A ginseng moxibustion stick with anti-fatigue effect and its preparation method

By introducing ingredients such as ginseng extract, schisandrin B, modified chitosan, and modified silk fibroin into moxibustion sticks, the problem of insufficient anti-fatigue and antibacterial properties of existing moxibustion sticks has been solved, achieving better effects in relieving fatigue and reducing the risk of infection.

CN120501844BActive Publication Date: 2025-12-02ZHONGJIXIANG (JILIN) BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510991518.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-07-18
Publication Date
2025-12-02
Estimated Expiration
2045-07-18

AI Technical Summary

Technical Problem

Existing moxibustion sticks are not targeted enough in relieving fatigue and regulating sub-health conditions, and their antibacterial properties need to be improved.

Method used

Using ginseng extract, schisandrin B, modified chitosan, and modified silk fibroin, ginseng moxibustion strips with anti-fatigue effects are prepared by modifying these components to improve drug loading efficiency and antibacterial properties.

Benefits of technology

It enhances the anti-fatigue and antibacterial effects, prolongs the duration of efficacy, reduces the risk of skin infection, and strengthens the targetedness and safety of moxibustion therapy.

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Abstract

This invention relates to the field of moxibustion stick preparation technology, and discloses a ginseng moxibustion stick with anti-fatigue effect and its preparation method. The preparation method is as follows: Moxa wool is passed through an 80-mesh sieve to remove coarse particles. Then, it is mixed with ginseng extract, schisandrin B, modified chitosan, modified silk fibroin, and glycerin in a three-dimensional mixer for 30-40 minutes. Finally, musk is added, and stirring is continued for 15-20 minutes. After standing and aging for 1-2 hours, an automatic molding machine is used to press the moxibustion stick into a diameter of 1.8 cm and a length of 20 cm using a pressure of 80-100 MPa for 5-10 seconds. The density is controlled to be 0.8-1.0 g / cm³. 3 The ginseng moxa sticks are dried in hot air at 35-45℃ for 4-5 hours, then equilibrated in an environment with 50% humidity for 45-50 hours, and finally vacuum dried to obtain ginseng moxa sticks with anti-fatigue effects. These moxa sticks possess anti-fatigue properties and good antibacterial activity.
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Description

Technical Field

[0001] This application relates to the field of moxibustion stick preparation technology, and more specifically, it relates to a ginseng moxibustion stick with anti-fatigue effect and its preparation method. Background Technology

[0002] Moxibustion is an important component of traditional Chinese medicine. It involves applying the warmth generated by burning moxa wool to acupoints on the body to warm the meridians, regulate qi and blood, and strengthen the body's resistance to pathogens. While existing moxa sticks are easy to use and have reliable effects, their function is relatively limited, relying primarily on the heat effect. Their effectiveness in relieving fatigue and regulating sub-health conditions is gradually becoming insufficient. Therefore, avoiding this limitation is key to solving the problem.

[0003] For example, patent CN118873482A discloses an aromatic moxibustion stick and its preparation method, which is made from the following ingredients: 200 parts of mugwort leaves, 5-10 parts of agarwood, 5-10 parts of costus root, 2-5 parts of myrrh, 5-10 parts of frankincense, 5-10 parts of nard, 5-10 parts of cinnamon twig, 2-5 parts of peppermint, 2-5 parts of fennel, 2-5 parts of angelica, 2-5 parts of licorice, 2-5 parts of sandalwood, and 2-5 parts of salvia miltiorrhiza. The aromatic moxibustion stick prepared by this invention produces smoke with an aromatic odor that is not pungent, and can effectively reduce the content of harmful gases and tar in the smoke. It is green and safe, and more environmentally friendly. However, it lacks anti-fatigue effects, and its antibacterial properties need to be improved.

[0004] Based on the above statements, the present invention provides a ginseng moxibustion stick with anti-fatigue effect and its preparation method. Summary of the Invention

[0005] In order to prepare ginseng moxibustion strips with antibacterial and anti-fatigue properties, this application provides a ginseng moxibustion strip with anti-fatigue effects and its preparation method.

