Citral essential oil-based turpinia formosana bacteriostatic ointment as well as preparation method and application thereof

Abstract

The invention provides citral essential oil-based turpinia formosana bacteriostatic ointment as well as a preparation method and application thereof, and relates to the technical field of plant ointment. The invention provides a citral essential oil composition which comprises the following components in percentage by mass: 1%-3% of citral essential oil, 8%-15% of a compound extract, 15%-20% of biological wax, 1%-3% of a defoaming agent and the balance of vegetable oil, the extraction method of the compound extract comprises the following steps: performing mixed extraction on the sassafras leaves and the turpinia arguta leaves to obtain a mixed extract, and performing tannic acid polymerization coating on the surface of the mixed extract to obtain the compound extract. The bacteriostatic ointment provided by the invention has good bacteriostatic, itching-relieving and mosquito-repelling effects, can be stored for a long time in a high-temperature environment, and has good stability.

Description

Technical Field

[0001] The invention relates to the technical field of plant ointments, and in particular to a citral essential oil-based safflower antibacterial ointment and a preparation method and application thereof. Background Art

[0002] Turpinia arguta Seem is a deciduous shrub of the genus Turpinia in the family Staphyleaceae. It is a local standard medicinal material in my country with rich medicinal value. It is recorded in the Chinese Pharmacopoeia that it has the effects of clearing away heat and detoxifying, relieving sore throat and swelling, and promoting blood circulation and relieving pain. It is often used to treat symptoms such as sore throat, sore throat, sore swelling, and pain from falls. Turpinia arguta Seem leaves contain a variety of pharmacologically active ingredients, which can effectively inhibit the growth and reproduction of a variety of bacteria by interfering with bacterial cell wall synthesis, protein synthesis, and nucleic acid metabolism, thereby exerting antibacterial and antibacterial effects. However, in the prior art, when Turpinia arguta Seem is used, it is usually extracted with alcohol and then compounded with other matrix components. It is difficult to fully utilize the efficacy of Turpinia arguta Seem, so it is urgent to provide a solution to improve the above problems. Summary of the invention

[0003] The invention aims to provide a citral essential oil-based safflower antibacterial ointment and a preparation method and application thereof.

[0004] In a first aspect, the present invention provides a citral essential oil-based safflower antibacterial ointment, which comprises, by mass percentage, 1%-3% citral essential oil, 8%-15% composite extract, 15%-20% bio-wax, 1%-3% defoaming agent and the remainder of vegetable oil; the extraction method of the composite extract comprises: mixing and extracting camphor leaves and safflower leaves to obtain a mixed extract, and polymerizing and coating the surface of the mixed extract with tannic acid to obtain a composite extract.

[0005] Optionally, the sum of the relative contents of β-citral and α-citral in the citral essential oil is greater than 60.0%.

[0006] Optionally, the biowax comprises beeswax.

[0007] Optionally, the defoaming agent includes one of sodium chloride and sodium sulfate.

[0008] Optionally, the vegetable oil includes one of camellia seed oil, camphor tree seed kernel oil and olive oil.

[0009] Optionally, the preparation method of the composite extract includes: mixing camphor leaf powder and safflower leaf powder to obtain a composite powder; performing alcohol extraction on the composite powder and separating the alcohol extract and alcohol residue; performing supercritical extraction on the alcohol residue and separating the extract; combining the alcohol extract and the extract and concentrating them by rotary evaporation to obtain a mixed extract; and polymerizing tannic acid on the surface of the mixed extract to obtain a composite extract.

[0010] Optionally, the sassafras leaf powder and the safflower leaf powder are mixed and then passed through a 50-60 mesh sieve, and the sieved material is collected to obtain a composite powder.

[0011] Optionally, the water content of the composite powder is less than or equal to 10%.

[0012] Optionally, the sassafras leaf powder and the sassafras leaf powder are mixed and then preheated at 50°C-70°C.

[0013] Optionally, the sassafras leaf powder and the safflower leaf powder are mixed and then ball-milled to obtain a composite powder.

[0014] Optionally, the mass ratio of the sassafras leaf powder to the sassafras leaf powder is 1:(0.8-1.2).

[0015] Optionally, the composite powder is extracted in anhydrous ethanol for 6h-8h and then the alcohol extract and the alcohol extraction residue are separated.

[0016] Optionally, the solid-to-liquid ratio of the composite powder after mixing with anhydrous ethanol is 0.005 g / mL-0.008 g / mL.

[0017] Optionally, the composite powder is extracted in anhydrous ethanol at 50° C.-70° C. in a closed environment.

[0018] Optionally, the composite powder is ultrasonically dispersed in the anhydrous ethanol and stirred at a rotation speed of 200 rpm-300 rpm and subjected to alcohol extraction.

[0019] Optionally, carbon dioxide is used as a supercritical fluid to perform supercritical extraction on the alcohol-extracted residue; wherein: the carbon dioxide is used to perform supercritical extraction on the alcohol-extracted residue for 2h-3h.

