Preparation method of compound plant bacteriostatic composition

Abstract

The invention provides a preparation method of a compound plant antibacterial composition, which comprises the following steps: mixing 50-70 parts of propylene glycol, 10-20 parts of Australian tea tree essential oil in the step S1, 5-10 parts of sandalwood essential oil, 25-35 parts of cedar essential oil and 15-25 parts of grape seed oil, and stirring at room temperature for 40-60 minutes to obtain a mixed solution A; 2-5 parts of sodium hyaluronate and 5-8 parts of Tween 20 are stirred for 10-20 min at the room temperature, and a mixed solution B is obtained; and S3, stirring the mixed solution A obtained in the step S2 and the mixed solution B obtained in the step S3 at room temperature for 40-70 minutes, and standing for 3-6 hours to obtain the compound plant bacteriostatic composition. The composition has a remarkable inhibition effect on escherichia coli, staphylococcus aureus and tritirachium album, is mild and non-irritant, and is suitable for being widely applied to cosmetics.

Description

Technical Field

[0001] The invention belongs to the field of preparation of antibacterial products, and specifically relates to a method for preparing a compound plant antibacterial composition. Background Art

[0002] Essential oils are volatile aromatic substances extracted from the flowers, fruits, leaves, rhizomes and other parts of various plants through distillation, pressing, solvent extraction and other methods. They not only have unique aromas, but also have a variety of biological activities, including but not limited to antibacterial, anti-inflammatory, sedative, refreshing and other effects. Essential oils are widely used in aromatherapy, beauty and skin care, household cleaning, food seasoning, pharmaceuticals and other fields.

[0003] Patent CN106619438A discloses a plant-derived antibacterial agent and a hand soap and toothpaste containing the antibacterial agent. The antibacterial agent comprises the following Chinese herbal extracts in weight percentage: 30-90% of pomegranate peel extract, 5-30% of rhubarb extract, 5-20% of sophora flavescens extract, 1-10% of white peony extract, 1-10% of olive leaf extract, and 0.01-5% of propolis extract. The prepared plant-derived antibacterial agent can inhibit Gram-positive bacteria, Gram-negative bacteria, yeasts and anaerobic bacteria, and has a wide antibacterial spectrum. It is applied to toothpaste and hand soap, has a good preservative effect, can reduce the amount of chemical synthetic preservatives, thereby reducing the irritation of the product and improving the safety of the product.

[0004] With the in-depth study of the efficacy of essential oils, coupled with the high volatility and small molecules of essential oils, they are easily absorbed by the human body and can quickly penetrate into the organs of the human body, balancing the body's functions and beautifying the skin. The application of antibacterial plant essential oils is becoming more and more extensive, but the existing plant antibacterial products are not ideal in terms of antibacterial effects. Summary of the invention

[0005] The purpose of the present invention is to provide a method for preparing a compound plant antibacterial composition, by extracting Australian tea tree essential oil, sandalwood essential oil, cedar essential oil and grape seed oil as main components to prepare a pure natural plant antibacterial essential oil with good antibacterial effect and high safety.

[0006] In order to achieve the above object, the present invention provides the following technical solutions: A compound plant antibacterial composition comprises the following components in parts by weight: 10-20 parts of Australian tea tree essential oil, 5-10 parts of sandalwood essential oil, 25-35 parts of cedar essential oil and 15-25 parts of grape seed oil.

[0007] Furthermore, the composition also includes 3-8 parts of magnolol and 5-10 parts of sodium citrate.

[0008] Furthermore, the composition also includes 2-5 parts of sodium hyaluronate and 5-8 parts of Tween 20.

[0009] The preparation method of the above-mentioned compound plant antibacterial composition comprises the following steps: S1: prepare Australian tea tree essential oil, sandalwood essential oil, cedarwood essential oil and grape seed oil respectively; S2: Mix 50-70 parts of propylene glycol, 10-20 parts of Australian tea tree essential oil, 5-10 parts of sandalwood essential oil, 25-35 parts of cedar essential oil and 15-25 parts of grape seed oil described in step S1, and stir at room temperature for 40-60 minutes to obtain a mixed solution A; S3: Stir 2-5 parts of sodium hyaluronate and 5-8 parts of Tween 20 at room temperature for 10-20 minutes to obtain a mixed solution B; S4: Stir the mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 at room temperature for 40-70 minutes and let stand for 3-6 hours to obtain the compound plant antibacterial composition.