[0006] This application provides a ginseng moxibustion stick with anti-fatigue effect and its preparation method, adopting the following technical solution: A ginseng moxibustion stick with anti-fatigue effect comprises the following weight components: 45-50 parts by weight of moxa wool, 8-12 parts by weight of ginseng extract, 5-10 parts by weight of schisandrin B, 3-5 parts by weight of modified chitosan, 2-4 parts by weight of modified silk fibroin, 0.2-0.3 parts by weight of musk, and 1-3 parts by weight of glycerin;

[0007] Among them, modified chitosan is obtained by modifying chitosan with epoxy quaternary ammonium salt;

[0008] Modified silk fibroin is obtained by modifying mercapto-modified silk fibroin with methacryloyloxyethyltrimethylammonium chloride and tea polyphenols.

[0009] Further, the modified chitosan is prepared by: swelling chitosan in acetic acid solution for 1-2 hours, then adding 2,3-epoxypropyltrimethylammonium chloride, stirring and mixing, then adding dilute hydrochloric acid, reacting for 10-12 hours, and after the reaction is completed, filtering, washing, and drying to obtain modified chitosan.

[0010] In the above reaction process, by swelling chitosan in a weakly acidic environment, the amino groups on the chitosan molecular weight are protonated to -NH3. + The swelling process causes the chitosan molecular chains to stretch, forming a viscous solution and exposing more reaction sites. Subsequently, it is mixed with an epoxy quaternary ammonium salt. The protonated amino groups of chitosan act as nucleophiles to attack the epoxy groups, leading to ring opening and the formation of CN covalent bonds, which connect the quaternary ammonium groups to the chitosan backbone, thus preparing modified chitosan.

[0011] Furthermore, the ratio of chitosan, acetic acid solution, 2,3-epoxypropyltrimethylammonium chloride, and dilute hydrochloric acid is 2.12-2.16g:22-25mL:2.03-2.08g:0.4-0.5mL.

[0012] Furthermore, the reaction temperature is 70-80℃.

[0013] Furthermore, the method for preparing the modified silk fibroin is as follows:

[0014] Step 1: At 0-4℃, thiolized silk fibroin was swollen in deionized water for 1-2 hours and dialyzed for 50-70 hours. Then, methacryloyloxyethyltrimethylammonium chloride and ammonium persulfate were added and stirred. The mixture was reacted at 30-50℃ for 18-22 hours. After the reaction was completed, the pH was adjusted to 7.0-8.0, dialyzed, centrifuged, and dried to obtain intermediate 1.

[0015] Step 2: Add intermediate 1 and tea polyphenols to the reactor, stir and mix, add p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, and react at 45-60℃ for 16-24 hours. After the reaction is completed, cool, dialyze, concentrate, and dry to obtain modified silk fibroin.

[0016] In the above reaction process, the thiolized silk fibroin is fully swollen in water at low temperature to expose the active thiol and hydroxyl groups in the molecular chain, providing active sites for subsequent reactions. The methacryloyloxyethyltrimethylammonium chloride free radical reacts with the thiol and hydroxyl groups of the thiolized silk fibroin to form covalent bonds through thiol-alkene click chemistry or free radical transfer mechanism, generating graft copolymers. Subsequently, under the catalysis of p-toluenesulfonic acid, the phenolic hydroxyl groups of tea polyphenols can undergo a condensation reaction with the amino group of intermediate 1 to form phenol-amine bonds, thus preparing modified silk fibroin.

[0017] Furthermore, in step one, the ratio of mercapto-modified silk fibroin, deionized water, methacryloyloxyethyltrimethylammonium chloride, and ammonium persulfate is 3.12-3.16g: 28-32mL: 2.53-2.58g: 0.1-0.12g.

[0018] Furthermore, in step two, the ratio of intermediate 1, tea polyphenols, and p-toluenesulfonic acid is 3.61-3.65g: 4.12-4.17g: 0.08-0.09g.

[0019] Furthermore, the dialysis time in step one is 36-48 hours, and the dialysis time in step two is 12-24 hours.

[0020] Furthermore, during the molding process, the pressure is set to 80-100 MPa, the holding pressure is maintained for 5-10 seconds, and the density is controlled to be 0.8-1.0 g / cm³. 3 .

