Preparation process of pure plant essential oil disinfectant

Abstract

The invention discloses a preparation process of a pure plant essential oil disinfectant, and relates to the technical field of disinfectants. The problems that plant essential oil is poor in solubility in a water phase, low in stability and the like are solved. The method specifically comprises the following steps: preparing raw materials; preparing a nano emulsion; preparing a solvent and mixing; constructing a natural stable system to obtain a primary product; filtering and sterilizing; and carrying out sterile filling on the disinfectant finished product. The invention provides a pure plant essential oil disinfectant prepared by dissolving type 1 and 8 melaleuca alternifolia essential oil in water, efficient dispersion is realized through a nano-emulsification and natural stabilization technology so as to form a stable aqueous solution, an amphiphilic structure of soapbark saponin is utilized, aglycone and essential oil terpene form a supramolecular compound, and the stable aqueous solution can be used for sterilizing the melaleuca alternifolia essential oil and the melaleuca alternifolia essential oil and the melaleuca alternifolia essential oil. The technical problems of poor dissolvability and low stability of plant essential oil in a water phase are solved, and the plant essential oil has broad-spectrum antibacterial and antiviral characteristics and can meet the disinfection requirements in multiple fields such as medical treatment, object surface treatment, home furnishing and personal care.

Description

Technical Field

[0001] This invention relates to the field of disinfectant technology, and in particular to a preparation process for a pure plant essential oil disinfectant. Background Technology

[0002] With rapid social development and progress, and the increasing awareness of environmental protection and the quality of life, disinfection technology is facing severe challenges. Inorganic and organic disinfectants, collectively known as chemical disinfectants, while possessing some disinfection effects, are not safe to use, exhibiting certain toxic side effects and compound residues, which are detrimental to both human health and the environment. In contrast, plant-based disinfectants have natural advantages. They are made from effective bactericidal components extracted from natural plants or medicinal herbs, and have been used in my country for thousands of years. For example, ancient people used mugwort and calamus to ward off plagues, and perilla and camphor to repel foul odors and kill insects. They are highly effective, non-irritating, residue-free, and have good environmental compatibility.

[0003] Melaleuca alternifolia is a plant of the Myrtaceae family native to Australia. Its essential oil is mainly classified into three chemical types: 1,8-cineole, terpineol-4, and intermediate. Among them, the 1,8-cineole essential oil has attracted widespread attention due to its outstanding antibacterial and anti-inflammatory effects; studies have shown that it has significant inhibitory effects on various bacteria, fungi, and viruses. However, traditional Melaleuca alternifolia essential oil disinfectant products face the following technical bottlenecks: 1. Poor water solubility of the essential oil: The main components of Melaleuca alternifolia essential oil are terpenoid compounds (1,8-cineole, α-terpineol, etc.), which have low water solubility (usually <0.1%), making it difficult to form a stable aqueous solution;

[0004] 2. Volatile active ingredients: Monoterpenoids in essential oils are easily oxidized and volatilized, resulting in a short product shelf life;

[0005] 3. Highly irritating: Direct contact with the skin may cause irritation.

[0006] Based on this, we propose a preparation process for a pure plant essential oil disinfectant that dissolves type 1,8 Melaleuca alternifolia essential oil in water. This process solves the technical problems of poor solubility and low stability of plant essential oils in aqueous phase. It has broad-spectrum antibacterial and antiviral properties and can be applied to disinfection needs in multiple fields such as medical treatment, surface treatment, home care, and personal care. Summary of the Invention

[0007] The purpose of this invention is to address the shortcomings of existing technologies by proposing a preparation process for a pure plant essential oil disinfectant.

[0008] To achieve the above objectives, the present invention adopts the following technical solution:

[0009] A preparation process for a pure plant essential oil disinfectant includes the following steps:

[0010] S1: Raw material preparation: Melaleuca alternifolia essential oil, soap bark extract, food-grade propylene glycol, citric acid, trehalose, xanthan gum, and deionized water;

[0011] S2: Preparation of nanoemulsion;

[0012] S3: Solvent preparation and mixing;

[0013] S4: Construct a natural and stable system to obtain the initial product;

[0014] S5: Filtration and sterilization treatment;

[0015] S6: Aseptic filling of the disinfectant solution;

[0016] The essential oil of Melaleuca alternifolia is of type 1,8, and the content of 1,8-cineole in the essential oil is ≥60%.

[0017] Preferably, the food-grade propylene glycol is obtained from plant fermentation and has a purity of ≥99.5%;

[0018] The citric acid is obtained from extraction from natural citrus fruits;

[0019] The xanthan gum is obtained from microbial fermentation;

[0020] The conductivity of the deionized water is ≤5μS / cm.

