Natural, healthy and non-irritant antibacterial floral water and production method thereof

By constructing a natural antibacterial system with Magnolia officinalis bark extract as the core, and combining a stepwise preparation process of polysaccharide colloidal network and chelated antioxidant liquid, the problems of unstable antibacterial properties, ingredient safety and poor user experience of existing antibacterial floral waters have been solved, achieving multiple effects of high-efficiency antibacterial, moisturizing and soothing.

CN121818458APending Publication Date: 2026-04-10GUANGXI UNIV +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-12
Publication Date
2026-04-10

AI Technical Summary

Technical Problem

Existing antibacterial floral waters have unstable antibacterial effects, questionable ingredient safety, and poor user experience. In particular, the addition of chemical ingredients may irritate the skin, and their single function cannot meet diverse skincare needs.

Method used

Using natural ingredients such as magnolia bark extract, menthol, jasmine fragrance, and thymol, combined with dealdehyde ethanol, stabilizers, and moisturizers, a precise process is used to construct an antibacterial, stable, and moisturizing floral water system. This process includes the stepwise preparation of polysaccharide colloidal networks, chelated-antioxidant solutions, and the mixing of biphasic systems to ensure synergistic effects of the ingredients.

Benefits of technology

It achieves multiple effects of highly effective antibacterial, moisturizing and soothing, and the product stability and safety are significantly improved, meeting the needs of natural, safe and multifunctional personal care, and overcoming the technical defects of traditional floral water.

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Abstract

The invention provides natural, healthy and non-irritant antibacterial floral water and a production method thereof, and belongs to the technical field of daily products. The antibacterial floral water is prepared from the following raw materials in percentage by weight: 0.21 to 0.63 percent of cortex magnoliae officinalis extract, 0.07 to 0.19 percent of menthol, 0.91 to 1.23 percent of jasmine essence, 0.88 to 1.14 percent of musk fragrant phenol, 68.45 to 72.09 percent of a solvent 1, 17.47 to 21.64 percent of a solvent 2, 0.08 to 0.13 percent of a stabilizer and 4.13 to 7.24 percent of a humectant. The preparation method comprises the following steps: respectively preparing the raw materials into a system 1 and a system 2, uniformly mixing, standing, and carrying out sterile filling. The natural cortex magnoliae officinalis extract is taken as a core, so that the composition is efficient, antibacterial, mild and non-irritant, the formula is scientific, and the preparation process is easy to industrialize.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily products, in particular to a natural, healthy and non-irritating antibacterial toilet water and a production method thereof. BACKGROUND

[0002] Magnolia officinalis bark extract contains various active ingredients, among which magnolol and honokiol are the most important antibacterial active substances, having broad-spectrum antibacterial, anti-inflammatory and other biological activities. Toilet water is a daily necessity in people's daily life, having the functions of cooling, relieving itching, disinfection, etc. With the improvement of people's living standards and the enhancement of health consciousness, the demand for toilet water is not only limited to the traditional functions of cooling and relieving itching, but also puts forward higher requirements on antibacterial, natural, safe, etc.

[0003] There are many problems in the antibacterial toilet water on the market. On the one hand, the antibacterial effect is uneven, lacking unified standards and strict testing, and some products even have false propaganda, misleading consumers. For example, some products claim to have strong antibacterial effect, but in actual use, they cannot achieve the expected effect. On the other hand, the safety of the ingredients is questionable. In order to pursue strong antibacterial effect, some products add chemical ingredients harmful to the human body, such as benzophenone-4, which may cause skin irritation or other potential health risks if used for a long time. At the same time, in terms of use experience, some antibacterial toilet water has the problems of pungent smell, greasy texture and easy to cause allergy, affecting the willingness of consumers to use. The current market is still dominated by products with chemical synthetic antibacterial agents, but the application research of natural plant source antibacterial ingredients has become the focus of industry innovation.

[0004] Chinese patent document "Magnolia officinalis toilet water and its preparation method" (publication number: CN108186428A) has a wide range of component ratio intervals, and does not specify the optimized value and the synergistic ratio with other components, which makes it difficult to ensure the stability of product efficacy. The technology does not disclose specific antibacterial detection data, which cannot confirm the inhibition effect on common pathogenic bacteria, and lacks safety verification such as skin irritation test and pH value detection, making it difficult to support the claim of "natural and non-irritating". The preparation process mentions "mixing and stirring", but does not specify the key parameters such as de-aldehyde ethanol concentration and mixing temperature, resulting in large batch quality differences in industrial production, and the magnolia officinalis extract is not purified, impurities can affect the color, odor and activity of the product, increasing the risk of irritation. In addition, the formula does not consider the synergy of components, does not add moisturizing agent and stabilizer, and the use experience is not good, the function is single and limited to mosquito repellent, which cannot meet the diversified skin care needs, and there are defects in aspects such as activity of raw materials, efficacy verification and controllability of process. SUMMARY

[0005] This invention provides a natural, healthy, and non-irritating antibacterial floral water and its production method, in order to solve the problems of poor antibacterial properties, irritation, and unpleasant experience of existing antibacterial floral waters in natural skincare.

[0006] To solve the above technical problems, the present invention adopts the following technical solution:

[0007] A natural, healthy, and non-irritating antibacterial floral water, comprising the following ingredients by weight percentage: 0.21-0.63% Magnolia officinalis bark extract, 0.07-0.19% menthol, 0.91-1.23% jasmine fragrance, 0.88-1.14% thymol, 68.45-72.09% solvent 1, 17.47-21.64% solvent 2, 0.08-0.13% stabilizer, and 4.13-7.24% moisturizer.

