the smoothness of the composition, reducing its stickiness. Squalane has a structure similar to squalene, a component of human sebum, making it easy to integrate into the skin and form a protective film on the skin surface. Avocados are rich in unsaturated fatty acids, which not only promote lipid accumulation but also moisturize, repair, and soothe the skin.
[0017] Furthermore, the emulsifier includes anionic emulsifiers, cationic emulsifiers, and nonionic emulsifiers.
[0018] Furthermore, the emulsifier includes at least one of olive oil cetyl ester / sorbitan olive oil ester, glyceryl stearate / PEG-100 stearate, arachidonic alcohol / docosahexadecyl alcohol / eicosyl glucoside.
[0019] Furthermore, the co-emulsifier includes at least one of cetearyl alcohol, cetyl alcohol, stearyl alcohol, stearic acid, and lauric acid.
[0020] The above technical solution enables the oil and water phases to mix fully, forming a stable emulsion system.
[0021] Furthermore, the thickener includes at least one of xanthan gum, carbomer polymer, cyanoethyl cellulose, sodium acrylate / sodium acryloyl dimethyl taurate copolymer, acrylic polymer, polyacrylamide / C13-14 isoalkane / lauryl polyoxyethylene ether, and sodium polyacrylate.
[0022] The above technical solution enables the composition to form a gel network, thereby making the composition more stable.
[0023] Furthermore, the preservative includes at least one of p-hydroxyacetophenone, phenoxyethanol, and hexanediol.
[0024] Furthermore, the pH adjuster includes at least one of sodium hydroxide, potassium hydroxide, and triethanolamine.
[0025] The present invention has the following beneficial effects: 1. The preparation method of Dendrobium nobile extract of the present invention combines ultrasound-assisted extraction, amphiphilic crystalline copolymer composite dissolution, and supercritical fluid extraction technology to efficiently extract water-soluble and lipid-soluble active ingredients from Dendrobium nobile. Furthermore, the copolymer encapsulates the active substances within the molecules, achieving nano-sized active ingredients. When these nano-sized active ingredients are applied to facial compositions, they achieve slow release and enhance skin penetration, ensuring the active ingredients exert their full effect. In addition, the extraction method of the present invention is gentle, suitable for heat-sensitive ingredients, leaves low organic solvent residue, saves energy, and exhibits good selectivity.
[0026] 2. The facial care composition of the present invention can enhance the moisture content of the stratum corneum, block inflammatory factors, and improve the skin barrier function, thereby achieving the effect of acne removal. Attached Figure Description
[0027] Figure 1 Images were captured by volunteers before (a1) and after (a2) using Example 9 of the present invention.
[0028] Figure 2 Images were captured for volunteers before (b1) and after (b2) using Example 10 of the present invention.
[0029] Figure 3 Images were captured by volunteers before (c1) and after (c2) using Example 11 of the present invention.
[0030] Figure 4 Images were captured for volunteers before (d1) and after (d2) using Example 12 of the present invention.
[0031] Figure 5 Images were collected from volunteers of this invention before (e1) and after (e2) use of Comparative Example 8.
[0032] Figure 6 Images were collected from volunteers of this invention before (f1) and after (f2) use of Comparative Example 9. Detailed Implementation
[0033] To make the technical problems, solutions, and advantages of this invention clearer, a detailed description will be provided below with reference to specific examples. However, the scope of protection of this invention is not limited to the following specific embodiments. The described embodiments are merely some, not all, of the embodiments of this invention, and are not intended to limit the invention. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.
[0034] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.
[0035] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.
[0036] In the quantitative experiments in the following examples, three replicate experiments were set up, and the data are the average of the three replicate experiments or the average ± standard deviation.
[0037] The present invention includes Examples 1 to 8 and Comparative Examples 1 to 5 to verify the extraction process of the present invention. The specific parameters and operations are shown in Tables 1 to 2.
[0038] Table 1
[0039] Table 2
[0040] The concentrations of the ethanol-water solutions in Tables 1 and 2 are the concentrations of ethanol in steps S3 and S5.
[0041] Specifically, the preparation method of Dendrobium nobile extract in this embodiment includes the following steps: S1. Wash Dendrobium nobile and freeze at -40℃, then freeze dry under vacuum at 50Pa and -50℃. After drying, pulverize and pass through a 50-mesh sieve to obtain Dendrobium nobile granules. S2. Grind the amphiphilic crystalline polymer to 150 mesh, and then mix it with Dendrobium nobile particles. The mass ratio of the amphiphilic crystalline polymer to Dendrobium nobile is shown in Table 1. The first mixture is obtained. S3. The first mixture is immersed in an aqueous ethanol solution with the volume fraction specified in Table 1 and subjected to ultrasonic-assisted extraction. The power, extraction time and extraction temperature of the ultrasonic-assisted extraction are shown in Table 1 to obtain the second mixture. S4. The second mixture is transferred to a supercritical carbon dioxide extraction vessel for supercritical carbon dioxide extraction. The extraction temperature, extraction pressure and extraction time are shown in Table 1. After extraction, the third mixture is obtained by depressurization crystallization at 2 MPa / min through a pressure reducing valve. S5. The third mixture is immersed in an aqueous ethanol solution with a volume fraction of 30-50%, and then crystallized after being subjected to a pressure reducing valve at 2 MPa / min to obtain Dendrobium nobile extract.
