Preparation method of snow chrysanthemum and lithospermum officinale traditional Chinese medicine lipstick with anti-inflammatory and repairing effects

Abstract

The present invention relates to a preparation method of a snow chrysanthemum and lithospermum herbal lipstick with anti-inflammatory and repairing effects. In view of the problems that the active ingredients of existing Chinese herbal lipsticks are easily degraded, easily broken at low temperatures, and have insufficient anti-inflammatory and repairing effects, the invention pioneers a freeze-crushing-supercritical extraction-microsphere self-assembly process: 1. Snow chrysanthemum, lithospermum, and roselle are quickly frozen in liquid nitrogen and then crushed by high-pressure microjet, combined with hexadecyltrimethylammonium bromide / supercritical CO2 extraction to improve the yield of shikonin; 2. The extract is injected into an olive oil carrier containing camel fat wax to self-assemble into core-shell microspheres, realizing lip temperature-triggered self-repair; 3. Cynomorium songaricum polysaccharide is added to react with salivary enzymes to form a bioadhesive film, and synergistically with licorice extract, sea buckthorn seed oil, etc. to improve the TNF-α inhibition rate. It is suitable for lip protection in extreme environments such as high cold, sandstorms, and strong ultraviolet rays on the plateau, filling the technical gap in the field of molecular-level sustained release and intelligent response repair of Chinese herbal lipstick.

Description

Technical Field

[0001] The invention belongs to the technical field of natural cosmetics, and in particular relates to a method for preparing a snow chrysanthemum and lithospermum traditional Chinese medicine lipstick with anti-inflammatory and repairing effects. Background Art

[0002] Lipstick, also known as lip balm or lip stick, makes lips rosy and shiny, moisturizes and protects lips, enhances facial beauty, and corrects lip contours. It is a must-have cosmetic for women. It comes in stick, pencil, and ointment forms, but the stick form is the most common.

[0003] Current Chinese herbal lipsticks suffer from three major drawbacks: First, the extraction process for the active ingredients is crude, such as in CN107625681A, resulting in insufficient anti-inflammatory efficacy. Second, the matrix is ​​poorly compatible; beeswax exhibits poor fracture resistance at sub-zero temperatures, making it unsuitable for use in high-altitude, cold regions. Third, their efficacy is limited. Existing products, such as CN201710187284.3, focus on cheilitis treatment but fail to address the synergistic effects of dust and UV damage. Market research shows that the incidence of cheilitis in arid and cold regions like the Inner Mongolia Autonomous Region is as high as 35%, creating an urgent need for multifunctional lipsticks that combine anti-inflammatory, repairing, and extreme environmental protection.

[0004] The closest document, CN107625681A (a moisturizing lipstick containing Chinese herbs), discloses a formula containing peach blossom extract and astragalus root, but its technical solution has significant shortcomings: ① The simple mixing of components results in a low transdermal absorption rate, far below the body's repair needs; ② Unmodified beeswax has a high breakage rate in low-temperature environments; ③ It lacks UV protection, and the SPF value decreases by >40% after 2 hours of use in plateau areas. Another document, CN201810909693.4, although using supercritical extraction, does not solve the problem of sustained release of active ingredients, and anthocyanin release is not effective. 1 / 2 The root cause of these shortcomings lies in the failure to systematically integrate the extraction, protection, and delivery of active ingredients in traditional Chinese medicine with the requirements for extreme environmental protection.

[0005] Based on the high cold (≤-40℃), strong ultraviolet (UVI≥10), sandstorm (PM 10 ≥500μg / m³) of regional characteristics, this invention breaks through the stereotype of simply compounding ingredients: 1. It pioneers liquid nitrogen freeze-fracture, combined with cetyltrimethylammonium bromide / supercritical CO₂ extraction, increasing the yield of shikonin from 75% to 92.3%; 2. It constructs thermosensitive core-shell microspheres, achieving self-healing properties through the copolymerization of camel tallow wax and snow chrysanthemum flavonoids; 3. It leverages the enzyme-responsive film-forming properties of Cynomorium songaricum polysaccharide to create a durable barrier with a moisture permeability of ≤15g / m²·h. These innovations make the product irreplaceable for specialized applications such as radiation cheilitis repair and border frostbite prevention. Summary of the Invention

[0006] A method for preparing a snow chrysanthemum and lithospermum officinale traditional Chinese medicine lipstick with anti-inflammatory and repairing effects, characterized in that, in parts by weight, it comprises the following steps:

[0007] (1) Raw material pretreatment: mix snow chrysanthemum, lithospermum officinale and roselle in a weight ratio of 1: (0.8-1.2): (0.8-1.2), take 10-30 weight parts and grind to 300-400 mesh;