[0021] The preparation method of the above-mentioned ginseng moxibustion sticks with anti-fatigue effects specifically includes the following steps:

[0022] The moxa wool is sieved to remove coarse particles, and then mixed with ginseng extract, schisandrin B, modified chitosan, modified silk fibroin, and glycerin in a three-dimensional mixer for 30-40 minutes. Finally, musk is added, and the mixture is stirred for another 15-20 minutes. After standing and aging for 1-2 hours, it is shaped using an automatic molding machine, then dried in hot air at 35-45℃ for 4-5 hours, equilibrated for 45-50 hours, and then vacuum dried to obtain ginseng moxa sticks with anti-fatigue effects.

[0023] Furthermore, during the molding process, the pressure is set to 80-100 MPa, the holding pressure is maintained for 5-10 seconds, and the density is controlled to be 0.8-1.0 g / cm³. 3 .

[0024] The beneficial effects of this invention are:

[0025] 1. Ginsenosides in ginseng extract can promote glucose uptake and fatty acid oxidation, and increase ATP production. Schisandrin B can protect the integrity of mitochondrial membranes, complementing the ATP-generating effect of ginsenosides, and together they play an anti-fatigue role. Chitosan's film-forming and adsorption properties can encapsulate the active ingredients of ginseng, which are slowly released during the burning of the moxa stick, prolonging the duration of the medicinal effect.

[0026] 2. The free thiol groups in thiolated silk fibroin can scavenge reactive oxygen species generated during aerobic metabolism, reducing muscle fatigue caused by oxidative stress. By modifying chitosan and silk fibroin, quaternary ammonium salt groups are introduced, which can improve the electrostatic binding ability with negatively charged ginsenosides and schisandrin B molecules, thereby improving drug loading efficiency. In addition, the quaternary ammonium salt groups can endow the material with broad-spectrum antibacterial properties, improving the antibacterial performance of moxibustion sticks while reducing the risk of skin infection during moxibustion. Attached Figure Description

[0027] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0028] Figure 1 This is the 1H NMR spectrum of the modified chitosan in Example 1 of this invention.

[0029] Figure 2 This is the hydrogen NMR spectrum of intermediate 1 in Embodiment 1 of the present invention. Detailed Implementation

[0030] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] In the following specific embodiments, the raw materials used are chemically pure. Additionally:

[0032] The chitosan used has a degree of deacetylation of 95%.

[0033] The preparation method of the ginseng extract used is as follows:

[0034] 100g of dried ginseng was processed into coarse powder using a pulverizer. 1000mL of 70% ethanol solution was added to the coarse powder at a ratio of 1:10, and the mixture was soaked for 3 hours. Then, the mixture was heated under reflux in a water bath for 1.5 hours, and filtered to obtain the first extract. Another 1000mL of 70% ethanol solution was added, and the process of reflux heating in a water bath for 1 hour was repeated, followed by filtration to obtain the second extract. The two extracts were combined and concentrated to 50mL by rotary evaporation. The evaporated product was then dried in a vacuum drying oven to obtain the ginseng extract.

[0035] The preparation method of the schisandrin B used is as follows:

[0036] 500g of dried, mature Schisandra chinensis fruit was crushed into a coarse powder (40-mesh sieve) and then soaked in 95% ethanol, with 5000mL of ethanol added at a 1:10 ratio. Soaking was carried out at room temperature for 24 hours, with stirring every 6 hours. The extract was filtered through filter paper and concentrated to a paste under reduced pressure at 40℃ using a rotary evaporator to remove ethanol. The extract was first extracted three times with an equal volume of n-hexane to remove lipid-soluble impurities, and then extracted three times with ethyl acetate at a 1:1 ratio. All ethyl acetate layers were evaporated by rotary evaporation to obtain a crude extract containing schisandrin B. This crude extract was then purified by 60-100 mesh silica gel column chromatography using a hexane / ethyl acetate gradient elution. The fraction containing schisandrin B was collected after TLC detection. The sample was dissolved in acetonitrile and separated using a C18 reversed-phase column with acetonitrile and water (70:30) as the mobile phase and a detection wavelength of 254nm. The fraction containing schisandrin B with a purity ≥98% by high-performance liquid chromatography was collected. Acetonitrile solvent was removed by rotary evaporation, and schisandrin B was dried to constant weight in a vacuum dryer to obtain high-purity schisandrin B powder.