[0008] Furthermore, the ingredients include the following ingredients by weight percentage: 0.44% Magnolia officinalis bark extract, 0.15% menthol, 1.19% jasmine fragrance, 1.12% thymol, 70.50% solvent 1, 21.06% solvent 2, 0.11% stabilizer, and 5% humectant.

[0009] Furthermore, solvent 1 is dealdehyde ethanol.

[0010] Furthermore, the solvent 2 is deionized water.

[0011] Furthermore, the stabilizer comprises 0.015% chrysanthemum extract, 0.031% konjac glucomannan, 0.011% sodium gluconate, 0.008% trehalose, 0.006% vitamin E succinate, 0.010% potassium citrate, 0.005% zinc hyaluronic acid, and 0.024% dipotassium glycyrrhizate.

[0012] Furthermore, the stabilizer preparation steps are as follows:

[0013] (1) Add 70-90 mL of deionized water to the glass reactor, turn on the stirrer, heat to 42-48℃, add konjac glucomannan and zinc hyaluronic acid, stir while adding for 25-30 min, keep warm and let stand, control the viscosity of the system to 180-220 mPa·s, and ensure that the polysaccharide is fully swollen to form a preliminary colloidal system.

[0014] (2) Take 20-40 mL of deionized water and pour it into another reaction vessel. Add sodium gluconate, potassium citrate and vitamin E succinate. Turn on the stirring and heat to 50-55℃. Stir for 15-20 min. Adjust the pH of the system to 5.5-6.5 with citric acid solution. Control the transmittance of the system to ≥95% until the raw materials are completely dissolved to form a homogeneous solution.

[0015] (3) Pump the solution prepared in step 2 into the polysaccharide colloidal system in step 1, and add chrysanthemum extract and trehalose at the same time. Turn on high speed stirring, control the temperature at 45-50℃, and continue stirring for 40-45 minutes. During this period, take a sample every 5-15 minutes to test the transparency of the system. The transmittance is required to be ≥96%. If the transmittance is lower than 96%, add 0.00022-0.00044wt% of zinc hyaluronic acid according to the total mass of the floral water.

[0016] (4) Reduce the system temperature to 30-35℃, reduce the stirring speed to 70-90r / min, add dipotassium glycyrrhizate, stir for 15-18min until completely dissolved, add the remaining 10mL of deionized water, stir for 8-10min to adjust the system viscosity to 250-280mPa·s, turn off the stirring, keep it at 30-35℃ for 7-9h, take a sample during the period to observe whether the system separates into layers; finally, filter it under 0.1-0.15MPa pressure using a polyethersulfone microporous filter membrane to remove trace amounts of undissolved impurities and obtain the stabilizer product.

[0017] Furthermore, the moisturizer is composed of 1.8% Tremella fuciformis polysaccharide, 1.3% panthenol, and 1.9% sorbitol.

[0018] A method for producing a natural, healthy, and non-irritating antibacterial floral water, characterized by comprising the following steps:

[0019] (1) The extract of Magnolia officinalis bark, menthol, jasmine essence and thymol were dissolved in solvent 1 to prepare system 1;

[0020] (2) Rosemary extract, sodium hyaluronate, sodium citrate, tremella polysaccharide, panthenol, and sorbitol were dissolved in solvent 2 to prepare system 2;

[0021] (3) Add system 2 to system 1 and mix evenly. After standing, fill aseptically.

[0022] Furthermore, the number of days for resting in step (3) is 3-5 days.

[0023] Furthermore, the ambient temperature during the settling process in step (3) is 20-25℃.

[0024] The mechanisms of action of each preparation step are as follows:

[0025] I. Mechanism of Action of Stabilizer Preparation Steps

[0026] (I) Polysaccharide swelling and construction of colloidal systems

[0027] Deionized water was added to a glass reactor and the mixture was stirred and heated. Konjac glucomannan and zinc hyaluronic acid were then added, and the mixture was stirred continuously while maintaining the temperature and allowing it to stand. The core mechanism lies in constructing a stable three-dimensional colloidal network. Deionized water acts as a solvent carrier, preventing impurity ions from interfering with the polysaccharide molecular conformation; the heating conditions promote the unfolding of the linear polysaccharide chains of konjac glucomannan, reducing intermolecular entanglement and aggregation, and, combined with stirring, achieving uniform dispersion; the Zn in zinc hyaluronic acid... 2+ Coordination bonds are formed with the hydroxyl groups of konjac glucomannan, driving the two to interpenetrate and form a preliminary three-dimensional network structure. By controlling the viscosity of the system, the polysaccharide is ensured to swell sufficiently, laying the spatial foundation for subsequent encapsulation of active ingredients and inhibition of aggregation. The coordinated selection of temperature and stirring parameters in this step can avoid network structure defects caused by insufficient swelling of polysaccharide, ensuring the efficient performance of subsequent stable functions.

[0028] (II) Preparation of chelation-antioxidant solution

[0029] Deionized water was added to the reaction vessel to dissolve sodium gluconate, potassium citrate, and vitamin E succinate, and to adjust the pH and transmittance. The mechanism involved synergistic effects of multiple functions. 3+ Cu 2+ Metal ions are eliminated to prevent their catalytic effect on the subsequent oxidation of active ingredients; sodium gluconate enhances compatibility with dealdehyde ethanol by adjusting the osmotic pressure of the aqueous phase, creating conditions for the fusion of the two-phase system; vitamin E succinate, as a lipid-soluble antioxidant, is uniformly dispersed at the aqueous-lipid interface under stirring and heating to form an antioxidant pretreatment layer. Adjusting the pH to a suitable range using citric acid solution maintains the activity of the chelating agent while avoiding damage to the component structure from extreme pH; controlling the transmittance ensures complete dissolution of the raw materials and avoids undissolved particles affecting the homogeneity of the subsequent system. The parameter selection in this step achieves synergistic pretreatment of chelation, osmotic pressure adjustment, and antioxidant effects.