[0010] Furthermore, the preparation process of the Australian tea tree essential oil in step S1 is: take the Australian tea tree raw material, wash and dry it for use, add distilled water thereto at a solid-liquid ratio of 1g:10-15ml, soak it for 4-6h, then heat and extract it at 110-130℃ for 3-5h, take the volatile oil, dry it with anhydrous sodium sulfate, and filter it to obtain the Australian tea tree essential oil.

[0011] Furthermore, the preparation process of the sandalwood essential oil in step S1 is as follows: weighing a cleaned and dried sandalwood raw material; adding distilled water to one end of a simultaneous distillation extraction device at a solid-liquid ratio of 1g:12-16ml, and heating to a slight boil; adding anhydrous ether to the other end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:7-10ml, and distilling and extracting at a temperature of 80-85°C for 4-6h; drying the extract over anhydrous sodium sulfate, and removing the anhydrous ether with a rotary evaporator to obtain sandalwood essential oil.

[0012] Furthermore, the preparation process of the cedar essential oil in step S1 is: taking cedar bark, drying and crushing it, and then performing supercritical CO2 extraction, using ethanol as a carrier, extracting for 1-3 hours at a temperature of 65-75°C and a pressure of 20-35MPa; the extract is rotary evaporated and dried to obtain cedar essential oil.

[0013] Furthermore, the preparation process of the grape seed oil in step S1 is as follows: taking the grape seed raw material, washing, drying, and crushing it for later use, adding ethanol solution thereto at a solid-liquid ratio of 1g:15-20ml, extracting at 80-100°C for 4-6h, and then drying with anhydrous sodium sulfate and filtering to obtain grape seed essential oil.

[0014] Furthermore, in step S4, the mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 are stirred at room temperature for 10-20 minutes, and then 3-8 parts of magnolol and 5-10 parts of sodium citrate are added and stirred for 30-50 minutes, and the mixture is allowed to stand for 3-6 hours to obtain the compound plant antibacterial composition.

[0015] The prepared compound plant antibacterial composition is applied in cosmetic products.

[0016] Australian tea tree essential oil is a natural essential oil extracted from the leaves of the Australian tea tree. It is known for its powerful antibacterial, anti-inflammatory and antifungal properties and is widely used in many fields such as personal care, household cleaning and healthcare. Its main components are terpenes: such as 1,8-cineole, which has significant antibacterial and anti-inflammatory effects; monoterpene alcohols: such as α-terpineol and γ-terpineol, which also have antibacterial activity; monoterpenes: such as α-pinene and β-pinene, which give tea tree essential oil its unique aroma.

[0017] Sandalwood essential oil is a precious essential oil extracted from sandalwood. Sandalwood is mainly produced in India, Indonesia and Australia, and is highly respected for its unique aroma and multiple benefits. Sandalwood essential oil is widely used in many fields such as aromatherapy, beauty and skin care, religious ceremonies and personal care. Main ingredients: Santalinol gives sandalwood essential oil a unique aroma and multiple benefits; santalene also has antibacterial and anti-inflammatory effects.

[0018] Cedarwood essential oil is a natural essential oil extracted from the wood of cedar trees. With its unique woody aroma and multiple benefits, cedarwood essential oil is widely used in aromatherapy, personal care, household cleaning, and healthcare. Its main ingredients: cedarol, an important monoterpene alcohol, gives cedarwood essential oil its unique aroma and has antibacterial and anti-inflammatory effects; cedrene, a monoterpene that helps enhance the antibacterial properties of cedarwood essential oil.

[0019] Grapeseed oil is a natural vegetable oil extracted from grape seeds, which has rich nutritional value and multiple health benefits. It is not only used as a healthy cooking oil in cooking, but also widely used in beauty and skin care, health products and natural therapies. Its main ingredients such as unsaturated fatty acids, mainly linoleic acid (about 70%), which is an Omega-6 polyunsaturated fatty acid; vitamin E: has a strong antioxidant effect and helps protect cells from free radical damage; polyphenolic compounds: such as proanthocyanidins (OPCs), these compounds have antioxidant, anti-inflammatory and anti-allergic effects.