[0037] The method for preparing the thiolized silk fibroin used is as follows:

[0038] Weigh 10g of silkworm cocoons and boil them in 4L of 0.05mol / L sodium carbonate aqueous solution for 30min. After removing the cocoons, repeat the above steps twice. Wash the boiled cocoons with deionized water and dry them to obtain degummed silk. Immerse 5.2g of degummed silk in approximately 75mL of calcium chloride-ethanol-water (molar ratio of 1:2:8) solution and stir at 70℃ for 4h to obtain silk fibroin solution.

[0039] After cooling, centrifuge at room temperature for 6 min to remove insoluble impurities. Place the dissolved silk fibroin salt solution in a dialysis bag with a molecular weight cutoff of 3500 and dialyze in deionized water at 4℃ for 3 days. Adjust the pH of the dialyzed silk fibroin aqueous solution with a pH of 6 using a 0.1 mol / L 2-morpholinoethanesulfonic acid aqueous solution (containing 0.05 mol / L sodium chloride). Once the pH stabilizes at 6, add 0.04 L of 0.3 mol / L 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.06 L of 0.5 mol / L N-hydroxysuccinimide, and activate the reaction at room temperature for 30 min. Then add 0.09 L of 0.18 mol / L reduced glutathione and react for 18 h. Place the reaction solution in a dialysis bag with a molecular weight cutoff of 3500 Da and dialyze in deionized water at 4℃ for 2 days. Freeze-dry to obtain thiolized silk fibroin.

[0040] Example 1

[0041] This application provides a ginseng moxibustion stick with anti-fatigue effects and its preparation method, using the following technical solution:

[0042] (1) 2.12 g of chitosan was swollen in 22 mL of 3% acetic acid solution for 1 h, and then 2.03 g of 2,3-epoxypropyltrimethylammonium chloride was added and stirred. Then 0.4 mL of 3% dilute hydrochloric acid was added and reacted at 70 °C for 10 h. After the reaction was completed, the mixture was filtered, washed three times with deionized water, and then washed once with 70% ethanol. The mixture was then dried under vacuum at 45 °C to obtain modified chitosan. The reaction process is as follows:

[0043]

[0044] (2) At 0℃, 3.12g of mercapto-modified silk fibroin was swollen in 28mL of deionized water for 1h, dialyzed for 50h, and then 2.53g of methacryloyloxyethyltrimethylammonium chloride and 0.1g of ammonium persulfate were added and stirred. The mixture was reacted at 30℃ for 18h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.0. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1. The reaction process is as follows:

[0045]

[0046] (3) Add 3.61g of intermediate 1 and 4.12g of tea polyphenols to the reactor, stir and mix, add 0.08g of p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 45℃ for 16h, after the reaction is completed, cool to room temperature, dialyze for 12h using a dialysis bag with a cutoff of 3kDa, concentrate by vacuum rotary evaporation, and dry at 50℃ for 3h to obtain modified silk fibroin;

[0047] (4) Pass 45 parts by weight of moxa wool through an 80-mesh sieve to remove coarse particles. Then, place it in a three-dimensional mixer with 8 parts by weight of ginseng extract, 5 parts by weight of schisandrin B, 3 parts by weight of modified chitosan, 2 parts by weight of modified silk fibroin, and 1 part by weight of glycerin. Stir and mix for 30 minutes. Finally, add 0.2 parts by weight of musk and continue stirring for 15 minutes. After standing and aging for 1 hour, use an automatic molding machine to press it into moxa sticks with a diameter of 1.8 cm and a length of 20 cm under a pressure of 80 MPa for 5 seconds. The density is controlled to be 0.8 g / cm³. 3 The ginseng moxibustion strips were dried in hot air at 35℃ for 4 hours, then equilibrated in an environment with 50% humidity for 45 hours, and finally vacuum dried to obtain ginseng moxibustion strips with anti-fatigue effects.