[0030] (III) Composite reaction and active fusion

[0031] The chelated-antioxidant solution is pumped into a polysaccharide colloidal system, along with chrysanthemum extract and trehalose, while controlling temperature and stirring parameters. The core objective is to achieve molecular-level synergy and functional enhancement. The pumping method avoids liquid impact damaging the polysaccharide network. Luteolin in the chrysanthemum extract and vitamin E succinate form an "aqueous-interface" antioxidant network. Luteolin quenches free radicals in the aqueous phase, and vitamin E succinate blocks the oxidation of lipid phase components, providing dual protection against active ingredient degradation. Trehalose stabilizes the polysaccharide network conformation through hydrogen bonds, preventing network collapse caused by temperature fluctuations. High-speed stirring promotes full collisions of molecules, ensuring uniform dispersion of antioxidants and chelating agents within the colloidal network. Controlling the temperature at 45-50℃ ensures efficient molecular motion for full integration while preventing active ingredient deactivation due to high temperatures. This step, with its synergistic parameter control, achieves an organic integration of antioxidant and steric stabilization functions.

[0032] (iv) System harmonization and post-processing

[0033] Cooling and reducing the stirring rate, followed by dissolution with dipotassium glycyrrhizate, volume adjustment, and filtration, aims to perfect functionality and ensure stability. Cooling and reducing the stirring rate minimize system turbulence, preventing network structure damage; the anti-inflammatory components of dipotassium glycyrrhizate neutralize potential irritation from ethanol, and its hydroxyl groups form weak coordination bonds with zinc hyaluronic acid, further enhancing system stability; adding remaining deionized water to adjust volume and viscosity ensures precise stabilizer concentration, suitable for the needs of the floral water system; maintaining temperature and allowing it to stand promotes molecular self-assembly to form supramolecular structures, reducing component migration during storage; polyethersulfone microporous membrane filtration removes trace impurities, ensuring product purity. The synergistic effect of these parameters achieves a unified "stabilization-repair" function while ensuring compatibility between the stabilizer and the floral water system through precise control, avoiding sensory defects.

[0034] II. Mechanism of Action of the Preparation Steps for Antibacterial Floral Water

[0035] (I) Preparation of System 1

[0036] The core objective of dissolving magnolol bark extract, menthol, jasmine fragrance, and thymol in dealdehyded ethanol is to achieve the dissolution and pre-activation of lipid-soluble active ingredients. Dealdehyded ethanol disrupts the intermolecular forces between magnolol and honokiol in the magnolol bark extract through hydrogen bonding, achieving efficient dissolution while avoiding the irritating residue of ordinary ethanol. Menthol and thymol form a molecular complex through van der Waals forces, enhancing lipid-soluble penetration. Terpenoids in jasmine fragrance reduce the surface tension of the system, guiding the antibacterial components to target and migrate towards the bacterial cell membrane, laying the foundation for subsequent antibacterial effects. This step achieves the dissolution and functional pretreatment of active ingredients through solvent selection and inter-component interactions.

[0037] (II) Preparation of System 2

[0038] The mechanism of dissolving stabilizers and humectants in deionized water is to construct a water-soluble synergistic system. The polysaccharide network in the stabilizer encapsulates the humectant components, preventing incompatibility issues caused by direct contact with lipid-phase components. In the humectant, tremella polysaccharides form a physical water-locking film, panthenol promotes skin barrier repair, and sorbitol regulates osmotic pressure. These three components synergistically construct a moisturizing system, while simultaneously forming a "repair-moisturize" synergy with dipotassium glycyrrhizate in the stabilizer, alleviating the dryness and irritation caused by ethanol. Deionized water, acting as a carrier, ensures uniform dispersion of the components, creating conditions for subsequent integration with System 1. This step achieves the synergistic integration of stabilizing and moisturizing functions.

[0039] (III) Mixing and settling and filling

[0040] The core of adding System 2 to System 1, mixing, and allowing it to stand before filling is to achieve biphase fusion and molecular reconstruction. The slow addition of System 2 avoids phase separation caused by interfacial impact. The hydrophilic groups of sodium hyaluronate form hydrogen bonds with ethanol molecules, maintaining biphase continuity; sodium citrate dissociates ions to neutralize the acidic groups of magnolol, enhancing its dispersion uniformity; during standing, molecules achieve full synergy through Brownian motion, and the hydrophobic groups of menthol insert into bacterial cell membranes, opening penetration channels for antibacterial components. Tremella fuciformis polysaccharide and panthenol form "moisturizing-antibacterial" composite microspheres, prolonging the action time of active ingredients. Controlling the number of days and temperature of standing ensures sufficient molecular rearrangement to form a stable supramolecular structure while avoiding component deterioration caused by prolonged standing. Finally, aseptic filling ensures product hygiene and safety. The parameter selection in this step achieves a balance of antibacterial, stabilizing, and moisturizing functions, as well as product quality assurance.

[0041] Compared with the prior art, the present invention has the following advantages and technical effects:

[0042] I. Innovation and Synergistic Effect of Raw Material System

[0043] This invention overcomes the technical limitations of traditional floral waters that rely on chemically synthesized antibacterial agents, constructing a natural antibacterial system with magnolia bark extract as its core. Magnolol and honokiol exert broad-spectrum antibacterial effects by disrupting the integrity of bacterial cell membranes, forming a synergistic antibacterial effect with thymol—thymol's lipid solubility enhances the accumulation efficiency of magnolol in cell membranes. The combined effect of these two significantly improves antibacterial activity, solving the technical problem of insufficient antibacterial efficacy of single natural ingredients.