[0042] Similarly, the preparation method for the comparative example can be obtained. If there are substances that are not added or operations that are omitted, they can be omitted in the corresponding preparation steps.
[0043] This invention prepares a facial care composition using the Dendrobium nobile extract prepared by the process of Example 3, and sets up Examples 9-12 and Comparative Example 8; then, a facial care composition is prepared using the Dendrobium nobile extract prepared by the process of Comparative Example 3, and set up Comparative Example 9; the specific components and contents are shown in Table 3, and the units are weight percentages.
[0044] Table 3
[0045] The preparation methods of the facial compositions in the above embodiments and comparative examples are conventional configuration and mixing techniques in the art, and will not be described in detail here.
[0046] Testing and Inspection 1. The extract yields of Examples 1-8 and Comparative Examples 1-5 were calculated, and the specific test results are shown in Table 4.
[0047] 2. Recruit 20 female volunteers aged 25 to 30 to evaluate the instrument's effectiveness in Examples 9 to 12 and Comparative Examples 6 to 7.
[0048] 2.1 Experimental Basis: Referenced to HAB / R-WI-314, "Evaluation Methods for the Acne-Clearing Efficacy of Cosmetics - Human Trial Method". 2.1.1 Judgment Principles Parameters: The primary parameters are the number of pimples or blackheads (including whiteheads) and graphic analysis, while the secondary parameter is the skin a* value.
[0049] Positive results: A significant improvement in the number of pimples and blackheads (including whiteheads) after product use or in the sample area compared to before product use or the control area (p<0.05), combined with visual comparison of images, indicates that the sample has acne-removing efficacy. A significant improvement in any primary parameter after product use or in the sample area compared to before product use or the control area (p<0.05) indicates that the sample helps the skin recover after acne occurs.
[0050] Negative results: If, compared to the area before product use or the control area, there is no significant improvement in the number of pimples and blackheads (including whiteheads) after product use or in the sample area, and there is no significant improvement in visual comparison with images, then the sample does not have acne-removing effects. If, compared to the area before product use or the control area, there is no significant improvement in secondary parameters after product use or in the sample area, then the sample does not help the skin recover after acne occurs.
[0051] 2.2 Test principle: The number of pimples and changes in skin a* value were measured by instruments before and after three consecutive days of sample use in the subject population to evaluate the efficacy of the sample.
[0052] 2.3 Testing Instrument: Multifunctional 3D Skin Imaging Analyzer (Antera 3D®HC1023Q), which uses 24 LEDs of 7 different wavelengths to perform spatial and spectral analysis and optical methods and mathematical algorithms to acquire three-dimensional images; and extracts data from images related to the three-dimensional shape of the skin.
[0053] 2.4 Images were collected from the experimental areas of volunteers with acne, and the number of acne and skin a* value were analyzed and recorded as the initial value T0d.
[0054] 2.5 Application method: After cleansing the skin, apply an appropriate amount of sample evenly to the test area of the face with acne, and use twice a day.
[0055] 2.6 After sample use: Images of the test area were acquired 3 days after sample use, and the number of pimples and skin a* value were analyzed and recorded as the post-sample value T3d.
[0056] The specific test results are shown in Tables 5 and 6.
[0057] Table 4 shows the extract yield.
[0058] Table 4
[0059] The test results of Examples 1 to 8 show that the preparation method of the present invention has a high yield, and the process conditions of Example 3 are the preferred process conditions, with an extract yield of 20.4%.
[0060] Comparing the test results of Example 3 with those of Comparative Examples 1-5, it can be seen that the extraction effect is better when using a combination of ultrasound-assisted extraction, amphiphilic crystalline copolymer compound dissolution, and supercritical fluid extraction, compared to extraction using any one or two of these techniques. This indicates that the three techniques have a synergistic effect.
[0061] A comparison of the test results of Example 3 and Comparative Example 1 shows that the amphiphilic crystalline copolymer used in this invention can significantly improve the extract yield.
[0062] A comparison of the test results of Example 3 and Comparative Examples 6-7 shows that when the ratio of the amphiphilic crystalline copolymer to Dendrobium nobile granules exceeds the range specified in this invention, the yield of the extract decreases.
[0063] Table 5 shows the initial and post-sample values for the experimental area. The Sig. value for normality testing is >0.050, indicating that the data follows a normal distribution. The t-test is used; otherwise, the non-parametric Wilcoxon test is used.
[0064] Table 5
[0065] Table 6 is a table showing the analysis of the discrepancies.
[0066] Table 6
[0067] 'a' refers to the p-value used in the intra-regional difference analysis of the initial value (T0d) and the test value (Txd) at each follow-up time. p < 0.050 indicates a significant difference in T0d between the time after sample use and the time before sample use; p ≥ 0.050 indicates no significant difference in T0d between the time after sample use and the time before sample use.