[0008] (2) Freeze-crushing: The mixed powder after pulverization in step (1) is quickly frozen to below -150°C with liquid nitrogen and maintained for 3-10 minutes, and then crushed with high-pressure microfluidics at a pressure of 150-250 MPa for 2-5 cycles;

[0009] (3) Supercritical extraction: Place the crushed material from step (2) in a supercritical CO2 extraction kettle, continue to add hexadecyltrimethylammonium bromide at a concentration of 0.5-2% w / w, continue dynamic extraction at 35-45°C, 20-30 MPa, and continue with a circulation flow rate of 3 L / h for 1-3 hours. Collect the extract in a separation kettle;

[0010] (4) Microsphere self-assembly: The extract obtained in step (3) is injected into a 10-50 weight part olive oil carrier containing 3-12 weight parts of camel fat wax, wherein the weight ratio of camel fat wax to olive oil is 1:(2-6), and the reaction is continued at 40-50°C with stirring for 20-40 minutes to form "core-shell microspheres";

[0011] (5) Preparation of the final product: The core-shell microspheres prepared in the above step (4) are mixed with 5-15 parts by weight of licorice extract, 3-10 parts by weight of sea buckthorn seed oil, 2-6 parts by weight of Cynomorium songaricum polysaccharide, 2-6 parts by weight of vitamin E, 1-4 parts by weight of modified sodium montmorillonite, and 0.5-3 parts by weight of nano-titanium dioxide, and homogenized at 5000-10000 rpm for 3-10 minutes, and then injection molded. The mixture is then cooled gradually from 55-65°C to 35-45°C within 5-15 minutes, and then cooled to 5-15°C within 3-8 minutes. The mixture is then demoulded, sterilized, packaged, and sealed to obtain the snow chrysanthemum and lithospermum herbal lipstick with anti-inflammatory and repairing effects of the present invention.

[0012] The preparation method of the modified sodium montmorillonite is as follows:

[0013] S1. Raw material pretreatment: Sodium montmorillonite (cation exchange capacity ≥ 100 mmol / 100 g) was mixed with deionized water in a weight ratio of 1:10 and ultrasonically dispersed to obtain a suspension at an ultrasonic frequency of 40 kHz for 30 min.

[0014] S2. Ion exchange: Continue to add 5-8% of the mass of sodium montmorillonite aminosilane coupling agent KH-550 to S1, stir and react at 60°C for 2 hours;

[0015] S3. Organic modification: adding sweet almond oil and concentrated sulfuric acid; reflux reaction at 75±5°C for 3 hours, and centrifugation; wherein the weight ratio of sodium montmorillonite to sweet almond oil is 1:(0.5-0.8), and the weight of concentrated sulfuric acid is 0.05-0.1% of the weight of sweet almond oil;

[0016] S4. Post-processing: The product obtained by centrifugation in S3 was washed three times with anhydrous ethanol and three times with acetone respectively; dried under vacuum at 60°C, and then subjected to air flow milling.

[0017] The core-shell microspheres have the following structure: the core layer is a composite crystal formed by shikonin and roselle anthocyanin through π-π stacking; the shell layer is a copolymer of snow chrysanthemum flavonoids and camel fat wax combined through hydrophobic interaction.

[0018] The method for preparing the olive oil carrier containing camel fat wax in step (4) is as follows: heating camel fat wax and olive oil to 75±2° C., melting and stirring to obtain the carrier.

[0019] The gloss recovery rate is ≥90% within 30 minutes at a lip temperature of 32-36°C; the repair mechanism is the melting and flow of camel fat wax in the shell and the reorganization of hydrogen bonds of snow chrysanthemum flavonoids.

[0020] Anti-inflammatory: TNF-α inhibition rate in LPS-induced macrophage model ≥80%; Repair: 7-day lip chapped lip repair rate in human trials ≥85%; Sustained release: Anthocyanin release in vitro 1 / 2 ≥4 hours.

[0021] It can be used in the following scenarios: lip protection in high-altitude cold areas (≤-20℃); lip mucosal barrier repair in sandstorm weather (PM10≥500μg / m³); prevention of radiation damage from strong ultraviolet rays (UVI≥10) in plateaus.

[0022] After being placed in a -40℃ environment for 24 hours, the breaking force is ≥700g; under the ultraviolet intensity of 3000m above sea level, the SPF value is ≥15.

[0023] After contacting the lips, Cynomorium songaricum polysaccharide reacts with salivary amylase to form a bioadhesive gel film with a moisture permeability of ≤15g / m²·h, which can continuously release active ingredients for 6-8 hours.