[0044] The innovative design of the stabilizer system embodies a technological breakthrough in multi-component synergy. Konjac glucomannan and zinc hyaluronic acid form a three-dimensional colloidal network through intermolecular coordination, providing a sustained-release carrier for the active ingredients and hindering their aggregation through steric hindrance. Flavonoids from chrysanthemum extract and vitamin E succinate construct a dual antioxidant network at the aqueous phase-interface, blocking free radical chain reactions from different phase regions. Citrate ions dissociated from potassium citrate eliminate oxidation catalysts by chelating metal ions, forming a functional complement to the aforementioned antioxidant components. This multi-mechanism synergistic stabilization system effectively solves the industry pain points of easy oxidation and difficult storage of natural active ingredients.

[0045] The moisturizing system uses a compound formula of tremella polysaccharide, panthenol and sorbitol. The three components work synergistically through different mechanisms of action: tremella polysaccharide forms a physical water-locking film, panthenol promotes skin barrier repair, and sorbitol regulates the osmotic pressure of the stratum corneum. Together, they alleviate the skin dryness that may be caused by de-formaldehyde ethanol, achieving a functional balance of "antibacterial-moisturizing". This overcomes the technical deficiency of traditional floral water that only focuses on antibacterial properties while neglecting skin care.

[0046] II. Scientific nature and technical effectiveness of process design

[0047] The stepwise preparation process of this invention embodies the technological innovation of precise control. In the preparation of the stabilizer, the stepwise construction of the polysaccharide colloidal system and the chelating-antioxidant solution avoids the risk of precipitation caused by direct interaction between components; the selection of high-speed stirring process parameters at 45-50℃ ensures sufficient molecular collision and fusion while avoiding the destruction of active ingredients by high temperature, thus achieving a balance between thermodynamic stability and component activity.

[0048] The two-phase mixing process solves the technical challenge of oil-water immiscibility. By controlling the slow addition rate of system 2 to system 1, combined with the amphiphilic regulating effect of zinc hyaluronic acid, a stable colloidal dispersion system is formed between the water-soluble and fat-soluble components, significantly improving the product's uniformity and stability. The 20-25℃ settling process provides suitable conditions for molecular rearrangement, promoting supramolecular structure formation and effectively preventing stratification during storage.

[0049] The use of dealdehyde ethanol reflects an innovative safety design. Compared to traditional ethanol, dealdehyde ethanol removes irritating aldehyde impurities. Combined with the anti-inflammatory and soothing effects of dipotassium glycyrrhizate, it significantly reduces the product's irritation to the skin. At the same time, it retains the penetration-enhancing function of ethanol as a solvent, achieving a balance of "highly effective antibacterial and low irritation," thus solving the problem of strong irritation in traditional alcohol-containing floral waters.

[0050] III. Practical Value and Technological Progress

[0051] The technical solution of this invention has outstanding practicality. The prepared floral water simultaneously possesses multiple effects such as antibacterial, moisturizing, and soothing, meeting consumers' demand for natural, safe, and multifunctional personal care products. All raw materials are selected from food-grade or cosmetic-grade natural ingredients, exhibiting excellent biocompatibility and aligning with the development trend of green chemistry.

[0052] In terms of technical effectiveness, this invention effectively solves the problems of poor stability, single efficacy, and strong irritation of natural antibacterial ingredients in existing technologies through innovative raw material compatibility and process optimization, forming a technical solution with independent innovation characteristics. Its multi-component synergistic mechanism and precise process control method provide new ideas for the research and development of natural antibacterial cosmetics, and have value for technological advancement and industrial application. Attached Figure Description

[0053] Figure 1 This is a sample diagram of the present invention. Detailed Implementation

[0054] I. Implementation Examples

[0055] Example 1

[0056] 1. Raw material ratio (wt%): 0.44% Magnolia officinalis bark extract (containing magnolol and honokiol active ingredients), 0.15% menthol, 1.19% jasmine fragrance, 1.12% thymol, 70.50% dealdehyde ethanol, 21.06% deionized water, 0.11% stabilizer (containing 0.015% chrysanthemum extract, 0.031% konjac glucomannan, 0.011% sodium gluconate, 0.008% trehalose, 0.006% vitamin E succinate, 0.010% potassium citrate, 0.005% zinc hyaluronic acid, 0.024% dipotassium glycyrrhizate), 5% moisturizer (containing 1.8% tremella polysaccharide, 1.3% panthenol, 1.9% sorbitol).

[0057] 2. Stabilizer preparation steps

[0058] (1) Add 80 mL of deionized water to a 500 mL glass reactor equipped with a magnetic stirrer and a precision thermometer, turn on the stirrer (100 r / min), heat to 45 °C, add 0.031% konjac glucomannan and 0.005% zinc hyaluronic acid, add and stir for 28 min, keep warm and stand for 10 min, and use a 25 °C rotational viscometer to measure the viscosity of the system to be 200 mPa·s, to ensure that the polysaccharide is fully swollen to form a preliminary colloidal system;

[0059] (2) Pour 30 mL of deionized water into a 200 mL reaction vessel, add 0.011% sodium gluconate, 0.010% potassium citrate, and 0.006% vitamin E succinate, turn on the stirrer (180 r / min), heat to 52 °C, stir for 18 min, adjust the pH of the system to 6.0 with 0.1 mol / L citric acid solution, and measure the transmittance of the system at 450 nm wavelength, which is 96%, until the raw materials are completely dissolved to form a homogeneous solution;

[0060] (3) The solution prepared in step (2) is pumped into the polysaccharide colloidal system in step (1) at a rate of 10 mL / min. At the same time, 0.015% chrysanthemum extract and 0.008% trehalose are added. High-speed stirring is started (400 r / min), the temperature is controlled at 48℃, and stirring is continued for 42 min. During this period, samples are taken every 10 min to detect the transparency of the system. The transmittance is measured at a wavelength of 450 nm and is ≥96%. No zinc hyaluronic acid needs to be added.