[0020] Compared with the prior art, the advantages and beneficial effects of the present invention are: The invention takes Australian tea tree, sandalwood, cedar and grape as main components, and adopts steam method, simultaneous distillation extraction method, supercritical carbon dioxide extraction method, ethanol extraction method and the like according to different characteristics to obtain Australian tea tree essential oil, sandalwood essential oil, cedar essential oil and grape essential oil, etc., and the obtained essential oil components have high effective component content; the above essential oil products are used as main components as a plant antibacterial composition, and a synergistic antibacterial effect is exerted, and a good inhibitory effect is achieved on Gram-positive bacteria, Gram-negative bacteria, fungi and the like; the plant antibacterial composition product is mild, safe, non-irritating and does not harm human skin. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. 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.

[0022] Example 1 This embodiment provides a method for preparing a compound plant antibacterial composition, comprising the following steps: S1: Take the Australian tea tree raw material, wash and dry it for later use, add distilled water into it according to the solid-liquid ratio of 1g:10ml, soak it for 4h, then heat and extract it at 110℃ for 3h, take the volatile oil and dry it with anhydrous sodium sulfate, filter it to obtain the Australian tea tree essential oil; Weigh the cleaned and dried sandalwood raw material; add distilled water to one end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:12ml, and heat to a slight boil; add anhydrous ether to the other end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:7ml, and distill and extract at a temperature of 80°C for 4h; dry the extract over anhydrous sodium sulfate, remove the anhydrous ether with a rotary evaporator, and obtain sandalwood essential oil; Take cedar bark, dry and crush it, and then extract it with supercritical CO2, using ethanol as a carrier, and extract it at a temperature of 65°C and a pressure of 20MPa for 1 hour; the extract is subjected to rotary evaporation to remove ethanol and dried to obtain cedar essential oil; The grape seed raw material is washed, dried, and crushed for later use, and an ethanol solution is added thereto at a solid-liquid ratio of 1g:15ml, and the mixture is extracted at 80°C for 4h, and then dried over anhydrous sodium sulfate and filtered to obtain grape seed essential oil; S2: Mix 50 g of propylene glycol, 10 g of Australian tea tree essential oil, 5 g of sandalwood essential oil, 25 g of cedar essential oil and 15 g of grape seed oil described in step S1, and stir at room temperature at a rate of 700 r / min for 40 min to obtain a mixed solution A; S3: 2 g of sodium hyaluronate and 5 g of Tween 20 were stirred at room temperature at a rate of 500 r / min for 10 min to obtain a mixed solution B; S4: The mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 are stirred at room temperature at a rate of 800 r / min for 40 min and allowed to stand for 3 h to obtain the compound plant antibacterial composition.

[0023] Example 2 This embodiment provides a method for preparing a compound plant antibacterial composition, comprising the following steps: S1: Take the Australian tea tree raw material, wash and dry it for later use, add distilled water into it at a solid-liquid ratio of 1g:15ml, soak it for 6h, then heat and extract it at 130℃ for 5h, take the volatile oil and dry it with anhydrous sodium sulfate, and filter it to obtain the Australian tea tree essential oil; Weigh the cleaned and dried sandalwood raw material; add distilled water to one end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:16ml, and heat to a slight boil; add anhydrous ether to the other end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:10ml, and distill and extract at a temperature of 85°C for 6h; dry the extract over anhydrous sodium sulfate, remove the anhydrous ether with a rotary evaporator, and obtain sandalwood essential oil; Take cedar bark, dry and crush it, and then perform supercritical CO2 extraction, use ethanol as a carrier, and extract for 3 hours at a temperature of 75°C and a pressure of 35MPa; the extract is subjected to rotary evaporation to remove ethanol and dried to obtain cedar essential oil; The grape seed raw material is washed, dried, and crushed for later use, and an ethanol solution is added thereto at a solid-liquid ratio of 1g:20ml, and the mixture is extracted at 100°C for 6h, and then dried over anhydrous sodium sulfate and filtered to obtain grape seed essential oil; S2: Mix 70 g of propylene glycol, 20 g of Australian tea tree essential oil, 10 g of sandalwood essential oil, 35 g of cedar essential oil and 25 g of grape seed oil described in step S1, and stir at room temperature at a rate of 500 r / min for 60 min to obtain a mixed solution A; S3: 5 g of sodium hyaluronate and 8 g of Tween 20 were stirred at room temperature at a rate of 550 r / min for 20 min to obtain a mixed solution B; S4: The mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 are stirred at room temperature at a rate of 600 r / min for 70 min and allowed to stand for 6 h to obtain the compound plant antibacterial composition.