[0024] -40℃ freezing test: no cracking after 20 freeze-thaw cycles; dust simulation test: PM 2.5 Adsorption rate ≥90%; Plateau UV test: SPF value attenuation rate ≤10%.

[0025] It can be used in the following fields: protection and repair of radiation cheilitis in cancer patients; prevention of lip frostbite in border guards in high-altitude cold areas; and dust barrier for lips during desert scientific expeditions.

[0026] In the present invention, the herbal base materials are snow chrysanthemum, lithospermum officinale and roselle; the oil carriers are camel tallow wax and olive oil; and the functional additives are six ingredients including roasted licorice root / sea buckthorn seed oil.

[0027] Beneficial technical effects of the present invention:

[0028] The present invention uses a freeze-crushing-supercritical extraction process to retain the active ingredients of Chinese herbal medicine to the greatest extent. The core-shell microspheres constructed can achieve self-repair under the triggering of lip temperature. The bioadhesive film formed by the reaction of Cynomorium songaricum polysaccharide and salivary enzymes can continuously release the active ingredients for 6-8 hours. 1 / 2 The product has a breaking strength of 825g at -40℃, no cracking after 20 freeze-thaw cycles, and maintains an SPF value of 18.7 in plateau UV environments, with an attenuation rate of ≤5%. 2.5 The product boasts a 93.7% absorption rate. Clinical testing has shown a 91.3% chapped lip repair rate within 7 days, an 86.7% TNF-α inhibition rate, and a >99% sterilization rate against Escherichia coli and Staphylococcus aureus. Sensory evaluations indicate a moisturizing rating of 4.8 out of 5. Accelerated stability testing revealed no oil content after three months, surpassing existing herbal lipstick performance. DETAILED DESCRIPTION

[0029] Before further describing the specific embodiments of the present invention, it should be understood that the scope of the present invention is not limited to the specific embodiments described below. It should also be understood that the terminology used in the examples is intended to describe specific embodiments and is not intended to limit the scope of the present invention. The experimental procedures in the following examples, where specific conditions are not specified, were generally performed under conventional conditions or according to the conditions recommended by the respective manufacturers.

[0030] When the embodiments provide numerical ranges, it should be understood that, unless otherwise specified in the present invention, both endpoints of each numerical range and any numerical value between the two endpoints may be selected. Unless otherwise defined, all technical and scientific terms used in the present invention have the same meaning as those generally understood by those skilled in the art. In addition to the specific methods, equipment, and materials used in the embodiments, according to the prior art mastery and the description of the present invention by those skilled in the art, any methods, equipment, and materials of the prior art similar or identical to the methods, equipment, and materials described in the embodiments of the present invention may also be used to implement the present invention.

[0031] Unless otherwise specified, the test methods, detection methods, and preparation methods disclosed in the present invention all adopt conventional techniques in this technical field.

[0032] Related raw material sources:

[0033] Snow chrysanthemum, harvested at the bud stage, with a moisture content of ≤8%, sourced from an organic planting base in Alxa League, Inner Mongolia Autonomous Region. Its main function is to protect against UV damage.

[0034] Lithospermum officinale, shikonin content ≥ 2.5% (HPLC), sourced from Lithospermum officinale planting cooperative in Chengde, Hebei Province, and its main function is to repair inflammation.

[0035] Roselle, anthocyanin ≥15mg / g, sourced from the Qujing Plateau planting base in Yunnan, primarily functions as a natural pigment and antioxidant.

[0036] Roasted licorice root, glycyrrhizic acid ≥8.0%, sourced from the Longxi Traditional Chinese Medicine Market in Gansu Province (batch number 2023-GS), has the main effect of synergistic anti-inflammatory and synergistic effects;

[0037] Sea buckthorn seed oil, palmitoleic acid (C16:1) ≥28%, sourced from Jiangxi Wanhua Spice Co., Ltd. (item number WH-2305), primarily used for mucosal repair and low-temperature moisturizing.

[0038] Cynomorium songaricum polysaccharide, polysaccharide content ≥85%, viscosity 500-800mPa·s, sourced from Bayannur Mongolian Medicine Resource Center, Inner Mongolia Autonomous Region, mainly functions as an enzyme-responsive film-forming material;

[0039] Olive oil acid value ≤ 0.5mg KOH / gLa Tourangelle (LAT-00570), mainly acts as base oil and microsphere carrier;

[0040] Camel tallow wax, acid value ≤1mg KOH / g, saponification value 90-110, sourced from Xinjiang Camel Industry Group (XJLT-2023), mainly functions as a low-temperature ductile matrix;

[0041] Vitamin E, d-α-tocopherol content ≥96%, sourced from Zhejiang NHU Co., Ltd. (NH-VE99), primarily acts as an antioxidant stabilizer;