[0061] (4) Reduce the system temperature to 32℃, reduce the stirring rate to 80r / min, add 0.024% dipotassium glycyrrhizate, and stir for 16min until completely dissolved; add the remaining 10mL of deionized water, and stir for 9min to adjust the system viscosity to 260mPa·s (measured at 25℃); after turning off the stirring, keep it at 32℃ for 8h, and take samples every 2h during the period. The system did not separate into layers; finally, filter it under 0.12MPa pressure using a 0.22μm polyethersulfone microporous membrane to remove trace amounts of undissolved impurities and obtain the stabilizer product.

[0062] 3. Preparation process of antibacterial floral water

[0063] (1) Preparation of System 1: Dissolve 0.44% Magnolia officinalis bark extract, 0.15% menthol, 1.19% jasmine fragrance and 1.12% thymol in 70.50% dealdehyde ethanol and stir at 25°C for 150 r / min until completely dissolved;

[0064] (2) Preparation of System 2: Dissolve the 0.11% stabilizer and 5% humectant (1.8% Tremella polysaccharide, 1.3% panthenol, 1.9% sorbitol) prepared above in 21.06% deionized water and stir at 25°C for 100 r / min until completely dissolved;

[0065] (3) Mixing and filling: Add system 2 to system 1 at a rate of 5 mL / min, mix and stir at 25℃ for 30 min; let stand at 25℃ for 5 days, filter through a 0.45 μm filter membrane and then aseptically fill to obtain the antibacterial toilet water product.

[0066] Example 2

[0067] 1. Raw material ratio (wt%): 0.41% Magnolia officinalis bark extract, 0.12% menthol, 1.06% jasmine fragrance, 1.14% thymol, 71.05% dealdehyde ethanol, 20.84% ​​deionized water, 0.11% stabilizer (same as the raw material composition in Example 1), 5% humectant (same as the raw material composition in Example 1).

[0068] 2. Stabilizer preparation steps

[0069] (1) Add 75 mL of deionized water to a 500 mL glass reactor, turn on the stirrer (95 r / min), heat to 43 °C, add 0.031% konjac glucomannan and 0.005% zinc hyaluronic acid, stir for 26 min, keep warm and stand for 10 min, the viscosity of the system (25 °C) is 190 mPa·s;

[0070] (2) Take 25 mL of deionized water and pour it into a 200 mL reaction vessel. Add 0.011% sodium gluconate, 0.010% potassium citrate, and 0.006% vitamin E succinate. Stir at 170 r / min and heat at 51 °C for 16 min. Adjust the pH to 5.8 with 0.1 mol / L citric acid. The transmittance (450 nm) is 95.5%, forming a homogeneous solution.

[0071] (3) Pump the solution from step (2) into the system from step (1) at a rate of 9 mL / min, add 0.015% chrysanthemum extract and 0.008% trehalose, stir at 45°C and 380 r / min for 40 min, and measure the transparency every 8 min. The transmittance is ≥96%.

[0072] (4) Cool down to 31℃, add 0.024% dipotassium glycyrrhizate while stirring at 80r / min, and dissolve completely in 15min; add 10mL deionized water and stir for 8min to adjust the viscosity to 250mPa·s; keep warm at 31℃ for 7.5h, and no stratification occurs; filter through a 0.22μm filter membrane under 0.11MPa pressure to obtain the stabilizer product.

[0073] 3. Preparation process of antibacterial floral water

[0074] (1) System 1: Dissolve 0.41% Magnolia officinalis bark extract (containing magnolol and honokiol), 0.12% menthol, 1.06% jasmine fragrance and 1.14% thymol in 71.05% dealdehyde ethanol and stir at 22°C at 140 r / min until dissolved;

[0075] (2) System 2: Dissolve 0.11% stabilizer and 5% humectant in 20.84% ​​deionized water and stir at 22°C for 90 r / min until dissolved;

[0076] (3) Add system 2 to system 1, mix and stir at 22℃ for 30 min; let stand at 22℃ for 4 days, filter and aseptically fill.

[0077] Example 3

[0078] 1. Raw material ratio (wt%): 0.21% Magnolia officinalis bark extract, 0.07% menthol, 0.91% jasmine fragrance, 1.14% thymol, 70.44% dealdehyde ethanol, 21.64% deionized water, 0.11% stabilizer (same as the raw material composition in Example 1), 5% humectant (same as the raw material composition in Example 1).

[0079] 2. Stabilizer preparation steps

[0080] (1) Add 70 mL of deionized water to a glass reactor, stir at 90 r / min, heat at 42 °C, add 0.031% konjac glucomannan and 0.005% zinc hyaluronic acid, stir for 25 min, keep warm and stand for 10 min, viscosity 180 mPa·s (25 °C).