[0020] Optionally, after combining the alcohol extract and the extraction liquid, they are kept warm at 40° C.-45° C. for 1 h-2 h.

[0021] Optionally, the alcohol extract and the extraction liquid are combined and then ultrasonically dispersed.

[0022] Optionally, after combining the alcohol extract and the extraction liquid, they are concentrated by rotary evaporation at 40° C.-50° C. and the alcohol extraction solvent is recovered.

[0023] Optionally, the mixed extract is prepared by rotary evaporation and then drying.

[0024] Optionally, the mixed extract is mixed in the tannic acid solution and a trimethylammonium hydrochloride buffer is added dropwise, followed by separation and drying to obtain a composite extract.

[0025] Optionally, the mass ratio of the mixed extract to the tannic acid in the tannic acid solution is 1:(0.02-0.05).

[0026] Optionally, the mixed extract is dispersed in the tannic acid solution by ultrasonication.

[0027] Optionally, the pH of the trimethylammonium hydrochloride buffer is 8.5.

[0028] In a second aspect, the present invention provides a method for preparing any of the above-mentioned optional antibacterial ointments, comprising: heating and melting the biowax and adding vegetable oil to stir and mix, adding citral essential oil and the composite extract and stirring and mixing for 30 minutes to 40 minutes, adding a defoaming agent and stirring and mixing, vacuum degassing, and then cooling and shaping to obtain the antibacterial ointment.

[0029] In a third aspect, the present invention further provides an application of any of the above-mentioned optional antibacterial ointments, wherein the application includes antibacterial and antipruritic effects. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Unless otherwise defined, the technical terms or scientific terms used herein should be the common meanings understood by people with general skills in the field to which the present invention belongs.

[0031] The present invention provides a citral essential oil-based shanxiangyuan antibacterial ointment, including 1%-3% citral essential oil, 8%-15% composite extract, 15%-20% biowax, 1%-3% defoamer and surplus vegetable oil by mass percentage. In fact, vegetable oil and biowax are used as matrix components in the antibacterial ointment, not only with good biocompatibility, but also can form a protective barrier after being applied to the skin surface, and is conducive to the release of the antibacterial efficacy of citral essential oil and composite extract, and can also improve the effect of action, improve the timeliness of antibacterial and antipruritic. In addition, since biowax is usually solid at room temperature, it can be shaped for the antibacterial ointment.

[0032] In fact, citral essential oil can not only give antibacterial ointment aromatic smell, but also improve the antibacterial effect. Specifically, when the antibacterial ointment is applied to the surface of human skin, the citral molecules in citral essential oil can inhibit the growth and reproduction of bacteria and promote the death of bacteria, thereby achieving an antibacterial effect, while also being able to reduce the inflammatory response on the surface of the skin, thereby achieving an antipruritic effect, and the aromatic smell it brings can improve comfort and compliance. Specifically, citral essential oil can be extracted from natural plants, and the sum of the relative contents of β-citral and α-citral is greater than 60.0%.

[0033] Specifically, the extraction method of the composite extract includes: mixing and extracting sassafras leaves and sassafras leaves to obtain a mixed extract, and polymerizing and coating the surface of the mixed extract with tannic acid to obtain a composite extract. In fact, sassafras leaves and sassafras leaves contain a variety of natural compounds with antibacterial activity, such as flavonoids and triterpenoid saponins. Mixing and extracting sassafras leaves and sassafras leaves can effectively improve the mixing uniformity of the effective ingredients in sassafras leaves and sassafras leaves. After adding the antibacterial ointment, it can produce a synergistic effect with citral essential oil, thereby improving the overall antibacterial and antipruritic properties of the antibacterial ointment.

[0034] In fact, after tannic acid is polymerized on the surface of the mixed extract, the polytannic acid on the surface of the mixed extract can play a good protective role on the mixed extract, thereby improving the stability of the active ingredients in the antibacterial ointment during storage and avoiding degradation and inactivation of the active ingredients in the mixed extract. In addition, after the polytannic acid is used for coating, the compatibility of the mixed extract in the antibacterial ointment can be effectively improved, thereby effectively improving the overall stability of the antibacterial ointment. At the same time, tannic acid itself has a good antibacterial effect, which can further improve the antibacterial performance of the antibacterial ointment.

[0035] In some embodiments, the biowax used in the antibacterial ointment includes beeswax. In fact, beeswax is a relatively cheap and easily available biowax component, which can reduce the production cost of the antibacterial ointment. At the same time, it has good hardness and toughness, is easy to mix with vegetable oil and solidify to lock the active ingredients in the antibacterial ointment, and is conducive to applying it on the skin surface to form a film. In addition, the melting point of beeswax is generally 60°C-65°C, which is conducive to maintaining the structural stability of the antibacterial ointment during storage.