[0042] Sodium montmorillonite, cation exchange capacity ≥100 mmol / 100 g, particle size D50 = 3 μm, sourced from Zhejiang Fenghong New Materials Co., Ltd. (FH-LS), mainly used as a modified adsorbent carrier;

[0043] Sweet almond oil, iodine value 100-110gI2 / 100g, sourced from Jiangxi Wanhua Spice Co., Ltd. (WH-8007), mainly used as a sodium montmorillonite modifier;

[0044] Nano-titanium dioxide, rutile type, particle size 30-50nm, Evonik, Germany (Aeroxide® TiO2 P25), mainly functions as a physical sunscreen enhancer;

[0045] Aminosilane KH-550, purity ≥98%, sourced from Nanjing Shuguang Chemical Group Co., Ltd. (SG-KH550), primarily acts as a surface modifier for sodium montmorillonite;

[0046] Hexadecyltrimethylammonium bromide, biochemical reagent grade, ≥99%, sourced from Shanghai MacLean Chemical Reagent Co., Ltd. (C805989), primarily used as a phase transfer extraction catalyst;

[0047] Test standards for the present invention:

[0048] 1. Anti-inflammatory test: TNF-α inhibition rate

[0049] Test standard: ISO 10993-5 Medical device cytotoxicity test

[0050] Key parameters: Positive control: dexamethasone (10 μM); Sample concentration gradient: 0.1%, 0.5%, 1.0% (w / v)

[0051] Data requirements: Repeat 3 times, take the 1.0% concentration group data

[0052] 2. Repairability test: chapped lip repair rate

[0053] Test standard: GB / T 26528-2011 Guidelines for the evaluation of moisturizing efficacy of cosmetics

[0054] Specific process:

[0055] (1) Subject selection: Volunteers from Inner Mongolia Autonomous Region (n = 50, living in a -15°C environment); lip chappedness score ≥ 3 (0-5 scale).

[0056] (2) Test process: On day 0, take photos and record clinical scores; on days 1-7, apply 0.1g of the product every morning and evening; on day 7, re-evaluate (double-blind method by the same physician).

[0057] (3) Repair rate = (initial score - 7-day score) / initial score × 100%.

[0058] 3. Sustained release test: anthocyanin t 1 / 2

[0059] Test standard: 2020 edition of the Chinese Pharmacopoeia, Part IV, 0931 Release Determination Method;

[0060] Specific process: Franz diffusion cell was placed in a 37°C circulating water bath and continued to receive PBS + 0.5% Tween 80. Sampling points were 0.5, 1, 2, 4, 6, and 8 hours. Anthocyanin was detected by HPLC, and the cumulative release rate was calculated. The zero-order kinetics was fitted to obtain t 1 / 2

[0061] Parameter settings: diffusion area: 1.77 cm²; receiving liquid volume: 7 mL; anthocyanin detection wavelength: 520 nm.

[0062] 4. Low temperature performance test: -40℃ breaking strength

[0063] Test standard: GB / T 26528-2011 Lip cosmetics physical and chemical performance test

[0064] Instrument: CT3 Texture Analyzer (Brookfield)

[0065] Specific process: (1) Sample preparation: 12mm diameter lipstick cylinder; (2) Pretreatment: Place in a -40℃ constant temperature oven for 24 hours; (3) Test parameters: Probe TA3 / 100, test speed 0.5mm / s, trigger force 5g, deformation 2mm. (4) Result calculation: Breaking force = peak force value.

[0066] 5. Sun protection performance test: SPF value

[0067] Test standard: ISO 24444:2019 Evaluation of sunscreen efficacy of cosmetics

[0068] Specific process:

[0069] In vitro method (prescreening): UV-2000S UV transilluminator; sample thickness: 0.02 mm; calculation: SPF = CF × ΣEE(λ) × I(λ) × Abs(λ)

[0070] Plateau Verification: Location: Nagqu, Tibet Autonomous Region (4500m above sea level, UVI=11-13); Test duration: 4 hours of outdoor exposure.

[0071] 6. Self-repair test: gloss recovery rate

[0072] Test standard: ASTM D523-14 Specular gloss determination

[0073] Instrument: Micro scratch tester + gloss meter

[0074] Specific process: (1) Preparation: Polishing the lipstick surface (initial glossiness Gu ≥ 80); (2) Damage: Scratching with 2000 grit sandpaper (glossiness after damage Gd ≤ 30); (3) Repair: Place on a 32°C constant temperature table for 30 minutes; (4) Testing: Recovery rate = (Gr-Gd) / (Gu-Gd) × 100% (Gr is the glossiness after repair)

[0075] 7. Dust protection test: PM 2.5 Adsorption rate

[0076] Test standard: GB / T 35237-2017 Dust environment simulation test

[0077] Key Control: PM 2.5 Source: ISO 12103-1 A2 fine dust; Temperature and humidity: 25°C / 30%RH.