[0024] Example 3 This embodiment provides a method for preparing a compound plant antibacterial composition, comprising the following steps: S1: Take the Australian tea tree raw material, wash and dry it for later use, add distilled water into it at a solid-liquid ratio of 1g:12ml, soak it for 5h, then heat and extract it at 120℃ for 4.5h, take the volatile oil and dry it with anhydrous sodium sulfate, filter it to obtain the Australian tea tree essential oil; Weigh the cleaned and dried sandalwood raw material; add distilled water to one end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:14ml, and heat to a slight boil; add anhydrous ether to the other end of the simultaneous distillation extraction device at a solid-liquid ratio of 1g:8ml, and distill and extract at a temperature of 82°C for 5.5h; dry the extract over anhydrous sodium sulfate, remove the anhydrous ether with a rotary evaporator, and obtain sandalwood essential oil; Take cedar bark, dry and crush it, and then perform supercritical CO2 extraction, use ethanol as a carrier, and extract it at a temperature of 70°C and a pressure of 30MPa for 2.5 hours; the extract is subjected to rotary evaporation to remove ethanol and dried to obtain cedar essential oil; The grape seed raw material is washed, dried, and crushed for later use, and an ethanol solution is added thereto at a solid-liquid ratio of 1g:18ml, and the mixture is extracted at 90°C for 5.5h, and then dried over anhydrous sodium sulfate and filtered to obtain grape seed essential oil; S2: Mix 60 g of propylene glycol, 15 g of Australian tea tree essential oil, 8 g of sandalwood essential oil, 30 g of cedar essential oil and 22 g of grape seed oil, and stir at room temperature at a rate of 600 r / min for 50 min to obtain a mixed solution A; S3: 4 g of sodium hyaluronate and 7 g of Tween 20 were stirred at room temperature at a rate of 500 r / min for 15 min to obtain a mixed solution B; S4: The mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 were stirred at room temperature at a rate of 500 r / min for 15 min, 6 g of magnolol and 7 g of sodium citrate were added, stirring was continued for 45 min, and the mixture was allowed to stand for 5 h to obtain the compound plant antibacterial composition.

[0025] Comparative Example 1 Blank control.

[0026] Comparative Example 2 The difference from Example 3 is that only Australian tea tree essential oil is added in step S2, and the other steps remain unchanged.

[0027] Comparative Example 3 The difference from Example 3 is that only sandalwood essential oil is added in step S2, and the other steps remain unchanged.

[0028] Comparative Example 4 The difference from Example 3 is that only cedar essential oil is added in step S2, and the other steps remain unchanged.

[0029] Comparative Example 5 The difference from Example 3 is that only grape seed oil is added in step S2, and the other steps remain unchanged.

[0030] Performance test: antibacterial property. Bacterial suspension: After the Escherichia coli freeze-dried powder is coated on the plate, it is inverted at 37℃ for 24h; the next day, a single colony is inoculated into 100ml nutrient agar liquid medium and cultured at 37℃ for 24h; according to this method, the bacterial suspension is obtained after the fifth generation of Escherichia coli. Staphylococcus aureus and Candida albicans bacterial suspensions are prepared in the same way. The number of Escherichia coli colonies is 4.13×10 4 cfu / ml, the colony count of Staphylococcus aureus was 5.56×10 4 cfu / ml, the colony count of Candida albicans was 3.67×10 4 cfu / ml.

[0031] Nutrient agar liquid medium: 8g peptone, 3g sodium chloride, 3g beef extract, add 800ml water to dissolve, sterilize at 118℃ for 15min. Nutrient agar solid medium: 8g peptone, 3g sodium chloride, 3g beef extract, 15g agar, add 800ml water to dissolve; sterilize at 118℃ for 15min. Sabouraud solid medium: 8g peptone, 15g agar, 30g glucose, distilled water to 1L, 115℃ 20min high pressure steam sterilization. Performance test: Take 5ml of the antibacterial composition obtained in each embodiment and comparative example and place them in sterile test tubes, add 100μl of Escherichia coli, Staphylococcus aureus and Candida albicans suspension, mix evenly, and start timing for 20min; test the antibacterial rate; the results are as shown in the following table.