[0036] In some embodiments, the defoaming agent in the antibacterial ointment may be an inorganic salt, and specifically the defoaming agent may include one of sodium chloride and sodium sulfate. In fact, after the inorganic salt is added to the antibacterial ointment, the surface tension of the liquid in the molten state is adjusted, thereby promoting the rupture of bubbles therein, and the defoaming agent dispersed in the antibacterial ointment will not affect the performance of the antibacterial ointment, and will not cause harm to human skin.

[0037] In some embodiments, the vegetable oil in the antibacterial ointment can be one of camellia seed oil, camphor tree seed kernel oil, and olive oil. In fact, the use of vegetable oil can further reduce production costs. At the same time, camellia seed oil, camphor tree seed kernel oil, and olive oil all have certain water-retaining and moisturizing effects, which can reduce the irritation of the antibacterial ointment to the human skin after being applied to the human skin.

[0038] Specifically, the preparation method of the composite extract comprises the following steps: S1, mixing the sassafras leaf powder and the sassafras leaf powder to obtain a composite powder; S2, extracting the composite powder with alcohol and separating the alcohol extract and the alcohol extraction residue; S3, subjecting the alcohol extraction residue to supercritical extraction and separating the extract; S4, combining the alcohol extract and the extraction solution and concentrating by rotary evaporation to obtain a mixed extract; S5. The composite extract is prepared by polymerizing tannic acid on the surface of the mixed extract.

[0039] In fact, mixing the sassafras leaf powder with the sassafras leaf powder in step S1 is beneficial to the uniformity of the alcohol extraction residue after alcohol extraction in step S2, and is also beneficial to the uniformity of the active ingredients in the alcohol extract during alcohol extraction in step S2. Specifically, the use of sassafras leaf powder and sassafras leaf powder in step S1 helps to increase the specific surface area, which is beneficial to the dissolution of the internal alcohol-soluble active ingredients during the alcohol extraction process.

[0040] In some embodiments, after mixing the yellow sassafras leaf powder with the sassafras leaf powder in step S1, the powder is passed through a 50-60 mesh sieve, and the sieved material is collected as a composite powder. In fact, screening is beneficial to keep the particle size of the composite powder in the same range, which is beneficial to ensure the consistency of the particle size, and then the composite powder can be fully extracted during alcohol extraction, so that the alcohol-soluble components in the composite powder are uniformly dissolved. In addition, after mixing the yellow sassafras leaf powder with the sassafras leaf powder, a ball milling blending method can be used for grinding treatment to further improve the consistency of the particle size of the composite powder.

[0041] In some embodiments, the water content of the composite powder used in step S1 is less than or equal to 10%. In fact, by reducing the water content in the composite powder, the penetration efficiency of the alcohol extraction solvent during the alcohol extraction process can be improved, thereby improving the dissolution efficiency of the active substance in the composite powder, and improving the solubility of the active ingredients. In addition, impurities in the alcohol extraction process can be reduced. Specifically, after mixing the yellow camphor leaf powder and the safflower leaf powder, they can be preheated at 50°C-70°C, which can not only further reduce the water content, but also activate the active ingredients, thereby improving the dissolution efficiency of the active ingredients.

[0042] In some embodiments, in step S1, the sassafras leaf powder and the sassafras leaf powder are mixed at a mass ratio of 1: (0.8-1.2). In fact, by adjusting the amount of sassafras leaf powder and the sassafras leaf powder, the mixing ratio of the two active ingredients from different sources in the obtained alcohol extract can be adjusted, and then the antibacterial and antipruritic properties of the obtained antibacterial ointment can be comprehensively optimized, while avoiding the influence of too much single ingredient on the structural consistency. Specifically, the sassafras leaf powder and the sassafras leaf powder are both obtained by drying and crushing mature leaves.

[0043] In fact, when the composite powder is subjected to alcohol extraction in step S2, the alcohol extraction solvent can penetrate into the composite powder and dissolve the alcohol-soluble active substance therein into the alcohol extract, and obtain alcohol extraction residue. Specifically, after the composite powder is subjected to alcohol extraction in anhydrous ethanol for 6h-8h, solid-liquid separation is performed to obtain an alcohol extract and an alcohol extraction residue. In fact, by controlling the alcohol extraction time in anhydrous ethanol, it is beneficial to balance the alcohol extraction efficiency and production efficiency.

[0044] In some embodiments, the composite powder is pre-mixed in anhydrous ethanol in step S2, and the solid-liquid ratio after mixing is controlled to be 0.005 g / mL-0.008 g / mL. In fact, by controlling the solid-liquid ratio of the composite powder in anhydrous ethanol, it is helpful to improve the dispersion uniformity of the composite powder in anhydrous ethanol, and increase the concentration difference between the inside and outside, which is beneficial to the dissolution of the active ingredient in the composite powder.

[0045] Specifically, the composite powder can be ultrasonically dispersed in anhydrous ethanol, so that the ultrasonic cavitation effect can be used to avoid the agglomeration and sedimentation of the composite powder, while removing tiny bubbles adhering to the surface of the composite powder, promoting the contact between anhydrous ethanol and the composite powder, thereby improving the alcohol extraction efficiency.