[0078] 8. Cold resistance test: -40℃ freeze-thaw cycle

[0079] Test standard: ASTM D6662-06 Plastics Freeze-Thaw Resistance Test

[0080] Improved method: freezing stage, -40℃, 4 hours; thawing stage, 25℃, 4 hours.

[0081] Evaluation method: Macro: 20x magnifying glass to observe cracks; Micro: SEM scanning cross-sectional morphology; Function: repair rate test.

[0082] 9. Clinical special application test

[0083] (1) Protection against radiation cheilitis

[0084] Standard: CTCAE v5.0 Adverse Event Evaluation Criteria

[0085] Experimental design: Grouping: experimental group and control group; the number of experimental cases (people) is 30; intervention plan: experimental group, apply 4 times a day (during radiotherapy), control group, vaseline matrix.

[0086] (2) Prevention of frostbite in plateau

[0087] Test location: Ali Military Sub-district, Tibet Autonomous Region (4500m above sea level)

[0088] Monitoring indicators: lip temperature changes (infrared thermal imaging); transepidermal water loss (Tewameter TM300); frostbite incidence.

[0089] Example 1

[0090] A method for preparing a traditional Chinese medicine lipstick of snow chrysanthemum and lithospermum with anti-inflammatory and repairing effects comprises the following steps, calculated by weight:

[0091] (1) Raw material pretreatment: Mix snow chrysanthemum, lithospermum officinale, and roselle in a weight ratio of 1:1:1, and grind 20 parts by weight of the total of the three into 350 mesh;

[0092] (2) Freeze-crushing: The mixed powder after pulverization in step (1) was quickly frozen to -196°C with liquid nitrogen and maintained for 5 minutes, and then crushed with high-pressure microfluidics at a pressure of 200 MPa for 3 cycles;

[0093] (3) Supercritical extraction: The crushed material from step (2) was placed in a supercritical CO2 extraction kettle, and hexadecyltrimethylammonium bromide at a concentration of 1.0% w / w was added. Dynamic extraction was continued at 40°C, 20 MPa, and a circulation flow rate of 3 L / h for 2 hours. The extract was collected in a separation kettle.

[0094] (4) Microsphere self-assembly: The extract obtained in step (3) was injected into 32 parts by weight of an olive oil carrier containing 8 parts by weight of camel fat wax, wherein the weight ratio of camel fat wax to olive oil was 1:4, and the reaction was continued at 45°C with stirring for 30 minutes to form "core-shell microspheres";

[0095] (5) Preparation of the final product: The core-shell microspheres prepared in step (4) above were mixed with 10 parts by weight of licorice extract, 6 parts by weight of seabuckthorn seed oil, 4 parts by weight of Cynomorium songaricum polysaccharide, 4 parts by weight of vitamin E, 2.5 parts by weight of modified sodium montmorillonite, and 1.5 parts by weight of nano-titanium dioxide, and homogenized at 8000 rpm for 10 minutes, and then injection molded. The mixture was then cooled in a gradient manner from 60°C to 40°C within 10 minutes, and then cooled to 10°C within 5 minutes. The mixture was then demoulded, sterilized, packaged, and sealed to obtain the snow chrysanthemum and lithospermum herbal lipstick with anti-inflammatory and repairing effects as described in the present invention.

[0096] The preparation process of the modified sodium montmorillonite is as follows:

[0097] S1. Mix 100 g of sodium montmorillonite with 1000 g of deionized water and sonicate at 40 kHz for 30 min.

[0098] S2. Continue to add 6 g of KH-550 to the above S1, stir at 500 rpm for 2 h at 60 ° C, and finally centrifuge;

[0099] S3. The solid obtained by centrifugation in step S2 was added to the reactor, and then 60 g of sweet almond oil and 0.05 g of 0.08% concentrated sulfuric acid were added. The mixture was refluxed at 75 ° C for 3 hours, centrifuged, and washed three times with anhydrous ethanol, and then washed three times with acetone.

[0100] S4. The solid obtained by centrifugation and washing in S3 is dried under vacuum at 60°C for 24 hours and then subjected to air flow pulverization to obtain the modified sodium-montmorillonite.

[0101] The carrier liquid is prepared by mixing camel tallow wax and olive oil, heating the mixture to 75° C., melting the mixture, and stirring the mixture to form the carrier liquid.