[0081] (2) Add 20 mL of deionized water to the reaction vessel, add 0.011% sodium gluconate, 0.010% potassium citrate, and 0.006% vitamin E succinate, stir at 150 r / min, heat at 50℃ for 15 min, pH 5.5, transmittance 96%, to obtain a homogeneous solution;

[0082] (3) The solution was pumped into the polysaccharide system at 8 mL / min, and 0.015% chrysanthemum extract and 0.008% trehalose were added. The mixture was stirred at 45℃ and 350 r / min for 40 min. The transparency was measured every 5 min. The transmittance was ≥96%.

[0083] (4) Cool down to 30℃, stir at 70r / min and add 0.024% dipotassium glycyrrhizate, dissolve in 15min; add 10mL deionized water, adjust viscosity to 250mPa·s in 8min; keep warm at 30℃ for 7h, no stratification; filter with 0.22μm filter membrane under 0.1MPa pressure to obtain the stabilizer product.

[0084] 3. Preparation process of antibacterial floral water

[0085] Same as Example 1, only the raw material ratio was adjusted. The stirring temperature of System 1 was 25°C and the stirring speed was 150 r / min, and the stirring temperature of System 2 was 25°C and the stirring speed was 100 r / min. After mixing, the mixture was left to stand at 25°C for 5 days.

[0086] Example 4

[0087] 1. Raw material ratio (wt%): 0.40% Magnolia officinalis bark extract, 0.13% menthol, 1.12% jasmine fragrance, 1.23% thymol, 69.88% dealdehyde ethanol, 21.64% deionized water, 0.11% stabilizer (same as the raw material composition in Example 1), 5% humectant (same as the raw material composition in Example 1).

[0088] 2. Stabilizer preparation steps

[0089] (1) Add 70 mL of deionized water to a glass reactor, stir at 90 r / min, heat at 42 °C, add 0.031% konjac glucomannan and 0.005% zinc hyaluronic acid, stir for 25 min, keep warm and stand for 10 min, viscosity 180 mPa·s (25 °C).

[0090] (2) Add 20 mL of deionized water to the reaction vessel, add 0.011% sodium gluconate, 0.010% potassium citrate, and 0.006% vitamin E succinate, stir at 150 r / min, heat at 50℃ for 15 min, pH 5.5, transmittance 96%, to obtain a homogeneous solution;

[0091] (3) The solution was pumped into the polysaccharide system at 8 mL / min, and 0.015% chrysanthemum extract and 0.008% trehalose were added. The mixture was stirred at 45℃ and 350 r / min for 40 min. The transparency was measured every 5 min. The transmittance was ≥96%.

[0092] (4) Cool down to 30℃, stir at 70r / min and add 0.024% dipotassium glycyrrhizate, dissolve in 15min; add 10mL deionized water, adjust viscosity to 250mPa·s in 8min; keep warm at 30℃ for 7h, no stratification; filter with 0.22μm filter membrane under 0.1MPa pressure to obtain the stabilizer product.

[0093] 3. Preparation process of antibacterial floral water

[0094] Same as Example 1, only the raw material ratio was adjusted. The stirring temperature of System 1 was 25°C and the stirring speed was 150 r / min, and the stirring temperature of System 2 was 25°C and the stirring speed was 100 r / min. After mixing, the mixture was left to stand at 25°C for 5 days.

[0095] Example 5

[0096] 1. Raw material ratio (wt%): 0.38% Magnolia officinalis bark extract, 0.14% menthol, 0.99% jasmine fragrance, 1.14% thymol, 72.09% dealdehyde ethanol, 21.64% deionized water, 0.11% stabilizer (same as the raw material composition in Example 1), 5% humectant (same as the raw material composition in Example 1).

[0097] 2. Stabilizer preparation steps

[0098] (1) Add 85 mL of deionized water to a glass reactor, stir at 110 r / min, heat at 46 °C, add 0.031% konjac glucomannan and 0.005% zinc hyaluronic acid, stir for 29 min, keep warm and stand for 10 min, viscosity 210 mPa·s (25 °C).

[0099] (2) Add 35 mL of deionized water to the reaction vessel, add 0.011% sodium gluconate, 0.010% potassium citrate, and 0.006% vitamin E succinate, stir at 190 r / min, heat at 54℃ for 19 min, pH 6.2, transmittance 95.8%, and obtain a homogeneous solution;

[0100] (3) The solution was pumped into the polysaccharide system at 11 mL / min, and 0.015% chrysanthemum extract and 0.008% trehalose were added. The mixture was stirred at 49℃ and 420 r / min for 44 min. The transparency was measured every 12 min. The transmittance was ≥96%.

[0101] (4) Cool down to 34℃, stir at 85r / min and add 0.024% dipotassium glycyrrhizate, dissolve in 17min; add 10mL deionized water, adjust viscosity to 270mPa·s in 10min; keep warm at 34℃ for 8.5h, no stratification; filter with 0.22μm filter membrane under 0.14MPa pressure to obtain the stabilizer product.

[0102] 3. Preparation process of antibacterial floral water

[0103] Same as in Example 1, the stirring temperature of system 1 was 25°C and the stirring speed was 150 r / min, and the stirring temperature of system 2 was 25°C and the stirring speed was 100 r / min. After mixing, the mixture was allowed to stand at 25°C for 5 days, filtered, and then aseptically filled.

[0104] II. Comparative Example

[0105] Comparative Example 1

[0106] Preparation process: Take 800g of dried bark of Magnolia officinalis (crushed to 40 mesh), add 12L of distilled water, soak at 25℃ for 30 minutes, distill at normal pressure for 2 hours (distillation temperature 95-100℃), collect 8L of distillate, collect volatile oil and water-soluble components, add 1% borneol (g / ml) and 0.2% benzoic acid (g / ml) to the distillate, make up to 10L with deionized water, stir at 40℃ until completely dissolved, cool to room temperature and then directly fill into bottles.