[0021] Preferred method for preparing the nanoemulsion is as follows:

[0022] A1: Premix: Mix Melaleuca alternifolia essential oil with soap bark extract preheated to 60°C and stir magnetically for 10 minutes to form a pre-emulsion;

[0023] A2: High-pressure homogenization: A microfluidic nano-homogenizer was used at a pressure of 15000psi for 3 cycles to obtain a nanoemulsion with a particle size of <100nm.

[0024] Preferably, the amount of Melaleuca alternifolia essential oil added is 0.5-0.8 mL;

[0025] The soap bark extract is a 5% aqueous solution, and the amount of soap bark extract added is 0.4 mL;

[0026] The preemulsion has an HLB value in the range of 12-14.

[0027] Preferred method: The solvent is prepared by first adding deionized water to the preparation tank, then slowly adding food-grade propylene glycol, and finally stirring at 20-30°C until completely dissolved.

[0028] The method for preparing the solvent also includes filtering the solution through a 0.22 μm microporous membrane.

[0029] Preferred method for constructing the naturally stable system is as follows:

[0030] B1: Add 1% trehalose and 0.1% xanthan gum, stir at low speed at 45℃ for 2 hours to form a three-dimensional network structure;

[0031] B2: Adjust the pH to 4.0-5.0 with citric acid.

[0032] Preferably, the amount of citric acid added is 0.2g.

[0033] Preferably, the filtration and sterilization method uses a 0.22μm ceramic membrane.

[0034] Preferably, the filling process involves irradiating the product with ultraviolet light for 15 minutes, with the ultraviolet wavelength being 54nm.

[0035] Preferably, in step S3, 0.5% natural vitamin E is added to the solution.

[0036] The beneficial effects of this invention are as follows:

[0037] This invention proposes a process for preparing a pure plant essential oil disinfectant solution by dissolving 1,8-type Melaleuca alternifolia essential oil in water. The process utilizes nanoemulsification and natural stabilization techniques to achieve efficient dispersion and form a stable aqueous solution. Taking advantage of the amphiphilic structure of saponins from the bark, the aglycones form supramolecular complexes with the essential oil terpenes. The addition of propylene glycol effectively enhances the hydration capacity of 1,8-cineole, solving the technical problems of poor solubility and low stability of plant essential oils in aqueous phases. This solution possesses broad-spectrum antibacterial and antiviral properties and can be applied to disinfection needs in multiple fields such as medical treatment, surface treatment, home care, and personal care. Attached Figure Description

[0038] Figure 1 This is a schematic diagram of the preparation process of a pure plant essential oil disinfectant proposed in this invention.

[0039] Figure 2 This is a schematic diagram showing the bactericidal test results of the diluted product of the present invention against Staphylococcus aureus in Test Example 1.

[0040] Figure 3 This is a schematic diagram showing the bactericidal test results of the diluted product of the present invention against Pseudomonas aeruginosa in Test Example 2.

[0041] Figure 4 This is a schematic diagram showing the bactericidal test results of the diluted product of the present invention against Candida albicans in Test Example 3.

[0042] Figure 5 This is a schematic diagram showing the bactericidal test results of the product of the present invention on natural bacteria on the skin surface of 30 people in Test Example 4.

[0043] Figure 6 This is a schematic diagram showing the results of an acute eye irritation test performed on the product of the present invention in Test Example 5. Detailed Implementation

[0044] The technical solution of this patent will be further described in detail below with reference to specific embodiments.

[0045] The embodiments of this patent are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this patent, and should not be construed as limiting this patent.

[0046] Example 1:

[0047] A preparation process for a pure plant essential oil disinfectant, such as... Figure 1 As shown, it includes the following steps:

[0048] S1: Raw material preparation: Melaleuca alternifolia essential oil, soap bark extract, food-grade propylene glycol, citric acid, trehalose, xanthan gum, and deionized water;

[0049] Preferably, the essential oil of Melaleuca alternifolia is of type 1,8 Melaleuca alternifolia, and the content of 1,8-cineole in the essential oil of Melaleuca alternifolia is ≥60%.

[0050] Preferably, the food-grade propylene glycol is obtained from plant fermentation, and the purity of E1520 food-grade propylene glycol is ≥99.5%, free from heavy metal and microbial contamination. When used as a natural cosolvent, it must comply with FDA 21 CFR 184.1666 or GB 29216-2012 standards.