[0102] Example 2

[0103] The difference between Example 2 and Example 1 is that:

[0104] 1. Herbal base: Snow Chrysanthemum: Lithospermum: Roselle = 1:1.2:0.8, total weight 25 parts;

[0105] 2. Modified sodium montmorillonite: sodium montmorillonite: sweet almond oil = 1:0.7, wherein the amount of concentrated sulfuric acid is 0.1% by weight of sweet almond oil, and the concentration of concentrated sulfuric acid is the same as that in Example 1;

[0106] 3. Add the following to the final product: 12 parts by weight of licorice extract, 5 parts by weight of seabuckthorn seed oil, 3 parts by weight of Cynomorium songaricum polysaccharide, 5 parts by weight of vitamin E, 3 parts by weight of modified sodium montmorillonite, and 1 part by weight of nano-titanium dioxide.

[0107] Camel fat wax is 10 parts by weight, olive oil is 40 parts by weight, and step (4) is stirring at 42°C for 35 minutes;

[0108] Example 3

[0109] The difference between Example 3 and Example 1 is that:

[0110] 1. Herbal base: Snow Chrysanthemum: Lithospermum: Roselle = 1:0.8:1.2, total weight 15 parts;

[0111] 2. Modified sodium montmorillonite: sodium montmorillonite: sweet almond oil = 1:0.5, wherein the amount of concentrated sulfuric acid is 0.05% by weight of the sweet almond oil, and the concentration of concentrated sulfuric acid is consistent with that in Example 1;

[0112] 3. Add the following to the final product: 8 parts by weight of licorice extract, 8 parts by weight of seabuckthorn seed oil, 5 parts by weight of Cynomorium songaricum polysaccharide, 3 parts by weight of vitamin E, 2 parts by weight of modified sodium montmorillonite, and 2 parts by weight of nano-titanium dioxide.

[0113] Camel fat wax is 6 parts by weight, olive oil is 30 parts by weight, and step (4) is stirring at 48°C for 25 minutes;

[0114] Comparative Example 1

[0115] The difference between Comparative Example 1 and Example 1 is that liquid nitrogen crushing is omitted and room temperature crushing is used instead.

[0116] Comparative Example 2

[0117] The difference between Comparative Example 2 and Example 1 is that camel fat wax is replaced by beeswax.

[0118] Comparative Example 3

[0119] The difference between Comparative Example 3 and Example 1 is that Cynomorium songaricum polysaccharide is deleted.

[0120] Comparative Example 4

[0121] The difference between Comparative Example 4 and Example 1 is that no hexadecyltrimethylammonium bromide was added (supercritical extraction)

[0122] Comparative Example 5

[0123] The difference between Comparative Example 5 and Example 1 is that the sodium montmorillonite used is unmodified.

[0124] Comparative Example 6

[0125] Commercially available product, a major brand of Chinese herbal lipstick.

[0126] Test items

[0127] Table 1 Test results of the embodiments of the present invention, comparative examples and a certain brand of Chinese herbal lipstick on the market

[0128] Test items Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Shikonin retention rate (%) 92.3 88.7 85.7 68.5 78.2 81.0 71.8 75.4 73.9 -40℃ breaking strength (g) 825 845 750 710 480 (fracture) 731 696 501 520 TNF-α inhibition rate (%) 86.7 88.2 79.3 69.2 77.3 75.2 69.5 62.1 70.1 <![CDATA[Anthocyanin t 1 / 2 (h)]]> 7.2 6.8 7.5 3.1 4.2 2.3 3.8 2.9 3.5 <![CDATA[PM 2.5 Adsorption rate (%)]]> 93.7 88.1 94.2 84.9 82.1 41.5 70.3 35.2 40.3 Moisturizing degree (5 points) 4.8 4.6 4.9 3.2 3.3 3.1 3.5 3.5 3.4 Escherichia coli sterilization rate (%) 99.3 98.7 98.1 93.2 96.5 95.8 92.7 89.5 96.1 SPF value (3000m above sea level) 18.7 17.9 18.2 14.3 15.5 14.8 13.1 12.5 15.3 Gloss recovery rate (%) 94.5 92.8 95.1 81.3 84.1 68.7 80.5 52.3 83.3 Lip chapped repair rate (7 days, %) 91.3 84.7 87.5 78.2 80.5 71.1 72.6 67.8 80.2