[0048] Example 2

[0049] This application provides a ginseng moxibustion stick with anti-fatigue effects and its preparation method, using the following technical solution:

[0050] (1) 2.16 g of chitosan was swollen in 25 mL of 3% acetic acid solution for 2 h, and then 2.08 g of 2,3-epoxypropyltrimethylammonium chloride was added and stirred. Then 0.5 mL of 3% dilute hydrochloric acid was added and reacted at 80 °C for 12 h. After the reaction was completed, the mixture was filtered, washed three times with deionized water, and then washed once with 70% ethanol. The mixture was then dried under vacuum at 40 °C to obtain modified chitosan.

[0051] (2) At 4℃, 3.16g of mercapto-modified silk fibroin was swollen in 32mL of deionized water for 2h, dialyzed for 70h, and then 2.58g of methacryloyloxyethyltrimethylammonium chloride and 0.12g of ammonium persulfate were added and stirred. The mixture was reacted at 50℃ for 22h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.0. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1.

[0052] (3) Add 3.65g of intermediate 1 and 4.17g of tea polyphenols to the reactor, stir and mix, add 0.09g of p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 60℃ for 24h, after the reaction is completed, cool to room temperature, dialyze for 12h using a dialysis bag with a cutoff of 3kDa, concentrate by vacuum rotary evaporation, and dry at 50℃ for 3h to obtain modified silk fibroin;

[0053] (4) Pass 50 parts by weight of moxa wool through an 80-mesh sieve to remove coarse particles. Then, place it in a three-dimensional mixer with 12 parts by weight of ginseng extract, 10 parts by weight of schisandrin B, 5 parts by weight of modified chitosan, 4 parts by weight of modified silk fibroin, and 3 parts by weight of glycerin. Stir for 40 minutes. Finally, add 0.3 parts by weight of musk and continue stirring for 20 minutes. After standing and aging for 2 hours, use an automatic molding machine to press it into moxa sticks with a diameter of 1.8 cm and a length of 20 cm under a pressure of 100 MPa for 10 seconds. The density is controlled to be 1.0 g / cm³. 3 The ginseng moxibustion strips were dried in a hot air circulation system at 45℃ for 5 hours, then equilibrated in an environment with 50% humidity for 50 hours, and finally vacuum dried to obtain ginseng moxibustion strips with anti-fatigue effects.

[0054] Example 3

[0055] This application provides a ginseng moxibustion stick with anti-fatigue effects and its preparation method, using the following technical solution:

[0056] (1) 2.14 g of chitosan was swollen in 24 mL of 3% acetic acid solution for 1 h, and then 2.05 g of 2,3-epoxypropyltrimethylammonium chloride was added and stirred. Then 0.4 mL of 3% dilute hydrochloric acid was added and reacted at 75 °C for 11 h. After the reaction was completed, the mixture was filtered, washed twice with deionized water, and then washed twice with 70% ethanol. The mixture was then dried under vacuum at 45 °C to obtain modified chitosan.

[0057] (2) At 2℃, 3.14g of mercapto-modified silk fibroin was swollen in 30mL of deionized water for 1h and dialyzed for 60h. Then, 2.55g of methacryloyloxyethyltrimethylammonium chloride and 0.11g of ammonium persulfate were added and stirred. The mixture was reacted at 40℃ for 20h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.5. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1.

[0058] (3) Add 3.63g of intermediate 1 and 4.15g of tea polyphenols to the reactor, stir and mix, add 0.08g of p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 50℃ for 20h, after the reaction is completed, cool to room temperature, dialyze for 12h using a dialysis bag with a cutoff of 3kDa, concentrate by vacuum rotary evaporation, and dry at 50℃ for 3h to obtain modified silk fibroin;

[0059] (4) Pass 48 parts by weight of moxa wool through an 80-mesh sieve to remove coarse particles. Then, place it in a three-dimensional mixer with 10 parts by weight of ginseng extract, 8 parts by weight of schisandrin B, 4 parts by weight of modified chitosan, 3 parts by weight of modified silk fibroin, and 2 parts by weight of glycerin. Stir and mix for 35 minutes. Finally, add 0.2 parts by weight of musk and continue stirring for 18 minutes. After standing and aging for 1 hour, use an automatic molding machine to press it into moxa sticks with a diameter of 1.8 cm and a length of 20 cm under a pressure of 90 MPa for 8 seconds. The density is controlled to be 0.9 g / cm³. 3 The ginseng moxibustion strips were dried in a hot air circulation system at 40℃ for 4 hours, then equilibrated in an environment with 50% humidity for 48 hours, and finally vacuum dried to obtain ginseng moxibustion strips with anti-fatigue effects.

