Mild anti-corrosion composition as well as preparation method and application thereof

Abstract

The invention relates to the technical field of cosmetic anticorrosion, and particularly discloses a mild anticorrosion composition and a preparation method and application thereof.The composition is prepared from, by mass, 13.0%-16.7% of oil-soluble alcohol, 2.0%-5.0% of fatty acid salt, 1.0%-3.0% of plant extract, 1%-3% of polyol ester and the balance antibacterial grease; the fatty acid salt is zinc octoate and sodium lauroyl sarcosinate; the plant extract is a moutan bark extract and carnosic acid; the components take effect synergistically to achieve long-acting antibacterial and antiseptic effects, the components are mild and non-irritant, synergistic bacteriostasis is achieved through multiple mechanisms of pH adjustment, microbial cell membrane damage, metabolic enzyme activity inhibition and the like, the oil solubility is excellent, and the composition is suitable for pure oil agents, water-in-oil type cream and oil-in-water type cream. The problems that a traditional preservative is strong in irritation, poor in oil phase dispersion and difficult to pass the international standard test are solved, and the preservative has the characteristics of mildness, high efficiency and low addition amount.

Description

Technical Field

[0001] This invention relates to the field of cosmetic preservative technology, specifically to a mild preservative composition, its preparation method, and its application. Background Technology

[0002] Cosmetics are susceptible to microbial contamination during production, storage, and use, leading to product deterioration, loss of efficacy, and even skin safety issues. Traditional preservatives, such as parabens and formaldehyde releasers, while having significant antibacterial effects, suffer from drawbacks such as strong irritation and high risk of sensitization. Furthermore, their poor water solubility in oil-based systems (such as pure oils and creams) results in uneven dispersion, making it difficult to meet international preservative challenge standards such as USP 51.

[0003] Existing oil-soluble preservatives are mostly single substances with narrow antibacterial spectra (e.g., single esters are insufficient in inhibiting Gram-negative bacteria, and single alcohols have limited effectiveness against fungi), failing to cover complex microbial contamination scenarios. Furthermore, their antibacterial effects are short-lived and their preservative efficacy is poor. Especially in water-in-oil creams, traditional water-soluble preservatives tend to accumulate in the aqueous phase, leaving the oil phase with potential for microbial contamination, leading to product failure in USP 51 testing. Therefore, developing a compound preservative system that combines oil solubility, broad-spectrum antibacterial activity, and mildness, while passing the USP 51 preservative challenge test, is key to solving the preservative challenges of oil-based and water-in-oil cosmetics. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a mild anti-corrosion composition, its preparation method and application, so as to solve the problem that oil-soluble anti-corrosion components in the prior art cannot simultaneously possess oil solubility, broad-spectrum antibacterial properties and mildness.

[0005] The present invention solves the above-mentioned technical problems. The present invention provides a mild antiseptic composition comprising the following components, by mass percentage: 13.0%-16.7% oil-soluble alcohols, 2.0%-5.0% fatty acid salts, 1.0%-3.0% plant extracts, 1-3% polyol esters, and the balance being antibacterial oils. The antibacterial oil is one of triethyl citrate and glyceryl undecenoate; The oil-soluble alcohol is one of ethylhexylglycerol, octyl glycol, and hexyldecyl alcohol; The fatty acid salt is zinc octanoate; zinc octanoate releases zinc ions to destroy microbial cell membranes, and at the same time can form coordination bonds with plant extracts to improve antibacterial long-term efficacy. The polyol ester is polyglycerol-3 diisostearate; The plant extract is peony bark extract and sarsaparilla acid in a mass ratio of 3:1. The preparation of the peony bark extract involves grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 1-3:13-17 g / mL for extraction for 6-8 hours. After high-pressure inactivation, the extract is filtered by macroporous resin chromatography, and the filtrate is dried under reduced pressure. The alcohol-oil solution is composed of ethanol and isohexadecane at a volume ratio of 2-3:1. The mass concentrations of xylanase and keratinase are 0.5-0.8% and 2-4%, respectively. A "polar-nonpolar synergistic dissolution system" can efficiently dissolve paeonol, which disrupts microbial cell membranes and inhibits the activity of microbial respiratory enzymes. Succinic acid inhibits microbial DNA replication and reduces alcohol irritation, thus synergistically inhibiting bacteria. The oligoxylan and fatty acids obtained by enzymatic hydrolysis can be used as natural oil phase dispersants to improve the compatibility of the extract with the preservative composition, prevent the release of active ingredients, and increase antibacterial properties. The present invention also provides a method for preparing a mild preservative composition, comprising the following steps: Step 1: Add antibacterial oil to the reaction vessel and stir and melt it at 300-400 rpm for 10-20 minutes at a temperature of 50-55℃. Then add fatty acid salts that have been pulverized to a particle size of D90≤2μm, maintain the speed and ultrasonically disperse and stir for 8-12 minutes to obtain the oil phase. Step 2: Lower the temperature of the oil phase to 40-45℃, add oil-soluble alcohols and plant extracts, stir at 500-600 rpm for 10-20 minutes, and obtain a mild preservative composition after cooling and aging. The frequency of the ultrasonic dispersion is 15-20 kHz.