[0051] Preferably, citric acid is obtained from extraction from natural citrus fruits.

[0052] Preferably, xanthan gum is obtained from microbial fermentation.

[0053] Preferably, the conductivity of deionized water is ≤5μS / cm, the microbial limits meet the standards of the Chinese Pharmacopoeia or USP, and endotoxins are tested regularly (e.g., for use in highly sensitive foods).

[0054] S2: Preparation of nanoemulsion;

[0055] Furthermore, the preparation method of the nanoemulsion is as follows:

[0056] A1: Premix: Mix Melaleuca alternifolia essential oil with soap bark extract preheated to 60°C and stir magnetically for 10 minutes to form a pre-emulsion;

[0057] Preferably, the amount of Melaleuca alternifolia essential oil added is 0.5-0.8 mL;

[0058] Preferably, the soap bark extract is a 5% aqueous solution, and the amount of soap bark extract added is 0.4 mL;

[0059] Preferably, the HLB value of the pre-emulsion is in the range of 12-14.

[0060] A2: High-pressure homogenization: A microfluidic nano-homogenizer was used at a pressure of 15000psi for 3 cycles to obtain a nanoemulsion with a particle size of <100nm.

[0061] Preferably, the dynamic light scattering DLS detection PDI < 0.2.

[0062] S3: Solvent preparation and mixing;

[0063] Furthermore, the solvent is prepared by first adding deionized water to a preparation tank, then slowly adding food-grade propylene glycol to avoid excessively high local concentrations, and finally stirring at 20-30°C until completely dissolved.

[0064] Preferably, the ratio of deionized water to food-grade propylene glycol can be adjusted according to the application, with propylene glycol at 5%-15% being a further preferred ratio.

[0065] More preferably, the method for preparing the solvent further includes filtering the solution through a 0.22 μm microporous membrane to avoid microbial contamination.

[0066] S4: Construct a natural and stable system to obtain the initial product;

[0067] Furthermore, the construction method of the naturally stable system is as follows:

[0068] B1: Add 1% trehalose and 0.1% xanthan gum to the preparation tank and stir at low speed at 45°C for 2 hours to form a three-dimensional network structure;

[0069] B2: Adjust the pH to 4.0-5.0 with citric acid; enhance antibacterial properties and prevent hydrolysis.

[0070] Preferably, the amount of citric acid added is 0.2g.

[0071] As an alternative, citric acid can be replaced with sodium bicarbonate.

[0072] S5: Filtration and sterilization treatment;

[0073] Preferably, the filtration and sterilization method uses a 0.22μm ceramic membrane;

[0074] S6: Aseptic filling of the disinfectant solution;

[0075] Preferably, the disinfectant solution is irradiated with ultraviolet light for 15 minutes before being filled, with the ultraviolet wavelength being 54nm.

[0076] Preferred quality testing standards require: 1,8-cineole content GC-MS ≥ 30%, total essential oil content, particle size distribution, dynamic light scattering D50 < 100 nm, PDI < 0.25, antibacterial effect ISO 20743, Escherichia coli kill rate ≥ 99.9%, stability centrifugation test (4000 rpm × 30 min) with no oil phase separation.

[0077] In a further preferred embodiment, the disinfectant solution must be allowed to stand for 48 hours before aseptic filling to confirm that there is no stratification or sedimentation.

[0078] This invention preferably uses type 1,8 Melaleuca alternifolia essential oil as the main bactericidal component, natural emulsifier soap bark extract, natural solubilizer food-grade propylene glycol, and natural stabilizer trehalose, etc., to achieve efficient dispersion through nano-emulsification and natural stabilization technology, thereby forming a stable aqueous solution, which has a killing effect on common bacteria such as Staphylococcus aureus, Escherichia coli, Candida albicans, Pseudomonas aeruginosa, Bacillus subtilis, Mycobacterium, and natural bacteria on the surface of human skin.

[0079] This invention employs natural nanoemulsification technology, utilizing the amphiphilic structure of saponins from soap bark, where the aglycones form supramolecular complexes with essential oil terpenes; the addition of propylene glycol effectively enhances the hydration capacity of 1,8-cineole.

[0080] This invention employs a dual stabilization mechanism: graph LR A [essential oil nanodrops] --> B [saponin interface film] A --> C [trehalose glassy state protection] B --> D (electrostatic stabilization) C --> E (steric hindrance).

[0081] This invention employs a synergistic bactericidal system: the bactericidal efficiency of 1,8-cineole is increased by 3.5-6 times under acidic pH conditions; and the trace upregulation of α-terpineol (a natural component of essential oils) can disrupt microbial biofilms.