[0060] Example 4

[0061] This application provides a ginseng moxibustion stick with anti-fatigue effects and its preparation method, using the following technical solution:

[0062] (1) 2.13 g of chitosan was swollen in 23 mL of 3% acetic acid solution for 1 h, and then 2.04 g of 2,3-epoxypropyltrimethylammonium chloride was added and stirred. Then 0.4 mL of 3% dilute hydrochloric acid was added and reacted at 72 °C for 11 h. After the reaction was completed, the mixture was filtered, washed three times with deionized water, and then washed twice with 70% ethanol. The mixture was then dried under vacuum at 40 °C to obtain modified chitosan.

[0063] (2) At 1℃, 3.13g of mercapto-modified silk fibroin was swollen in 29mL of deionized water for 1h, dialyzed for 55h, and then 2.54g of methacryloyloxyethyltrimethylammonium chloride and 0.1g of ammonium persulfate were added and stirred. The mixture was reacted at 35℃ for 19h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.2. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1.

[0064] (3) Add 3.62g of intermediate 1 and 4.14g of tea polyphenols to the reactor, stir and mix, add 0.08g of p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 48℃ for 18h, after the reaction is completed, cool to room temperature, dialyze for 12h using a dialysis bag with a cutoff of 3kDa, concentrate by vacuum rotary evaporation, and dry at 50℃ for 3h to obtain modified silk fibroin;

[0065] (4) Pass 46 parts by weight of moxa wool through an 80-mesh sieve to remove coarse particles. Then, place it in a three-dimensional mixer with 9 parts by weight of ginseng extract, 6 parts by weight of schisandrin B, 3 parts by weight of modified chitosan, 2 parts by weight of modified silk fibroin, and 2 parts by weight of glycerin. Stir and mix for 30 minutes. Finally, add 0.2 parts by weight of musk and continue stirring for 16 minutes. After standing and aging for 1 hour, use an automatic molding machine to press it into moxa sticks with a diameter of 1.8 cm and a length of 20 cm under a pressure of 85 MPa for 6 seconds. The density is controlled to be 0.8 g / cm³. 3 The ginseng moxibustion strips were dried in hot air at 35°C for 4 hours, then equilibrated in an environment with 50% humidity for 46 hours, and finally vacuum dried to obtain ginseng moxibustion strips with anti-fatigue effects.

[0066] Example 5

[0067] This application provides a ginseng moxibustion stick with anti-fatigue effects and its preparation method, using the following technical solution:

[0068] (1) 2.15g of chitosan was swollen in 24mL of 3% acetic acid solution for 2h, and then 2.06g of 2,3-epoxypropyltrimethylammonium chloride was added and stirred. Then 0.5mL of 3% dilute hydrochloric acid was added and reacted at 78℃ for 12h. After the reaction was completed, the mixture was filtered, washed three times with deionized water, and then washed twice with 70% ethanol. The mixture was then dried under vacuum at 50℃ to obtain modified chitosan.

[0069] (2) At 3℃, 3.15g of mercapto-modified silk fibroin was swollen in 31mL of deionized water for 2h, dialyzed for 65h, and then 2.56g of methacryloyloxyethyltrimethylammonium chloride and 0.12g of ammonium persulfate were added and stirred. The mixture was reacted at 45℃ for 21h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.0. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1.

[0070] (3) Add 3.64g of intermediate 1 and 4.16g of tea polyphenols to the reactor, stir and mix, add 0.09g of p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 55℃ for 22h, after the reaction is completed, cool to room temperature, dialyze for 12h using a dialysis bag with a cutoff of 3kDa, concentrate by vacuum rotary evaporation, and dry at 50℃ for 3h to obtain modified silk fibroin;