[0006] This invention provides an application of a mild preservative composition, wherein the application is in pure oil, water-in-oil cream, and oil-in-water cream; The application is added at a rate of 0.5-5%; Preferably, the amount of the application added is 2-3%.

[0007] The beneficial effects of this invention are as follows: The mild preservative composition provided by this invention exhibits a significant synergistic effect among its components. Paeonol forms a stable weak coordination bond with zinc ions in fatty acid salts, significantly delaying the release rate of antibacterial components and achieving long-lasting antibacterial effect. Simultaneously, polyol esters can synergistically interact with oil-soluble alcohols, specifically enhancing the system's inhibitory effect on fungi such as Candida albicans. The enzymatic hydrolysis product, xylo-oligosaccharide, synergistically interacts with ethylhexylglycerin; xylo-oligosaccharide can adsorb onto the surface of microbial cell membranes, disrupting cell membrane integrity and accelerating the penetration of antibacterial components such as ethylhexylglycerin into the cells. The added polyglycerol-3... The triterpenoid structures of diisostearate and sagenic acid interact through hydrogen bonds, effectively reducing the interfacial tension of the system and preventing the release of active components such as sagenic acid and paeonol. Simultaneously, it inhibits the oxidative rancidity of the oil phase components, significantly improving the product's storage stability. The components of this invention work synergistically to achieve long-lasting antibacterial and preservative effects. The ingredients are mild and non-irritating, exhibiting good compatibility when added to other compositions without affecting the efficacy of the active ingredients. Through multiple mechanisms such as pH adjustment, disruption of microbial cell membranes, and inhibition of metabolic enzyme activity, it synergistically inhibits bacteria. It exhibits excellent oil solubility and is suitable for pure oil formulations, water-in-oil creams, and oil-in-water creams. This solves the problems of traditional preservatives being highly irritating, having poor oil phase dispersion, and being difficult to pass international standard tests. It is characterized by its mildness, high efficiency, and low dosage. Detailed Implementation

[0008] The present invention will be further described in detail below through specific implementation examples. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of protection of the present invention. After reading the present invention, any modifications of the present invention in various equivalent forms by those skilled in the art fall within the scope of the appended claims.

[0009] Unless otherwise specified, all raw materials and reagents used in this invention are from the conventional market.

[0010] Example 1 A method for preparing a mild preservative composition includes the following steps: Step 1: Add 78% triethyl citrate to the reactor and stir and melt at 52℃ and 350rpm for 15min. Add 2% polyglycerol-3 diisostearate and stir for 5min. Then add 3.0% zinc octanoate that has been ultra-finely pulverized to a particle size D90≤2μm. Maintain the stirring speed and ultrasonically disperse and stir at a frequency of 15kHz for 10min to obtain the oil phase. The plant extract is peony bark extract and sarsaparilla acid in a mass ratio of 3:1. Step 2: Reduce the temperature of the oil phase to 40°C, add 15% hexyldecyl alcohol and 2% plant extract, stir at 550 rpm for 15 min, and after cooling and aging, obtain a mild preservative composition. The preparation of the peony bark extract involves grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 2:15 g / mL for 7 hours. After high-pressure inactivation, the extract is filtered by macroporous resin chromatography, and the filtrate is dried under reduced pressure. The alcohol-oil solution is composed of ethanol and isohexadecane in a volume ratio of 2:1. The mass concentrations of xylanase and keratinase are 0.7% and 3%, respectively.