[0046] In some embodiments, in step S2, the composite powder is subjected to alcohol extraction in anhydrous ethanol in a closed environment at 50°C-70°C. In fact, by performing alcohol extraction at a temperature close to the boiling point of anhydrous ethanol, not only can the activity of the active ingredients in the composite powder be effectively improved, but also the rapid penetration and movement of anhydrous ethanol in the composite powder can be promoted, thereby dissolving the active ingredients in the composite powder into the alcohol extract. In addition, performing alcohol extraction in a closed environment is conducive to maintaining a pure environment, avoiding external impurities from contaminating the alcohol extract and preventing the volatilization of anhydrous ethanol.

[0047] In some embodiments, when the composite powder is extracted in anhydrous ethanol in step S2, a mechanical rotation speed of 200rpm-300rpm is used for stirring, so as to improve the dispersion uniformity of the composite powder during the extraction process, and at the same time promote the collision efficiency between anhydrous ethanol and the composite powder, and promote the rapid diffusion of active substances in anhydrous ethanol, thereby avoiding a decrease in the concentration difference between the inside and outside of the composite powder.

[0048] In fact, in step S3, the alcohol-extracted residue is subjected to supercritical extraction, and the supercritical fluid can penetrate into the alcohol-extracted residue to extract the active ingredients remaining therein. At the same time, the supercritical fluid can utilize the penetration and dissolution effect of the active ingredients to dissolve the active ingredients tightly combined with the tissue in the alcohol-extracted residue, thereby effectively improving the extraction rate and diversity of the active ingredients in the extract.

[0049] In some embodiments, carbon dioxide is used as a supercritical fluid to perform supercritical extraction on the alcohol-extracted residue in step S3. Specifically, since the supercritical carbon dioxide has a low polarity, it can selectively dissolve the fat-soluble components in the alcohol-extracted residue, while ignoring impurity components such as polysaccharides and proteins in the alcohol-extracted residue, thereby reducing the entry of impurities into the extract, helping to further enrich the effective ingredients in the composite powder, thereby enhancing the activity in antibacterial, antipruritic, and anti-inflammatory.

[0050] In some embodiments, carbon dioxide is used as a supercritical fluid in step S3 to perform supercritical extraction on the alcohol-extracted residue at a pressure of 10 MPa-30 MPa and 35° C.-55° C. In fact, by using a low temperature environment for supercritical extraction, the destruction of active ingredients in the alcohol-extracted residue by high temperature can be avoided.

[0051] Specifically, supercritical extraction of the alcohol-extracted residue for 2h-3h is beneficial to improving the extraction rate of active ingredients in the alcohol-extracted residue. In fact, in step S3, the supercritical mixed fluid obtained after supercritical extraction can be separated in a separation device, so that the supercritical fluid is gasified so that the target active ingredient is precipitated in the form of liquid or solid, thereby removing the supercritical fluid to obtain an extract containing only the target active ingredient.

[0052] In fact, after the alcohol extract and the extraction liquid are combined and the solvent is removed by rotary evaporation in step S4, the active ingredients can be concentrated, and it is also beneficial to polymerize and coat the surface tannic acid in step S5. Specifically, after the alcohol extract and the extraction liquid are combined in step S4, they are kept at 40°C-50°C for 1h-2h, which is beneficial to promote the mutual dispersion of the active ingredients in the alcohol extract and the extraction liquid, thereby improving the uniformity of the active ingredients in the subsequent mixed extract.

[0053] In some embodiments, ultrasonic dispersion treatment may be performed after the alcohol extract and the extract are combined in step S4 to further improve the dispersion uniformity of different active ingredients in the alcohol extract and the extract. Specifically, ultrasonic dispersion may be performed for 10 min to 15 min at a frequency of 20 kHz to 30 kHz after the alcohol extract and the extract are combined. By controlling the frequency and duration of ultrasonic treatment, excessive ultrasonic treatment may be avoided to damage the active ingredients in the alcohol extract and the extract.

[0054] In some embodiments, after the alcohol extract and the extract are combined in step S4, the alcohol extract solvent is concentrated by rotary evaporation at 40°C-50°C and recovered. In fact, the boiling point of the alcohol extract solvent can be reduced by reducing the volume during the rotary evaporation concentration process, so that the alcohol extract solvent can be evaporated at a lower temperature and the damage to the active ingredients can be reduced. Specifically, after the rotary evaporation concentration in step S4, the mixed extract is obtained after hot air drying at 30°C-40°C.

[0055] In fact, by polymerizing tannic acid on the surface of the mixed extract in step S5, the active ingredients in the mixed extract can be protected from the influence of external environmental factors, and the active ingredients can be prevented from being inactivated and destroyed in an environment of light and temperature changes, thereby improving the storage performance and stability of the antibacterial ointment. At the same time, the polytannic acid coating layer on the surface of the antibacterial ointment can effectively improve the compatibility in the composite matrix of bio-wax and vegetable oil.