[0129] Analysis of Table 1 above and comparison with Examples 1-3 show that the possible reasons for the performance differences in the above test items are: Example 1 uses an equal ratio of snow chrysanthemum, comfrey, and roselle (1:1:1) and a wax oil balanced carrier (1:4) to achieve optimal synergy between the active ingredient release rate and matrix performance: snow chrysanthemum flavonoids enhance the photostability of shikonin, roselle anthocyanins provide long-lasting color development, and the copolymer shell formed by camel fat wax and olive oil in a ratio of 1:4 maintains flexibility at low temperatures (anti-breaking at -40°C) while allowing the active ingredient to penetrate the skin efficiently. Example 2 increased the lithospermum ratio (1:1.2:0.8) and the wax content (wax:oil = 1:4), enhancing the anti-inflammatory pathway (enhanced TLR4 inhibition) through the increased shikonin concentration, but the high wax content slightly reduced moisturizing properties. In contrast, Example 3 increased the oil content in the carrier (wax:oil = 1:5), but reduced the total carrier volume to 36 parts. This increased the anthocyanin-shikonin π-π stacking density and improved color stability. The high oil content promoted the release of fat-soluble components, bringing moisturizing properties to a peak, but the reduced wax ratio resulted in slightly weaker low-temperature fracture resistance than in Example 2. The differences between the three methods essentially result from the coordinated regulation of the targeted ratio of the active ingredients and the rheological properties of the carrier.

[0130] Comparing Example 1 with Comparative Examples 1-5, we analyzed the possible causes of the performance differences in the above-mentioned test items: A comparison of Example 1 and Comparative Example 1 revealed that the lack of liquid nitrogen cryoprotection in Comparative Example 1 resulted in oxidative degradation of heat-sensitive components (shikonin and anthocyanins) during the fragmentation stage. Furthermore, insufficient cell wall fragmentation reduced extraction efficiency. Furthermore, enzyme activity was not inhibited at room temperature, leading to hydrolysis of some polysaccharides, ultimately resulting in decreased activity retention and weakened sustained-release properties. Microscopic manifestations of this were the presence of unbroken cell clumps in the extract and the detection of shikonin degradation products by HPLC.

[0131] Comparative analysis of Example 1 and Comparative Example 2 shows that the long-chain alkanes (C25-C31) in beeswax form a rigid crystalline network, generating stress concentration points at low temperatures, while the short-chain fatty acids (C16-C18) in camel fat wax have lower crystallinity. The beeswax matrix undergoes brittle fracture at -40°C, and its hydrophobicity is poorly compatible with snow chrysanthemum flavonoids, resulting in insufficient density of the microsphere shell and PM 2.5 The adsorption rate decreased.

[0132] Comparative analysis of Example 1 and Comparative Example 3 shows that the lack of Cynomorium songaricum polysaccharide in Comparative Example 3 makes it impossible for salivary amylase to trigger enzyme response cross-linking and form a bioadhesive gel film, resulting in rapid release of active ingredients (anthocyanidins t 1 / 2 The lack of a membrane barrier exacerbates transepidermal water loss. A paste lacking Cynomorium songaricum polysaccharide is distributed discretely on the lips and fails to form a continuous film.

[0133] A comparison of Example 1 and Comparative Example 4 reveals that the absence of cetyltrimethylammonium bromide as a phase transfer catalyst prevents supercritical CO2 from effectively extracting water-soluble flavonoids and fat-soluble naphthoquinones. Shikonin, which fails to form an ion pair with cetyltrimethylammonium bromide, remains in the plant residue, reducing the extraction yield. Furthermore, anthocyanins, lacking micellar encapsulation by cetyltrimethylammonium bromide, aggregate during subsequent self-assembly, resulting in uneven particle size distribution and reduced transdermal efficiency.

[0134] Comparative analysis of Example 1 and Comparative Example 5 shows that the unmodified sodium montmorillonite is hydrophilic and cannot effectively adsorb hydrophobic PM. 2.5 The interlayer channels of the modified clay are not expanded by sweet almond oil, resulting in a surface area only one-third that of the modified clay, significantly reducing its heavy metal adsorption capacity. In dust simulation tests, the adsorption rate of unmodified sodium montmorillonite was less than 50% due to electrostatic repulsion between the surface hydroxyl groups and the dust.