[0011] Example 2 A method for preparing a mild preservative composition includes the following steps: Step 1: Add 83% glycerol undecenoate to the reactor and stir and melt at 50℃ and 300 rpm for 10 min. Add 1% polyglycerol-3 diisostearate and stir for 4 min. Then add 2.0% zinc octanoate that has been ultra-finely pulverized to a particle size D90≤2μm. Maintain the stirring speed and ultrasonically disperse and stir at a frequency of 15kHz for 8 min to obtain the oil phase. The plant extract is peony bark extract and sarsaparilla acid in a mass ratio of 3:1. Step 2: Reduce the temperature of the oil phase to 40°C, add 13.0% caprylyl glycol and 1.0% plant extract, stir at 500 rpm for 10 min, and after cooling and aging, obtain a mild preservative composition. The preparation of the peony bark extract involves grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 1:13 g / mL for 6 hours. After high-pressure inactivation, the extract is filtered by macroporous resin chromatography, and the filtrate is dried under reduced pressure. The alcohol-oil solution is composed of ethanol and isohexadecane in a volume ratio of 2:1. The mass concentrations of xylanase and keratinase are 0.5% and 2%, respectively.

[0012] Example 3 A method for preparing a mild preservative composition includes the following steps: Step 1: Add 72.3% triethyl citrate to the reactor and stir and melt at 55℃ and 400rpm for 20min. Add 3% polyglycerol-3 diisostearate and stir for 6min. Then add 5.0% zinc octanoate that has been ultra-finely ground to a particle size D90≤2μm. Maintain the stirring speed and ultrasonically disperse and stir at a frequency of 20kHz for 12min to obtain the oil phase. The plant extract is peony bark extract and sarsaparilla acid in a mass ratio of 3:1. Step 2: Reduce the temperature of the oil phase to 45°C, add 16.7% ethylhexylglycerin and 3.0% plant extract, stir at 600 rpm for 20 min, and after cooling and aging, obtain a mild preservative composition. The preparation of the peony bark extract involves grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 3:17 g / mL for extraction for 8 hours. After high-pressure inactivation, the extract is filtered by macroporous resin chromatography, and the filtrate is dried under reduced pressure. The alcohol-oil solution is composed of ethanol and isohexadecane at a volume ratio of 3:1. The mass concentrations of xylanase and keratinase are 0.8% and 4%, respectively.

[0013] Example 4 A method for preparing a mild preservative composition includes the following steps: Step 1: Add 74.3% glycerol undecenoate to the reactor and stir and melt at 50℃ and 400 rpm for 10 min. Add 3% polyglycerol-3 diisostearate and stir for 4 min. Then add 5.0% zinc octanoate that has been ultra-finely ground to a particle size D90≤2μm. Maintain the stirring speed and ultrasonically disperse and stir at a frequency of 15kHz for 12 min to obtain the oil phase. The plant extract is peony bark extract and sarsaparilla acid in a mass ratio of 3:1. Step 2: Reduce the temperature of the oil phase to 40°C, add 16.7% hexyldecyl alcohol and 1.0% plant extract, stir at 600 rpm for 10 min, and after cooling and aging, obtain a mild preservative composition. The preparation of the peony bark extract involves grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 1:14 g / mL for 7 hours. After high-pressure inactivation, the extract is filtered by macroporous resin chromatography, and the filtrate is dried under reduced pressure. The alcohol-oil solution is composed of ethanol and isohexadecane in a volume ratio of 2:1. The mass concentrations of xylanase and keratinase are 0.6% and 2%, respectively.

[0014] Example 5 Pure plant essential oil Formula: 72% jojoba oil, 20% rosehip oil, 3% tocopherol, 3% preservative combination (Example 1), 0.1% fragrance.

[0015] Preparation: Mix all ingredients, stir at 50°C for 20 minutes until homogeneous, and fill after cooling.

[0016] USP 51 test results: Initial bacterial concentration: 10 6 CFU / g (mixed inoculation of 5 types of bacteria); 14 days: Bacteria decreased by ≥3 log (99.9%), yeast decreased by ≥2 log (99%), and mold showed no growth; 28 days: No bacterial resuscitation was observed in any strain, and the inhibition rate remained ≥99.9%.

[0017] Example 6 Oil-in-water repair cream Formula: 16% liquid paraffin, 2% beeswax, 0.8% magnesium stearate, 1% PEG-30 dihydroxystearate, 2% cetyl PEG / PPG-10 / 1 dimethylsiloxane, 8% glycerin, 2% sodium chloride, 65.7% deionized water, and 2.5% preservative combination (Example 2).