[0082] Example 2:

[0083] A preparation process for a pure plant essential oil disinfectant, in order to extend the shelf life of the disinfectant; this embodiment makes the following improvements based on embodiment 1: it further includes adding 0.5% natural vitamin E (tocopherol) after step S3 to extend the shelf life to 18 months.

[0084] Preferably, the production environment must meet ISO Class 8 cleanliness standards.

[0085] In this embodiment, the essential oil is completely water-soluble through physical nano-sizing and plant-based supramolecular complex. The resulting disinfectant has a transmittance of >90% (600nm wavelength), which meets medical-grade disinfection requirements and also satisfies organic product certification standards.

[0086] Experimental Example 1:

[0087] The product of this invention was diluted 1:1 with sterile hard water and subjected to a quantitative bactericidal suspension test. The action times were 2.5 min, 5 min and 7.5 min, respectively, and the test temperature was 20℃ ± 1℃.

[0088] Environmental conditions: temperature 21℃~22℃, relative humidity 49%~53%, the test was repeated 3 times.

[0089] Test parameters are shown in Figure 2 Results: The kill log value of Staphylococcus aureus in each test after 5 min of disinfection was ≥5.00.

[0090] Experimental Example 2:

[0091] The product of this invention was diluted 1:1 with sterile hard water and subjected to a quantitative bactericidal suspension test. The action times were 2.5 min, 5 min and 7.5 min, respectively, and the test temperature was 20℃ ± 1℃.

[0092] Environmental conditions: temperature 21℃~22℃, relative humidity 49%~52%, the test was repeated 3 times.

[0093] Test parameters are shown in Figure 3 Results: The kill log value of Pseudomonas aeruginosa in each test after 5 min of disinfection was ≥5.00.

[0094] Experimental Example 3:

[0095] The product of this invention was diluted 1:1 with sterile hard water and subjected to a quantitative bactericidal suspension test. The action times were 2.5 min, 5 min and 7.5 min, respectively, and the test temperature was 20℃ ± 1℃.

[0096] Environmental conditions: temperature 21℃~23℃, relative humidity 50%~54%, the test was repeated 3 times.

[0097] Test parameters are shown in Figure 4 Results: After 5 minutes of disinfection, the log killing value of Candida albicans in each test was ≥4.00.

[0098] Experimental Example 4:

[0099] Preparation before the experiment:

[0100] 1) Neutralizing agent: PBS containing 0.5% sodium thiosulfate, 0.2% lecithin, and 2.0% Tween-80;

[0101] 2) Culture medium: Tryptone soybean agar (TSA);

[0102] 3) The product of this invention was diluted 1:1 with sterile hard water and then tested;

[0103] Environmental conditions: Temperature 22℃~23℃, relative humidity 49%~51%.

[0104] Experiment: Thirty subjects were selected for a field disinfection experiment. Specifically: Before disinfection, subjects rubbed the mid-section of the inner forearms of both hands together thoroughly. A standard board (made of kraft paper with a 3.0cm x 10.0cm space in the center as the sampling site) was placed on the mid-section of the inner forearm of the subject's left forearm. The mid-section of the inner forearm of the left forearm was disinfected with disinfectant for 5 minutes. The sample was then collected with a neutralizing agent and used as the experimental group sample. The mid-section of the inner forearm of the right forearm was not disinfected, but the sample was collected with a diluent and used as the positive control group sample. The same batch of neutralizing agent and diluent was inoculated into a culture medium and used as the negative control group sample.

[0105] Test parameters are shown in Figure 5 Results: After 5 minutes of disinfection, the average log kill value of natural bacteria on the skin surface of 30 people was ≥1.00 in each test.

[0106] Experimental Example 5:

[0107] Experimental subjects: Three adult female Japanese white rabbits (with no abnormalities in either eye) of ordinary grade, provided by Hubei Yizhicheng Biotechnology Co., Ltd., were selected.

[0108] Test method: Direct eye drops;

[0109] Experimental steps:

[0110] 1) Take 0.1 ml of the original sample of this invention and instill it into the conjunctival sac of one eye of a Japanese white rabbit with large ears, while using physiological saline as a normal control on the other side;

[0111] 2) After instilling the test substance, the eye was passively closed for 4 seconds. After 30 seconds, the eye was rinsed with physiological saline at 1 hour, 24 hours, 48 ​​hours and 72 hours after instillation. The damage to the conjunctiva, iris and cornea of ​​the Japanese white rabbit was then observed with the naked eye.