[0135] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a Chinese herbal lipstick of snow chrysanthemum and lithospermum with anti-inflammatory and repairing effects, characterized in that: Calculated by weight, comprising the following steps: (1) Raw material pretreatment: mix snow chrysanthemum, lithospermum officinale, and roselle in a weight ratio of 1:0.8-1.2:0.8-1.2, and grind 10-30 parts by weight of the total amount of the three into 300-400 mesh; (2) Freeze-crushing: The mixed powder after pulverization in step (1) is quickly frozen to below -150°C with liquid nitrogen and maintained for 3-10 minutes, and then crushed with high-pressure microfluidics at a pressure of 150-250 MPa for 2-5 cycles; (3) Supercritical extraction: Place the crushed material from step (2) in a supercritical CO2 extraction kettle, continue to add hexadecyltrimethylammonium bromide at a concentration of 0.5-2% w / w, continue dynamic extraction at 35-45°C, 20-30 MPa, and continue with a circulation flow rate of 3 L / h for 1-3 hours. Collect the extract in a separation kettle; (4) Microsphere self-assembly: The extract obtained in step (3) is injected into a carrier containing 10-50 parts by weight of olive oil containing 3-12 parts by weight of camel tallow wax, wherein the weight ratio of camel tallow wax to olive oil is 1:2-6, and the reaction is continued at 40-50°C with stirring for 20-40 minutes to form core-shell microspheres; (5) Preparation of the final product: the core-shell microspheres prepared in the above step (4) are mixed with 5-15 parts by weight of licorice extract, 3-10 parts by weight of sea buckthorn seed oil, 2-6 parts by weight of Cynomorium songaricum polysaccharide, 2-6 parts by weight of vitamin E, 1-4 parts by weight of modified sodium montmorillonite, and 0.5-3 parts by weight of nano-titanium dioxide, and homogenized at 5000-10000 rpm for 3-10 minutes, and then injection molded. The mixture is then cooled in a gradient manner, and the temperature is lowered from 55-65°C to 35-45°C within 5-15 minutes, and then cooled to 5-15°C within 3-8 minutes. The mixture is then demoulded, sterilized, packaged, and sealed to obtain the snow chrysanthemum and lithospermum herbal lipstick with anti-inflammatory and repairing effects. The preparation method of the modified sodium montmorillonite is as follows: S1. Raw material pretreatment: sodium montmorillonite and deionized water were mixed in a ratio of 1:10 parts by weight and ultrasonically dispersed to obtain a suspension at an ultrasonic frequency of 40 kHz for 30 min; the cation exchange capacity of the sodium montmorillonite was ≥100 mmol / 100 g; S2. Ion exchange: Continue to add 5-8% of the mass of sodium montmorillonite aminosilane coupling agent KH-550 to S1, stir and react at 60°C for 2 hours; S3. Organic modification: adding sweet almond oil and concentrated sulfuric acid; reflux reaction at 75±5°C for 3 hours, centrifugation; wherein the weight ratio of sodium montmorillonite to sweet almond oil is 1:0.5-0.8, and the weight of concentrated sulfuric acid is 0.05-0.1% by weight of sweet almond oil; S4. Post-processing: The product obtained by centrifugation in S3 was washed three times with anhydrous ethanol and three times with acetone respectively; dried under vacuum at 60°C, and then subjected to air flow milling.

2. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The core-shell microspheres have the following structure: the core layer is a composite crystal formed by shikonin and roselle anthocyanin through π-π stacking; the shell layer is a copolymer of snow chrysanthemum flavonoids and camel fat wax bound by hydrophobic forces.

3. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The method for preparing the olive oil carrier containing camel fat wax in step (4) is as follows: heating camel fat wax and olive oil to 75±2° C., melting and stirring to obtain the carrier.

4. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared according to this method has the following characteristics: the gloss recovery rate is ≥90% within 30 minutes at a lip temperature of 32-36°C; the repair mechanism is the melting flow of camel fat wax in the shell layer and the reorganization of the hydrogen bonds of snow chrysanthemum flavonoids.

5. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared by this method has the following properties: anti-inflammatory: TNF-α inhibition rate in LPS-induced macrophage model ≥80%; repairability: lip chapped lip repair rate ≥85% in human test after 7 days; sustained release: anthocyanin release in vitro 1 / 2 ≥4 hours.

6. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared according to this method can be used in the following scenarios: lip protection in high-altitude cold areas with an ambient temperature of ≤-20°C; repairing the lip mucosal barrier in sandstorm weather with PM10 ≥500μg / m³; and preventing damage from strong ultraviolet radiation in plateaus with UVI ≥10.

7. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared by this method has the following characteristics: after being placed in an environment of -40°C for 24 hours, the breaking force is ≥700g; and the SPF value is ≥15 under the ultraviolet intensity at an altitude of 3000m.

8. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared by this method has the following characteristics: after contacting the lips, Cynomorium songaricum polysaccharide reacts with salivary amylase to form a bioadhesive gel film with a moisture permeability of ≤15g / m²·h, and can continuously release active ingredients for 6-8 hours.

9. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared by this method has the following characteristics: -40℃ freezing test: no cracking after 20 freeze-thaw cycles; dust simulation test: PM 2.5 Adsorption rate ≥90%; Plateau UV test: SPF value attenuation rate ≤10%.

10. The method for preparing the snow chrysanthemum and lithospermum erythrorhizon Chinese medicinal lipstick with anti-inflammatory and repairing effects according to claim 1, characterized in that: The lipstick prepared by this method can be used in the following fields: as a lip dust barrier in desert scientific research operations.