[0018] Preparation: The oil phase (liquid paraffin, beeswax, PEG-30 dihydroxystearate, cetyl PEG / PPG-10 / 1 dimethylsiloxane, preservative combination, magnesium stearate) and the aqueous phase (glycerol, sodium chloride, deionized water) were heated to 80°C respectively. The aqueous phase was slowly added to the oil phase and emulsified by rapid stirring. The mixture was stirred until room temperature was reached.

[0019] USP 51 test results: Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 3.6 log, Escherichia coli decreased by 3.9 log, Pseudomonas aeruginosa decreased by 3.5 log, Candida albicans decreased by 2.7 log, and Aspergillus niger showed no growth; 28 days: All bacterial counts were <10 CFU / g, meeting USP 51 requirements.

[0020] Example 7 Water-in-oil moisturizing cream Formula: Caprylic / Capric Triglyceride 10%, Glycerin 10%, Montanov™ 68 Emulsifier (Cetearyl Alcohol and Cetearyl Glucoside) 3%, Arlacel™ 165 Emulsifier (Glyceryl Stearate and PEG-100 Stearate) 2%, Sodium Hyaluronate 0.1%, Deionized Water 71.8%, Preservative Combination (Example 3) 3%, Fragrance 0.1%.

[0021] Preparation: The oil phase (caprylic / capric triglycerides, Montanov™ 68, Arlacel™ 165, preservative combination) and the aqueous phase (glycerol, sodium hyaluronate, deionized water) were heated to 80°C respectively. The oil phase was added to the aqueous phase for emulsification. The temperature was lowered to 45°C and the fragrance was added. The mixture was stirred until room temperature was reached.

[0022] USP 51 test results: Initial bacterial concentration: 10 6 CFU / g; 14 days: Pseudomonas aeruginosa decreased by 3.7 log, Candida albicans decreased by 2.6 log, and Aspergillus niger showed no growth; 28 days: All bacterial strains showed no activity and passed the test completely.

[0023] Example 8 Waterless lipstick Formula: 47% castor oil, 25% microcrystalline wax, 10% carnauba wax, 3% pigment, and 2% preservative combination (Example 3).

[0024] Preparation: Heat waxes and castor oil to 85°C to melt, add pigments and preservatives, stir evenly, and then pour into molds.

[0025] USP 51 test results: Initial bacterial concentration: 10 6 CFU / g; 28 days: Staphylococcus aureus and Escherichia coli inhibition rate ≥99.98%, Candida albicans and Aspergillus niger no longer survived.

[0026] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 does not contain zinc octoate, while everything else remains the same.

[0027] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 4.0 log, Escherichia coli decreased by 4.2 log, Pseudomonas aeruginosa decreased by 3.8 log, Candida albicans decreased by 2.5 log, and Aspergillus niger increased by 0.3 log (trace colonies appeared). 28 days: Bacterial count <10 CFU / g, Candida albicans 120 CFU / g, Aspergillus niger 50 CFU / g (Fungi did not meet the standard, not in compliance with USP 51).

[0028] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that Comparative Example 2 uses commercially available peony bark extract instead of the peony bark extract prepared in this invention, while everything else remains the same.

[0029] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 3.8 log, Escherichia coli decreased by 4.0 log, Pseudomonas aeruginosa decreased by 3.6 log, Candida albicans decreased by 3.2 log, and Aspergillus niger decreased by 1.0 log; 28 days: All bacterial counts were <10 CFU / g (meeting the standard), but the logarithmic decrease was 1.2-1.6 log lower than that of 14 days in Example 1.

[0030] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that Comparative Example 3 does not contain oxalic acid, while everything else remains the same.

[0031] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 5.0 log, Escherichia coli decreased by 5.3 log, Pseudomonas aeruginosa decreased by 4.8 log, Candida albicans decreased by 3.5 log, and Aspergillus niger decreased by 2.2 log; 28 days: All bacterial counts were <10 CFU / g (meeting the standard), with only fungal inhibition slightly weaker than in Example 1.

[0032] Comparative Example 4 The difference between Comparative Example 4 and Example 1 is that Comparative Example 4 does not contain polyglycerol-3 diisostearate, while all other aspects remain the same.