[0056] In some embodiments, after the mixed extract is mixed in the tannic acid solution in step S5, a trimethylammonium hydrochloride buffer is added dropwise to polymerize the tannic acid on the surface of the mixed extract to form polytannic acid, and then separated and dried to obtain a composite extract. In fact, after the mixed extract is mixed in the tannic acid solution, the tannic acid molecules can be adsorbed on the surface of the mixed extract, and then a buffer is added dropwise to adjust the pH environment, thereby promoting the self-polymerization of the tannic acid molecules. Specifically, the pH of the trimethylammonium hydrochloride buffer is 8.5.

[0057] In some embodiments, after the mixed extract is ultrasonically mixed in the tannic acid solution in step S5, the mass ratio of the mixed extract to the tannic acid in the tannic acid solution is 1:(0.02-0.05). In this way, a complete and uniform polytannic acid coating layer can be formed on the surface of the mixed extract, effectively improving the protective performance of the coating layer on the mixed extract, while preventing the coating layer from being too thick to affect the release of active ingredients in the mixed extract.

[0058] In some embodiments, in step S5, the mixed extract is dried and preheated before grinding and powdering to increase the looseness of the mixed extract, which is beneficial to increase the specific surface area of ​​the mixed extract, promote the uniform coating and molding of tannic acid on the surface of the mixed extract, and at the same time reduce the particle size of the prepared composite extract, which is beneficial to improve the dispersibility of the composite extract in the antibacterial ointment.

[0059] The present invention also provides a method for preparing the antibacterial ointment in any of the above embodiments, comprising: heating and melting the biowax and adding vegetable oil to stir and mix, adding citral essential oil and the composite extract and stirring and mixing for 30 minutes to 40 minutes, adding a defoaming agent, mixing, vacuum degassing, and then cooling and shaping to obtain the antibacterial ointment.

[0060] In fact, by heating and melting the biowax, the biowax that is solid at room temperature can be changed into a liquid state, which helps the biowax to be fully mixed with the vegetable oil, and can also be used as a dispersion matrix for the remaining ingredients to protect and shape. At the same time, after adding citral essential oil and the composite extract for stirring and mixing, it is beneficial to the uniformity of the dispersion of citral essential oil and the composite extract in the matrix, and helps the citral essential oil and the composite extract to interact and synergize. The defoamer added at last can remove the bubbles generated during the initial stirring process, thereby improving the appearance and quality of the antibacterial ointment, while avoiding residual impurities in the antibacterial ointment, which helps to improve the performance stability and storage performance of the antibacterial ointment.

[0061] The present invention also provides an application of the antibacterial ointment in any of the above embodiments, including antibacterial and antipruritic effects. In fact, mosquito bites will trigger an immune response in the human body, resulting in symptoms such as redness, swelling and itching at the bite site, which can easily cause people to scratch and damage the skin barrier, and easily cause bacterial infection and pain. Therefore, an antibacterial ointment can be applied to the bite site to form a skin barrier, and at the same time, citral essential oil and the composite extract can have an antibacterial and antipruritic effect.

[0062] Preparation Example 1 This preparation example 1 provides a method for preparing a composite extract, comprising the following steps: S1. Mix the yellow camphor leaf powder and the safflower leaf powder in a mass ratio of 1:1, pass through a 50-mesh sieve, collect the sieved material, and preheat it in an environment of 60° C. for 30 min. After the preheating process, turn it over to ensure uniform heating, and obtain a composite powder; S2, adding the composite powder and anhydrous ethanol to a reaction tank and controlling the solid-liquid ratio in the reaction tank to be 0.006 g / mL, using an ultrasonic device to ultrasonically disperse the solid-liquid mixture in the reaction tank to promote uniform dispersion of the composite powder in the anhydrous ethanol, heating the reaction tank to 60° C. and stirring at a speed of 200 rpm and extracting for 8 hours; after the extraction is completed, filtering while hot to obtain an alcohol extraction residue and an alcohol extract, and washing the alcohol extraction residue with anhydrous ethanol and merging the washing liquid into the alcohol extract; S3, transferring the alcohol extraction residue to a supercritical extraction device, using carbon dioxide as a supercritical fluid, performing supercritical extraction on the alcohol extraction residue at 40°C and a pressure of 20MPa for 2h, and then flowing the supercritical carbon dioxide containing the active substance to a separation kettle for decompression separation, thereby recovering the carbon dioxide, and adding anhydrous ethanol for re-dissolution to obtain an extract; S4, combining the alcohol extract and the extraction liquid, performing ultrasonic dispersion, and keeping them in a 45°C water bath for 2 hours, then concentrating them by rotary evaporation at 45°C and recovering anhydrous ethanol, collecting the concentrate, drying it in a 35°C hot air drying oven to constant weight, and then grinding it to obtain a mixed extract with an average particle size of 20 μm; S5. Put the mixed extract into a tannic acid aqueous solution with a concentration of 8 mg / mL and control the mass ratio of the mixed extract to tannic acid to be 1:0.03, then ultrasonically mix at a frequency of 20 kHz for 10 minutes, and then dropwise add a trimethylammonium hydrochloride buffer solution with a concentration of 1 mol / L and a pH of 8.5 to the mixed solution, and control the volume ratio of the tannic acid aqueous solution to the trimethylammonium hydrochloride buffer solution to be 1:0.2; after the addition is completed, stir for 30 minutes, separate by vacuum filtration, and dry the obtained solid to obtain a composite extract.