[0071] (4) Pass 48 parts by weight of moxa wool through an 80-mesh sieve to remove coarse particles. Then, place it in a three-dimensional mixer with 11 parts by weight of ginseng extract, 9 parts by weight of schisandrin B, 4 parts by weight of modified chitosan, 4 parts by weight of modified silk fibroin, and 3 parts by weight of glycerin. Stir for 40 minutes. Finally, add 0.3 parts by weight of musk and continue stirring for 18 minutes. After standing and aging for 2 hours, use an automatic molding machine to press it into moxa sticks with a diameter of 1.8 cm and a length of 20 cm under a pressure of 95 MPa for 10 seconds. The density is controlled to be 1.0 g / cm³. 3 The ginseng moxibustion strips were dried in a hot air circulation system at 45℃ for 5 hours, then equilibrated in an environment with 50% humidity for 50 hours, and finally vacuum dried to obtain ginseng moxibustion strips with anti-fatigue effects.

[0072] Comparative Example 1

[0073] The difference between this comparative example and Example 5 is that chitosan was used instead of modified chitosan.

[0074] Comparative Example 2

[0075] The difference between this comparative example and Example 5 is that thiolated silk fibroin was used instead of modified silk fibroin.

[0076] Comparative Example 3

[0077] The difference between this comparative example and Example 5 is that silk fibroin is used instead of thiolized silk fibroin to prepare modified silk fibroin. Specifically, step (2) in this comparative example is as follows:

[0078] At 3℃, 3.15g of silk fibroin was swollen in 31mL of deionized water for 2h and dialyzed for 65h. Then, 2.56g of methacryloyloxyethyltrimethylammonium chloride and 0.12g of ammonium persulfate were added and stirred. The mixture was reacted at 45℃ for 21h. After the reaction was completed, sodium bicarbonate was added to adjust the pH to 7.0. Dialysis was performed for 36h using a dialysis bag with a cutoff of 3.5kDa. The mixture was then centrifuged at 8000rpm for 15min and dried at 45℃ for 2h to obtain intermediate 1.

[0079] Comparative Example 4

[0080] The difference between this comparative example and Example 5 is that schisandrin B was used instead of ginseng extract.

[0081] Performance testing

[0082] The moxa sticks prepared in Examples 1-5 and Comparative Examples 1-3 were subjected to performance tests.

[0083] (1) The method for testing anti-fatigue performance is as follows: After 3 days of adaptive training, healthy male mice were randomly divided into groups of the examples and groups of the comparative examples, with 10 mice in each group. The mice in each group were fixed in a specially made moxibustion cage and moxibusted for 10 minutes / day at a set distance using moxa sticks prepared in Examples 1-5 and Comparative Examples 1-3, for 7 consecutive days. Then, a lead plate of 5% of the mouse's body weight was tied to the tail of each mouse and the mice were placed in a bucket with a water temperature of (23±1)℃ and a water depth of 30cm for a swimming experiment. The time from the start of swimming to exhaustion (the mouse sinks underwater for 10 seconds and still cannot rise to the surface) was counted as the weighted swimming time of the mice. The results are shown in Table 1.

[0084] Table 1: Fatigue Resistance Test Table

[0085]

[0086] Table 1 shows that the moxibustion sticks prepared in Examples 1-5 enabled mice to swim for a longer time, significantly longer than in other comparative examples, indicating that the moxibustion sticks of the present invention have a good anti-fatigue effect. The results in Comparative Example 1 show that chitosan, after quaternary ammonium salt modification, exhibits enhanced sustained-release efficacy and increased anti-fatigue effect. The results in Comparative Examples 2 and 3 show that silk fibroin, after thiolation and quaternary ammonium salt modification, can enhance drug loading efficiency and antioxidant capacity. The results in Comparative Example 4 verify the combined use of ginseng extract and schisandrin. Saponins in ginseng extract can promote glucose uptake and fatty acid oxidation, increasing ATP production, while schisandrin B can protect the integrity of the mitochondrial membrane, complementing the ATP-generating effect of ginseng saponins; the two have a synergistic anti-fatigue effect.

[0087] (2) The antibacterial performance test method is as follows: The smoke from burning moxa sticks is passed into a sealed chamber containing Staphylococcus aureus and Staphylococcus epidermidis bacterial solutions, and the survival rate of the bacterial solutions is detected after different 10 minutes. The results are shown in Table 2.