[0107] Comparative Example 2

[0108] Raw material ratio (wt%): 0.3% triclosan (chemical antibacterial agent), 0.1% benzophenone-4, 0.2% triethanolamine, 70% ethanol, water balance.

[0109] Preparation process: Mixing at room temperature, without settling.

[0110] Comparative Example 3

[0111] Raw material ratio (wt%): 0.44% Magnolia officinalis bark extract, 0% menthol (removed cooling component), 1.19% jasmine fragrance, 1.12% thymol, 70.50% dealdehyde ethanol, 21.21% deionized water, 0.11% stabilizer (same as raw material composition in Example 1), 5% humectant (same as raw material composition in Example 1).

[0112] Preparation process: Same as in Example 1.

[0113] III. Application Examples

[0114] Application Example 1: Antibacterial Scenario in Student Dormitories

[0115] Test subjects: Products of Example 1, Comparative Example 1, and Comparative Example 2, and the dormitory environment of 20 college students.

[0116] Test method: Spray on beds and tabletops daily for 7 consecutive days, and test the total number of bacterial colonies on the surface (CFU / cm³). 2 (and user feedback on skin irritation).

[0117] Application Example 2: Sensitive Skin Care Scenarios

[0118] Test subjects: Products from Example 2, Comparative Example 2, and Comparative Example 3, and 30 volunteers with sensitive skin.

[0119] Test method: Apply to the inner forearm daily for 14 consecutive days. The irritation index (0-5 points) and moisturizing rate (change in stratum corneum moisture content) are evaluated by patch test.

[0120] Application Example 3: Outdoor Protection Scenarios

[0121] Test subjects: Products of Example 3, Comparative Example 1, and Comparative Example 2, and 15 outdoor workers.

[0122] Test method: Spray on exposed skin before outdoor activities, and record the duration of cooling sensation (subjective rating 1-5 points) and antibacterial duration (detection of bacterial colony count on skin surface) every 2 hours.

[0123] IV. Test Data Results and Analysis

[0124] 1. Data Results

[0125] The detection data results of Examples 1-5 and Comparative Examples 1-3 of the present invention are shown in Table 1.

[0126]

[0127] 2. Data Comparison and Analysis

[0128] Antibacterial performance: The antibacterial rate of Examples 1-5 was ≥96.2%, with Example 1 reaching 99.8%, which was better than Comparative Example 2 (chemical antibacterial agent, 99.0%). Although Comparative Example 1 (existing technology) used Magnolia officinalis bark extract, the antibacterial rate was only 72.3%. The difference was due to: ① Existing technology uses simple distillation extraction, which results in some loss of active ingredients; ② Existing technology does not optimize the extract concentration.

[0129] Safety: The irritation index of the example is ≤0.3, which is non-irritating; the irritation index of Comparative Example 2 (chemical antibacterial agent) is 1.2, and the irritation index of Comparative Example 1 (prior art) is 1.5, which confirms the safety breakthrough of the natural formula of the present invention.

[0130] User experience: The cooling effect of the first example lasted for 3.5-5.0 hours, the moisturizing rate was 12-18%, and the odor satisfaction was ≥4.5; the cooling effect of the second example (without menthol) disappeared, verifying the synergistic necessity of menthol and glycerin; the moisturizing rate of the second examples (1 and 2) was <10%, and the odor satisfaction was <3.0, exposing the defects of the existing technology.

[0131] V. Antibacterial ability test

[0132] 1. Data Results: The Magnolia officinalis extract of Example 1 showed strong antibacterial activity at low concentrations, with high inhibition rates against commonly encountered bacteria (such as Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, and Candida albicans) and Aspergillus brasiliensis. The results are shown in Tables 2 and 3.

[0133]

[0134]

[0135] Based on the results of the minimum inhibitory concentration (MIC) tests of Magnolia officinalis bark extract against different bacterial species in Tables 2 and 3, the following conclusions can be drawn:

[0136] (1) It has a broad-spectrum and highly effective antibacterial effect against common bacteria and fungi.

[0137] Against Gram-negative bacteria (Escherichia coli, Pseudomonas aeruginosa): Magnolia officinalis extract at a concentration of 2% completely inhibited their growth, showing strong antibacterial activity. The antibacterial effect decreased at concentrations below 1%, indicating that the MIC for these two types of bacteria was between 1% and 2%.

[0138] Against Gram-positive bacteria (Staphylococcus aureus): the antibacterial activity is particularly outstanding, with only a 0.002% concentration required to completely inhibit growth, and the MIC is extremely low. This indicates that Magnolia officinalis extract has a very strong selective antibacterial effect against Staphylococcus aureus.

[0139] For fungi (Candida albicans, Aspergillus brasiliensis): the MIC for Candida albicans is 0.00125%, and the MIC for Aspergillus brasiliensis is 0.0025%. This indicates that the extract also has a highly effective inhibitory effect on common fungi, and the active concentration is much lower than the MIC for most bacteria.

[0140] (2) The antibacterial activity is significantly concentration-dependent.

[0141] All tested bacterial strains exhibited a clear threshold from "no growth (-)" to "growth (+)", indicating that the antibacterial effect of Magnolia officinalis extract follows a typical concentration-response relationship. Below the MIC, bacteria / fungi can grow normally; at or above the MIC, growth is inhibited.

[0142] (3) Provide experimental evidence for the product claims of "natural, healthy and non-irritating".

[0143] Magnolia officinalis extract achieves highly effective antibacterial activity at extremely low concentrations, reducing the amount of active ingredients in the formulation and thus minimizing potential skin irritation. Experimental data supports the invention's design philosophy of achieving gentle, non-irritating products while maintaining highly effective antibacterial activity.