[0063] Preparation Example 2 Preparation Example 2 provides a method for preparing a composite extract, which is different from Preparation Example 1 in that step S3 is not performed, and in step S4, only the alcohol extract is concentrated by rotary evaporation.

[0064] Preparation Example 3 This preparation example 3 provides a method for preparing a composite extract, comprising the following steps: D1. After passing the yellow camphor leaf powder and the safflower leaf powder through a 50-mesh sieve, the sieved materials are collected and preheated in a 60° C. environment for 30 minutes, and the sieved materials are turned over during the preheating process to ensure uniform heating. After the preheating, the yellow camphor leaf powder and the safflower leaf powder to be extracted are obtained; D2. Put the sassafras leaf powder to be extracted and the sassafras leaf powder to be extracted into different reaction tanks respectively, add anhydrous ethanol to control the solid-liquid ratio to 0.006 g / mL, use ultrasonic equipment to ultrasonically disperse the solid-liquid mixture in the reaction tank to promote uniform dispersion in anhydrous ethanol, heat the reaction tank to 60°C and stir and extract at a speed of 200 rpm for 8 hours; after the extraction, filter while hot to obtain sassafras alcohol extract and sassafras alcohol extract residue, sassafras alcohol extract and sassafras alcohol extract residue, rinse the sassafras alcohol extract residue with anhydrous ethanol and then merge the rinse liquid into the sassafras alcohol extract, rinse the sassafras alcohol extract residue with anhydrous ethanol and then merge the rinse liquid into the sassafras alcohol extract; D3, respectively transferring the alcohol extract residue of safrole and the alcohol extract residue of safflower to a supercritical extraction device, using carbon dioxide as a supercritical fluid, performing supercritical extraction on the alcohol extract residue at 40° C. and a pressure of 20 MPa for 2 h, and then flowing the supercritical carbon dioxide containing the active substance to a separation kettle for decompression separation, thereby recovering the carbon dioxide, and adding anhydrous ethanol for re-dissolution to obtain a safrole extract and a safflower extract, respectively; D4. Combine the sassafras extract and the sassafras alcohol extract, perform ultrasonic dispersion, keep them in a water bath at 45°C for 2 hours, concentrate them by rotary evaporation at 45°C and recover the anhydrous ethanol, collect the concentrate, dry them in a hot air drying oven at 35°C to constant weight, and grind them to obtain a sassafras extract with an average particle size of 20 μm; combine the sassafras extract and the sassafras alcohol extract, perform ultrasonic dispersion, keep them in a water bath at 45°C for 2 hours, concentrate them by rotary evaporation at 45°C and recover the anhydrous ethanol, collect the concentrate, dry them in a hot air drying oven at 35°C to constant weight, and grind them to obtain a sassafras extract with an average particle size of 20 μm; mix the sassafras extract and the sassafras extract in a mass ratio of 1:1 to obtain a mixed extract; D5. Put the mixed extract into a tannic acid aqueous solution with a concentration of 8 mg / mL and control the mass ratio of the mixed extract to tannic acid to be 1:0.03, then ultrasonically mix at a frequency of 20 kHz for 10 minutes, and then add trimethylammonium hydrochloride buffer solution with a concentration of 1 mol / L and a pH of 8.5 dropwise to the mixed solution, and control the volume ratio of the tannic acid aqueous solution to the trimethylammonium hydrochloride buffer solution to be 1:0.2; after the addition is completed, stir for 30 minutes, then separate by vacuum filtration, and dry the obtained solid to obtain a composite extract.

[0065] Preparation Example 4 Preparation Example 4 provides a method for preparing a composite extract, which is different from Preparation Example 1 in that in step S5, the mixed extract is added to a dopamine aqueous solution with a concentration of 5 mg / mL, and the mass ratio of the mixed extract to dopamine is controlled to be 1:0.03.

[0066] Preparation Example 5 This Preparation Example 5 provides a method for preparing a composite extract, which is different from Preparation Example 1 in that only an equal amount of sassafras leaf powder is used in step S1.

[0067] Preparation Example 6 Preparation Example 6 provides a method for preparing a composite extract, which is different from Preparation Example 1 in that only an equal amount of Scutellaria baicalensis leaf powder is used in step S1.