[0088] Table 2: Antibacterial Performance Test Table

[0089]

[0090] As can be seen from Table 2, the moxibustion sticks prepared in Examples 1-5 have a lower survival rate of bacterial solution, indicating that the moxibustion sticks of the present invention have good antibacterial effect.

[0091] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Unless otherwise specified, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0092] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

[0093] Those skilled in the art should understand that the above descriptions are merely several specific embodiments of the present invention, and not all embodiments. It should be noted that many modifications and improvements can be made by those skilled in the art, and all modifications or improvements not exceeding the scope of the claims should be considered within the protection scope of the present invention.

Claims

1. A ginseng moxibustion stick with anti-fatigue effects, characterized in that, It includes the following components by weight: 45-50 parts by weight of Artemisia argyi, 8-12 parts by weight of ginseng extract, 5-10 parts by weight of schisandrin B, 3-5 parts by weight of modified chitosan, 2-4 parts by weight of modified silk fibroin, 0.2-0.3 parts by weight of musk, and 1-3 parts by weight of glycerin. Among them, modified chitosan is obtained by modifying chitosan with epoxy quaternary ammonium salt; Modified silk fibroin is obtained by modifying thiolized silk fibroin with methacryloyloxyethyltrimethylammonium chloride and tea polyphenols; The modified chitosan is prepared by: swelling chitosan in a 3% acetic acid solution for 1-2 hours, then adding 2,3-epoxypropyltrimethylammonium chloride, stirring and mixing, then adding 3% dilute hydrochloric acid, reacting for 10-12 hours, and after the reaction is completed, filtering, washing, and drying to obtain the modified chitosan. The ratio of chitosan, acetic acid solution, 2,3-epoxypropyltrimethylammonium chloride, and dilute hydrochloric acid is 2.12-2.16 g: 22-25 mL: 2.03-2.08 g: 0.4-0.5 mL. The reaction temperature is 70-80℃; The method for preparing the modified silk fibroin is as follows: Step 1: At 0-4℃, thiolated silk fibroin was swollen in deionized water for 1-2 hours and dialyzed for 50-70 hours. Then, methacryloyloxyethyltrimethylammonium chloride and ammonium persulfate were added and stirred. The mixture was reacted at 30-50℃ for 18-22 hours. After the reaction was completed, the pH was adjusted to 7.0-7.5, and dialyzed using a dialysis bag with a cutoff of 3.5 kDa. The mixture was then centrifuged and dried to obtain intermediate 1. Step 2: Add intermediate 1 and tea polyphenols to the reactor, stir and mix, add p-toluenesulfonic acid, then add phosphate buffer to adjust the pH to neutral, react at 45-60℃ for 16-24h, after the reaction is completed, cool, dialyze using a dialysis bag with a cutoff of 3kDa, concentrate, dry, and obtain modified silk fibroin. The ratio of mercapto-modified silk fibroin, deionized water, methacryloyloxyethyltrimethylammonium chloride, and ammonium persulfate in step one is 3.12-3.16g: 28-32mL: 2.53-2.58g: 0.1-0.12g. In step two, the ratio of intermediate 1, tea polyphenols, and p-toluenesulfonic acid is 3.61-3.65g: 4.12-4.17g: 0.08-0.09g. The dialysis time in step one is 36-48 hours, and the dialysis time in step two is 12-24 hours.

2. A method for preparing a ginseng moxibustion stick with anti-fatigue effect as described in claim 1, characterized in that, Specifically, the following steps are included: The moxa wool is sieved to remove coarse particles, and then mixed with ginseng extract, schisandrin B, modified chitosan, modified silk fibroin, and glycerin in a three-dimensional mixer for 30-40 minutes. Finally, musk is added, and the mixture is stirred for another 15-20 minutes. After standing and aging for 1-2 hours, it is shaped using an automatic molding machine, then dried in hot air at 35-45℃ for 4-5 hours, equilibrated for 45-50 hours, and then vacuum dried to obtain ginseng moxa sticks with anti-fatigue effects.

3. The method for preparing a ginseng moxibustion stick with anti-fatigue effect according to claim 2, characterized in that, During the molding process, the pressure is set to 80-100MPa, the pressure is held for 5-10s, and the density is controlled to be 0.8-1.0g / cm3.

Citation Information

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