[0032] Table 1

[0033] From the above performance test results, it can be seen that Examples 1-3 have significant inhibitory effects on Escherichia coli, Staphylococcus aureus and Candida albicans. In particular, the comprehensive performance of Example 3 is the most outstanding. However, since Comparative Examples 1-5 do not adopt the necessary technical solutions, their corresponding performance tests are significantly worse than those of the Examples. The above experimental results further prove the importance of the technical solutions defined in the present invention for its technical effects.

[0034] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A compound plant antibacterial composition, characterized in that: The invention comprises the following components in parts by weight: 10-20 parts of Australian tea tree essential oil, 5-10 parts of sandalwood essential oil, 25-35 parts of cedar essential oil and 15-25 parts of grape seed oil.

2. A compound plant antibacterial composition according to claim 1, characterized in that: The composition also includes 3-8 parts of magnolol and 5-10 parts of sodium citrate.

3. A compound plant antibacterial composition according to claim 2, characterized in that: The composition also includes 2-5 parts of sodium hyaluronate and 5-8 parts of Tween 20.

4. A method for preparing a compound plant antibacterial composition, characterized in that: The steps include: S1: prepare Australian tea tree essential oil, sandalwood essential oil, cedarwood essential oil and grape seed oil respectively; S2: Mix 50-70 parts of propylene glycol, 10-20 parts of Australian tea tree essential oil, 5-10 parts of sandalwood essential oil, 25-35 parts of cedar essential oil and 15-25 parts of grape seed oil described in step S1, and stir at room temperature for 40-60 minutes to obtain a mixed solution A; S3: Stir 2-5 parts of sodium hyaluronate and 5-8 parts of Tween 20 at room temperature for 10-20 minutes to obtain a mixed solution B; S4: Stir the mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 at room temperature for 40-70 minutes and let stand for 3-6 hours to obtain the compound plant antibacterial composition.

5. The method for preparing a compound plant antibacterial composition according to claim 4, characterized in that: The preparation process of the Australian tea tree essential oil in step S1 is as follows: take the Australian tea tree raw material, wash and dry it for later use, add distilled water thereto at a solid-liquid ratio of 1g:10-15ml, soak it for 4-6h, then heat and extract it at 110-130℃ for 3-5h, take the volatile oil and dry it with anhydrous sodium sulfate, and filter it to obtain the Australian tea tree essential oil.

6. The method for preparing a compound plant antibacterial composition according to claim 4, characterized in that: The preparation process of the sandalwood essential oil in step S1 is as follows: weighing a cleaned and dried sandalwood raw material; adding distilled water to one end of a simultaneous distillation extraction device according to a solid-liquid ratio of 1g:12-16ml, and heating to a slight boil; adding anhydrous ether to the other end of the simultaneous distillation extraction device according to a solid-liquid ratio of 1g:7-10ml, and distilling and extracting at a temperature of 80-85°C for 4-6h; drying the extract over anhydrous sodium sulfate, and removing the anhydrous ether with a rotary evaporator to obtain the sandalwood essential oil.

7. The method for preparing a compound plant antibacterial composition according to claim 4, characterized in that: The preparation process of the cedar essential oil in step S1 is as follows: taking cedar bark, drying and crushing it, and then extracting it with supercritical CO2, using ethanol as a carrier, extracting it at a temperature of 65-75°C and a pressure of 20-35MPa for 1-3h; the extract is rotary evaporated and dried to obtain the cedar essential oil.

8. The method for preparing a compound plant antibacterial composition according to claim 4, characterized in that: The preparation process of grape seed oil in step S1 is as follows: taking grape seed raw materials, washing, drying, and crushing them for later use, adding ethanol solution thereto at a solid-liquid ratio of 1g:15-20ml, extracting at 80-100°C for 4-6h, and then drying with anhydrous sodium sulfate and filtering to obtain grape seed essential oil.

9. The method for preparing a compound plant antibacterial composition according to claim 4, characterized in that: In step S4, the mixed solution A obtained in step S2 and the mixed solution B obtained in step S3 are stirred at room temperature for 10-20 minutes, and then 3-8 parts of magnolol and 5-10 parts of sodium citrate are added and stirred for 30-50 minutes, and then allowed to stand for 3-6 hours to obtain the compound plant antibacterial composition.

10. Use of the compound plant antibacterial composition prepared according to any of claims 1 to 9 in cosmetic products.

Images