[0068] Preparation Example 7 This Preparation Example 7 provides a method for preparing a composite extract, which is different from Preparation Example 1 in that step S5 is not performed, and the composite extract is prepared in step S4.

[0069] Example 1

[0070] This Example 1 provides a preparation method of a citral essential oil-based Sanxiangyuan antibacterial ointment, comprising the following steps: heating beeswax in a water bath environment to melt, adding a partial amount of corn oil, adding the composite extract and citral essential oil prepared in Preparation Example 1, magnetically stirring and mixing for 30 minutes, adding sodium chloride, and adjusting the internal composition to 2% citral essential oil, 10% composite extract, 18% beeswax, 2% sodium chloride, and 78% corn oil, stirring and mixing, vacuum defoaming, pouring into a shaping mold, cooling and shaping, and preparing the citral essential oil-based Sanxiangyuan antibacterial ointment.

[0071] Example 2

[0072] This Example 2 provides a method for preparing a citral essential oil-based Sanshool antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 2 is used.

[0073] Example 3

[0074] This Example 3 provides a preparation method of a citral essential oil-based Sanshool antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 3 is used.

[0075] Comparative Example 1 This comparative example 1 provides a method for preparing a citral essential oil-based Sanshool antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 4 is used.

[0076] Comparative Example 2 This comparative example 2 provides a method for preparing a citral essential oil-based Sanshool antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 5 is used.

[0077] Comparative Example 3 This comparative example 3 provides a preparation method of a citral essential oil-based Sanguisorba officinalis antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 6 is used.

[0078] Comparative Example 4 This comparative example 4 provides a preparation method of a citral essential oil-based Sanshool antibacterial ointment, which is different from Example 1 in that the composite extract prepared in Preparation Example 7 is used.

[0079] Performance Testing Based on the test method recorded in GB / T 13917.9-2009, the Shanxiangyuan antibacterial ointment prepared in Examples 1 to 3 and Comparative Examples 1 to 4 was tested. 200 female mosquitoes were placed in a mosquito net with a length × height × width of 40 cm × 40 cm × 40 cm. After they adapted to the environment and resumed normal activities, the experimenter exposed the back of their hands in the mosquito net. When the frequency of mosquitoes staying on the back of their hands reached 30 times within 5 minutes, the current experimenter was selected as having a mosquito attracting physique.

[0080] After applying Shanxiangyuan antibacterial ointment on the back of the left hand of the test subjects with mosquito attraction physique, the backs of both hands were placed on both sides of the mosquito net respectively, and it was recorded whether mosquitoes came over to suck blood. The test was conducted for 5 minutes every 30 minutes. The mosquito repellent rate of the left hand back in the first test and the duration of the mosquito repellent effect during the test were recorded. The results are shown in Table 1 below, where mosquito repellent rate = 1 - (number of mosquitoes on the left hand back ÷ number of mosquitoes on the right hand back) × 100%. If the number of mosquitoes on the left hand back was more than 30 during the test, it was determined that the mosquito repellent effect was ineffective.

[0081] Based on the test method described in GB / T 13917.9-2009, the anti-itching test was conducted on the antibacterial ointment of Examples 1 to 3 and Comparative Examples 1 to 4. After the back of the right hand of the test personnel who performed the mosquito repellent test was cleaned, the antibacterial ointment was applied on the back of the right hand to test how long it took to stop the itching. The results are shown in Table 1. The time point when the test personnel felt no itching was the time point when the itching was stopped, and the unit was s.

[0082] Based on the method described in Appendix C4 of GB15979-2002 "Sanitary Standards for Disposable Hygiene Products", the antibacterial performance test was performed using Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 6538, and the antibacterial results after 5 minutes of action are shown in Table 2. After the Shanxiangyuan antibacterial ointment prepared in Examples 1 to 3 and Comparative Examples 1 to 4 was continuously aged for 15 days in a 40°C light environment, the Shanxiangyuan antibacterial ointment was subjected to a mosquito repellent and antipruritic test, and the mosquito repellent attenuation rate and the antipruritic onset time attenuation rate after aging were calculated, and the results are shown in Table 1.

[0083] Table 1 The mosquito repellent and itching-relieving performance test of Shanxiangyuan antibacterial ointment

[0084] Table 2 Antibacterial performance test of Shanxiangyuan antibacterial ointment

[0085] As can be seen from Table 1 and Table 2, the antibacterial ointment prepared by the present invention has good antibacterial, antipruritic and mosquito repellent effects. Specifically, since the alcohol extraction residue was not subjected to supercritical extraction in Example 2, the content of the effective ingredients of yellow camphor and safflower in the antibacterial ointment was reduced, thereby affecting the mosquito repellent effect and the antipruritic onset time. In Example 3, yellow camphor and safflower were separately extracted and then mixed, which affected the mixing uniformity of the yellow camphor effective ingredients and safflower effective ingredients in the antibacterial ointment, thereby having a negative impact on the mosquito repellent effect and the performance stability of the antibacterial ointment.