[0068] The test results from Examples 9-12 show that, compared with before use, the number of pimples and the skin a* value were significantly reduced after 3 days of using the samples from Examples 9-12. Figures 1-4 Image comparison analysis showed that the test sample improved acne, indicating that the sample has acne-removing effects and helps the skin recover after acne occurs.
[0069] Comparing the test results of Example 12 and Comparative Example 8, it can be seen that after using the sample of Comparative Example 8 for 3 days, compared with before the use, the number of pimples increased significantly by 2.00% (p>0.050), and the skin a* value decreased significantly by 2.09% (p>0.050). Figure 5 Image comparison analysis showed no improvement in acne, indicating that without the Dendrobium nobile extract prepared in this invention, the sample of Comparative Example 8 did not have acne-removing effects, and the sample of Comparative Example 8 did not help the skin recover after acne occurs.
[0070] Comparing the test results of Example 12 and Comparative Example 9, it can be seen that after using the sample of Comparative Example 9 for 3 days, compared with before the use, the number of pimples increased significantly by 2.33% (p>0.050), and the skin a* value decreased significantly by 6.64% (p<0.05). Figure 6 Image comparison analysis showed no improvement in acne, indicating that without the use of amphiphilic crystalline copolymers and supercritical extraction, the sample of Comparative Example 9 did not have acne-removing effects, but the sample helped the skin recover after acne occurred.
[0071] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.
[0072] It should also be noted that the various specific technical features described in the above embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.
[0073] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.
Claims
1. A method for extracting Dendrobium nobile, characterized in that, Includes the following steps: S1. Wash Dendrobium nobile and freeze it at -30 to -45°C. Then freeze-dry it under vacuum at 40 to 70 Pa and -50 to -60°C. After drying, pulverize it and pass it through a 10 to 50 mesh sieve to obtain Dendrobium nobile granules. S2. Grind the amphiphilic crystalline polymer to 100-150 mesh, and then mix it with Dendrobium nobile particles. The mass ratio of the amphiphilic crystalline polymer to Dendrobium nobile is 1:5-10 to obtain the first mixture. S3. The first mixture is immersed in an aqueous ethanol solution with a volume fraction of 30-50% and subjected to ultrasonic-assisted extraction. The ultrasonic extraction power is 200-500W, the extraction time is 45-60min, and the extraction temperature is 30-40℃ to obtain the second mixture. S4. The second mixture is subjected to supercritical carbon dioxide extraction at a temperature of 35–50°C, an extraction pressure of 20–35 MPa, and an extraction time of 30–120 min. After extraction, the mixture is crystallized under reduced pressure at 0.5–3 MPa / min to obtain the third mixture. S5. The third mixture is immersed in an aqueous ethanol solution with a volume fraction of 30-50% and then crystallized under reduced pressure of 0.5-3 MPa / min to obtain Dendrobium nobile extract.
2. The extraction method of Dendrobium nobile according to claim 1, characterized in that, The amphiphilic crystalline polymer includes any one of PEG-b-PCL, PEG-b-PLL, and APHBA-b-PEO.
3. A Dendrobium nobile extract prepared by the extraction method according to any one of claims 1 to 2.
4. A nursing composition, characterized in that, Includes the following components by weight percentage: The extract of Dendrobium nobile according to claim 3 comprises 0.05-5%; 0.1-10% humectant; 0.5-5% oil; 0.1-2% thickener; 1-5% emulsifier; 0.5-1% co-emulsifier; 0.03-1.5% preservative; 0.01-1.5% pH adjuster; and the balance being purified water.
5. The nursing composition according to claim 4, characterized in that, The moisturizer includes at least one of glycerin, propylene glycol, hyaluronic acid, ceramide, panthenol, and urea.
6. The nursing composition according to claim 4, characterized in that, The oils include at least one of polydimethylsiloxane, jojoba seed oil, deep-sea two-sectioned shepherd's purse seed oil, squalane, and shea butter.
7. The nursing composition according to claim 4, characterized in that, The emulsifiers include anionic emulsifiers, cationic emulsifiers, and nonionic emulsifiers.
8. The nursing composition according to claim 7, characterized in that, The emulsifier includes at least one of olive oil cetyl ester / sorbitan olive oil ester, glyceryl stearate / PEG-100 stearate, arachidonic alcohol / docosahexadecyl alcohol / eicosyl glucoside.
9. The nursing composition according to claim 4, characterized in that, The co-emulsifier includes at least one of cetearyl alcohol, cetyl alcohol, stearyl alcohol, stearic acid, and lauric acid.
10. The nursing composition according to claim 4, characterized in that, The thickener includes at least one of xanthan gum, carbomer polymer, cyanoethyl cellulose, sodium acrylate / sodium acryloyl dimethyl taurate copolymer, acrylic polymer, polyacrylamide / C13-14 isoalkane / lauryl polyoxyethylene ether, and sodium polyacrylate.