[0144] 2. Comparative analysis: The antibacterial effects of existing antibacterial floral waters on the market vary, and most rely on chemical antibacterial agents (such as triclosan). However, this invention achieves the same or even better antibacterial effect through natural Magnolia officinalis extract.

[0145] VI. Example 1: Safety, Stability, and Sensory Index Testing

[0146] The natural, healthy, non-irritating antibacterial floral water of Example 1 of this invention exhibits excellent performance in terms of safety, stability, and sensory indicators. Its color is a clear golden yellow, with clear water free of obvious impurities and black spots. The aroma possesses a unique layered quality, with a fresh jasmine top note, a herbal middle note, and a minty base note, providing a pleasant sensory experience. In terms of physicochemical properties, the relative density is 0.85815 g / ml, the turbidity test at 10℃ shows clear, non-turbid water, and it maintains its original color after being placed at (48±1)℃ for 24 hours. The pH is approximately 6, within the skin-friendly range of 5-7, demonstrating excellent stability. Regarding hygiene and safety, formaldehyde, lead, arsenic, mercury, and other indicators all passed the tests, with no harmful substance residues, ensuring safety. Through scientific formula design and rigorous preparation processes, the product of this invention achieves high standards in sensory, physicochemical, and hygiene and safety aspects, fully demonstrating its natural, healthy, and non-irritating characteristics and advantages.

[0147] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A natural, healthy, and non-irritating antibacterial floral water, characterized in that: The ingredients include the following ingredients by weight percentage: 0.21-0.63% Magnolia officinalis bark extract, 0.07-0.19% menthol, 0.91-1.23% jasmine fragrance, 0.88-1.14% thymol, 68.45-72.09% solvent 1, 17.47-21.64% solvent 2, 0.08-0.13% stabilizer, and 4.13-7.24% humectant.

2. The natural, healthy, and non-irritating antibacterial floral water according to claim 1, characterized in that, The ingredients include the following ingredients by weight percentage: 0.44% Magnolia officinalis bark extract, 0.15% menthol, 1.19% jasmine fragrance, 1.12% thymol, 70.50% solvent 1, 21.06% solvent, 0.11% stabilizer, and 5% humectant.

3. The natural, healthy, and non-irritating antibacterial floral water according to claim 1 or 2, characterized in that, Solvent 1 is dealdehyde ethanol.

4. The natural, healthy, and non-irritating antibacterial floral water according to claim 1 or 2, characterized in that, Solvent 2 is deionized water.

5. The natural, healthy, and non-irritating antibacterial floral water according to claim 2, characterized in that, The stabilizer comprises 0.015% chrysanthemum extract, 0.031% konjac glucomannan, 0.011% sodium gluconate, 0.008% trehalose, 0.006% vitamin E succinate, 0.010% potassium citrate, 0.005% zinc hyaluronic acid, and 0.024% dipotassium glycyrrhizate.

6. The natural, healthy, and non-irritating antibacterial floral water according to claim 5, characterized in that, The stabilizer preparation steps are as follows: (1) Add 70-90 mL of deionized water to the glass reactor, turn on the stirring and heat up, add konjac glucomannan and zinc hyaluronic acid, add and stir for 25-30 min, keep warm and let stand, control the viscosity of the system, and ensure that the polysaccharide fully swells to form a preliminary colloidal system. (2) Take 20-40 mL of deionized water and pour it into another reaction vessel. Add sodium gluconate, potassium citrate and vitamin E succinate. Turn on the stirring and heat. Stir for 15-20 min. Adjust the pH of the system with citric acid solution and control the transmittance of the system until the raw materials are completely dissolved to form a homogeneous solution. (3) Pump the solution prepared in step 2 into the polysaccharide colloidal system in step 1, and add chrysanthemum extract and trehalose at the same time. Turn on high speed stirring, control the temperature at 45-50℃, and continue stirring for 40-45 minutes. During this period, take samples to test the transparency of the system. (4) Cool the system down and reduce the stirring rate. Add dipotassium glycyrrhizate and stir until completely dissolved. Add the remaining 10 mL of deionized water and stir to adjust the viscosity of the system to 250-280 mPa·s. After turning off the stirring, keep the system at a constant temperature and observe whether the system separates into layers. Finally, filter the system under a pressure of 0.1-0.15 MPa using a polyethersulfone microporous membrane to remove trace amounts of undissolved impurities and obtain the stabilizer product.

7. The natural, healthy, and non-irritating antibacterial floral water according to claim 2, characterized in that, The moisturizer is composed of 1.8% Tremella fuciformis polysaccharide, 1.3% panthenol, and 1.9% sorbitol.

8. A method for producing a natural, healthy, and non-irritating antibacterial floral water according to any one of claims 1-7, characterized in that, Includes the following steps: (1) The extract of Magnolia officinalis bark, menthol, jasmine essence and thymol were dissolved in solvent 1 to prepare system 1; (2) Dissolve the stabilizer and humectant in solvent 2 to prepare system 2; (3) Add system 2 to system 1 and mix evenly. After standing, fill aseptically.

9. The method for producing the natural, healthy, and non-irritating antibacterial floral water according to claim 8, characterized in that, The number of days for resting in step (3) is 3-5 days.

10. The method for producing the natural, healthy, and non-irritating antibacterial floral water according to claim 8, characterized in that, The ambient temperature during the settling process in step (3) is 20-25℃.

Citation Information

Patent Citations

  • Magnolia officinalis floral water and preparation method thereof

    CN108186428A