[0086] In addition, dopamine was used for surface coating in Comparative Example 1, which also protected the active ingredients in the composite extract, but its protective effect was significantly weaker than that of tannic acid, and would affect the antibacterial performance of the antibacterial ointment. In Comparative Example 2, sassafras was used alone for extraction, and in Comparative Example 3, safflower was used alone for extraction, which greatly reduced the mosquito repellent effect and the antibacterial and antipruritic effects.

[0087] Although the embodiments of the present invention are described in detail above, it is obvious to those skilled in the art that various modifications and variations can be made to these embodiments. However, it should be understood that such modifications and variations are within the scope and spirit of the present invention as described in the claims. Moreover, the present invention described herein may have other embodiments and may be implemented or realized in a variety of ways.

Claims

1. A citral essential oil-based antibacterial ointment, characterized in that: The invention comprises, by mass percentage, 1%-3% citral essential oil, 8%-15% composite extract, 15%-20% bio-wax, 1%-3% defoaming agent and the remainder of vegetable oil; the extraction method of the composite extract comprises: mixed extraction of camphora leaves and safflower leaves to obtain a mixed extract, and tannic acid polymerized coating on the surface of the mixed extract to obtain a composite extract.

2. The antibacterial ointment according to claim 1, characterized in that: The sum of the relative contents of β-citral and α-citral in the citral essential oil is greater than 60.0%; and / or, the biowax includes beeswax; and / or, the defoaming agent includes one of sodium chloride and sodium sulfate; and / or, the vegetable oil includes one of camellia seed oil, camphor seed kernel oil, and olive oil.

3. The antibacterial ointment according to claim 1, characterized in that The preparation method of the composite extract comprises: mixing sassafras leaf powder and safflower leaf powder to obtain composite powder; performing alcohol extraction on the composite powder and separating the alcohol extract and alcohol extraction residue; performing supercritical extraction on the alcohol extraction residue and separating the extract; combining the alcohol extract and the extract and then concentrating by rotary evaporation to obtain a mixed extract; and performing tannic acid polymerization on the surface of the mixed extract to obtain the composite extract.

4. The antibacterial ointment according to claim 3, characterized in that: The sassafras leaf powder and the sassafras leaf powder are mixed and passed through a 50-60 mesh sieve, and the sieved material is collected to obtain a composite powder; and / or the water content of the composite powder is less than or equal to 10%; and / or the sassafras leaf powder and the sassafras leaf powder are mixed and preheated at 50° C.-70° C.; and / or the mass ratio of the sassafras leaf powder to the sassafras leaf powder is 1:(0.8-1.2).

5. The antibacterial ointment according to claim 3, characterized in that The composite powder is extracted in anhydrous ethanol for 6h-8h, and then the alcohol extract and the alcohol extraction residue are separated; wherein: the solid-liquid ratio of the composite powder and the anhydrous ethanol after mixing is 0.005g / mL-0.008g / mL; and / or, the composite powder is extracted in anhydrous ethanol in a closed environment at 50°C-70°C; and / or, the composite powder is ultrasonically dispersed in the anhydrous ethanol and stirred at a speed of 200rpm-300rpm and then extracted.

6. The antibacterial ointment according to claim 3, characterized in that The alcohol-extracted residue is subjected to supercritical extraction using carbon dioxide as a supercritical fluid; wherein: the alcohol-extracted residue is subjected to supercritical extraction using carbon dioxide for 2h-3h.

7. The antibacterial ointment according to claim 3, characterized in that: After combining the alcohol extract and the extraction liquid, heat them at 40° C.-45° C. for 1 h-2 h; and / or, after combining the alcohol extract and the extraction liquid, perform ultrasonic dispersion; and / or, after combining the alcohol extract and the extraction liquid, performing rotary evaporation concentration at 40° C.-50° C. and recovering the alcohol extraction solvent; and / or, performing rotary evaporation concentration and drying to obtain a mixed extract.

8. The antibacterial ointment according to claim 3, characterized in that The mixed extract is mixed in the tannic acid solution and a trimethylammonium hydrochloride buffer is added dropwise, followed by separation and drying to obtain a composite extract; wherein: the mass ratio of the mixed extract to the tannic acid in the tannic acid solution is 1:(0.02-0.05); and / or, the mixed extract is ultrasonically dispersed in the tannic acid solution; and / or, the pH of the trimethylammonium hydrochloride buffer is 8.

5.

9. A method for preparing the antibacterial ointment according to any one of claims 1 to 8, characterized in that: include: Heat and melt the biowax, add the vegetable oil and stir to mix, then add the citral essential oil and the composite extract and stir to mix for 30-40 minutes, add the defoaming agent and stir to mix, vacuum defoam, and then cool and shape to obtain an antibacterial ointment.

10. A use of the antibacterial ointment according to any one of claims 1 to 8, characterized in that: The applications include antibacterial and antipruritic effects.

Images