[0112] Test results: The acute eye irritation test response scores of this invention were: cornea 0, iris 0, conjunctival hyperemia 0, and conjunctival edema 0, indicating no irritation. Detailed parameters can be found in [link to detailed parameters]. Figure 6 .

[0113] Note: The testing and evaluation of test examples 1-4 are based on GB / T 38502-2020 "Laboratory Test Methods for the Sterilization Efficacy of Disinfectants" and "Disinfection Technical Specifications" (2002 edition);

[0114] The testing and evaluation of Experiment Example 5 were based on Section 2.3.4 of the "Disinfection Technical Specifications" (2002 edition).

[0115] Comparative Example 1:

[0116] The bactericidal and disinfectant effects of 0.3% and 0.7% concentrations of 1,8-cineole-type Melaleuca alternifolia essential oil were compared, and the results are shown in the table below:

[0117]

[0118] As shown above, for Staphylococcus aureus, a 0.7% concentration has stronger penetrating power and cell membrane disruption ability against stubborn bacteria. For Escherichia coli, a 0.7% concentration is particularly effective against bacteria within biofilms. For fungi (such as Candida albicans), spores may survive at a 0.3% concentration, but a 0.7% concentration can destroy the fungal cell wall. For enveloped viruses (such as influenza virus and SARS-CoV-2), a high concentration of 0.7% is more efficient at disrupting the viral lipid envelope. A 0.7% concentration can shorten the disinfection time by more than 50%.

[0119] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A preparation process for a pure plant essential oil disinfectant, characterized in that, Includes the following steps: S1: Raw material preparation: Melaleuca alternifolia essential oil, soap bark extract, food-grade propylene glycol, citric acid, trehalose, xanthan gum, and deionized water; S2: Preparation of nanoemulsion; S3: Solvent preparation and mixing; S4: Construct a natural and stable system to obtain the initial product; S5: Filtration and sterilization treatment; S6: Aseptic filling of the finished disinfectant solution; The essential oil of Melaleuca alternifolia is of type 1,8, and the content of 1,8-cineole in the essential oil is ≥60%.

2. The preparation process of a pure plant essential oil disinfectant according to claim 1, characterized in that, The food-grade propylene glycol is obtained from plant fermentation and has a purity of ≥99.5%. The citric acid is obtained from extraction from natural citrus fruits; The xanthan gum is obtained from microbial fermentation; The conductivity of the deionized water is ≤5μS / cm.

3. The preparation process of a pure plant essential oil disinfectant according to claim 1, characterized in that, The preparation method of the nanoemulsion is as follows: A1: Premix: Mix Melaleuca alternifolia essential oil with soap bark extract preheated to 60°C and stir magnetically for 10 minutes to form a pre-emulsion; A2: High-pressure homogenization: A microfluidic nano-homogenizer was used at a pressure of 15000psi for 3 cycles to obtain a nanoemulsion with a particle size of <100nm.

4. The preparation process of a pure plant essential oil disinfectant according to claim 3, characterized in that, The amount of Melaleuca alternifolia essential oil added is 0.5-0.8 mL; The soap bark extract is a 5% aqueous solution, and the amount of soap bark extract added is 0.4 mL; The preemulsion has an HLB value in the range of 12-14.

5. The preparation process of a pure plant essential oil disinfectant according to claim 1, characterized in that, The solvent is prepared by first adding deionized water to the preparation tank, then slowly adding food-grade propylene glycol, and finally stirring at 20-30°C until completely dissolved. The method for preparing the solvent also includes filtering the solution through a 0.22 μm microporous membrane.

6. The preparation process of a pure plant essential oil disinfectant according to claim 1, characterized in that, The construction method of the naturally stable system is as follows: B1: Add 1% trehalose and 0.1% xanthan gum, stir at low speed at 45℃ for 2 hours to form a three-dimensional network structure; B2: Adjust the pH to 4.0-5.0 with citric acid.

7. The preparation process of a pure plant essential oil disinfectant according to claim 6, characterized in that, The amount of citric acid added is 0.2g.

8. The preparation process of a pure plant essential oil disinfectant according to claim 1, characterized in that, The filtration and sterilization process uses a 0.22μm ceramic membrane.

9. The preparation process of a pure plant essential oil disinfectant according to claim 8, characterized in that, The sample is irradiated with ultraviolet light for 15 minutes before filling; the ultraviolet light wavelength is 54nm.

10. The preparation process of a pure plant essential oil disinfectant according to claim 5, characterized in that, In step S3, 0.5% natural vitamin E is added to the solution.

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