[0033] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 4.5 log, Escherichia coli decreased by 4.8 log, Pseudomonas aeruginosa decreased by 4.3 log, Candida albicans decreased by 4.0 log, and Aspergillus niger decreased by 2.5 log; 28 days: All bacterial counts were <10 CFU / g (meeting the standard), and the logarithm of the decrease at 14 days was 0.5-0.8 log lower than that in Example 1.

[0034] Comparative Example 5 The difference between Comparative Example 5 and Example 1 is that no oil-soluble alcohols were added to Comparative Example 5, while everything else remained the same.

[0035] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 1.8 log, Escherichia coli decreased by 2.0 log, Pseudomonas aeruginosa decreased by 1.5 log, Candida albicans decreased by 1.2 log, and Aspergillus niger increased by 0.8 log; 28 days: All bacterial counts were >10³ CFU / g (does not meet USP 51 requirements).

[0036] Comparative Example 6 The difference between Comparative Example 6 and Example 1 is that Comparative Example 6 does not contain antibacterial oils, while everything else remains the same.

[0037] Initial bacterial concentration: 10 7 CFU / g; 14 days: Staphylococcus aureus decreased by 2.2 log, Escherichia coli decreased by 2.5 log, Pseudomonas aeruginosa decreased by 1.9 log, Candida albicans decreased by 1.0 log, and Aspergillus niger increased by 0.5 log (obvious colonies appeared). 28 days: Staphylococcus aureus 350 CFU / g, Escherichia coli 280 CFU / g, Candida albicans 520 CFU / g, Aspergillus niger 180 CFU / g (all strains failed to meet the standards and do not comply with USP 51).

[0038] The antiseptic compositions prepared in Examples 1-4 were subjected to irritation tests. Fertilized chicken embryos were cultured in an incubator at 37.8℃ and 60% humidity for 10 days, and dead embryos were removed. The chicken embryo shells were carefully broken to expose the intact and transparent vascular membranes, and the surface was rinsed with physiological saline. The preservative composition prepared in the example was diluted with 8% glycerol solution. 0.1 mL of the 8% dilution of the test group, 0.1% sodium dodecyl sulfate solution of the positive group, and the blank control (physiological saline) were dropped onto the CAM surface respectively, and incubated for 5 min. After that, the vascular congestion, hemorrhage, and dissolution of the CAM were observed and scored according to the scoring standard (0-10 points).

[0039] Evaluation criteria: 0-3 points: no irritation; 3-6 points: slight irritation; 6-10 points: moderate / strong irritation. The experimental results are shown in Table 1.

[0040] Table 1. Diameter of inhibition zone As shown in Table 1, the irritation level of the preservative composition of the present invention is 0 or 1, indicating low irritation. It is a mild preservative composition and is suitable for addition to skin care products and cosmetics.

[0041] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A mild anti-corrosion composition, characterized in that, It contains the following ingredients, by weight percentage: 13.0%-16.7% oil-soluble alcohols, 2.0%-5.0% fatty acid salts, 1.0%-3.0% plant extracts, 1-3% polyol esters, and the balance being antibacterial oils; The plant extracts are peony bark extract and sarcopenic acid.

2. The mild anti-corrosion composition according to claim 1, characterized in that, The antibacterial oil is one of triethyl citrate and glyceryl undecenoate.

3. The mild anti-corrosion composition according to claim 1, characterized in that, The oil-soluble alcohol is one of ethylhexylglycerol, octyl glycol, and hexyldecyl alcohol.

4. The mild anti-corrosion composition according to claim 1, characterized in that, The fatty acid salt is zinc octanoate.

5. The mild anti-corrosion composition according to claim 1, characterized in that, The polyol ester is polyglycerol-3 diisostearate.

6. The mild anti-corrosion composition according to claim 1, characterized in that, The plant extract is a peony bark extract and sarsaparilla acid in a mass ratio of 3:

1.

7. The mild anti-corrosion composition according to claim 1, characterized in that, The peony bark extract was prepared by grinding and pulverizing peony bark, then adding it to an alcohol-oil solution containing xylanase and keratinase at a solid-liquid ratio of 1-3:13-17 g / mL for 6-8 hours. After high-pressure inactivation, the extract was filtered by macroporous resin chromatography, and the filtrate was dried under reduced pressure. The alcohol-oil solution was composed of ethanol and isohexadecane at a volume ratio of 2-3:

1. The mass concentrations of xylanase and keratinase were 0.5-0.8% and 2-4%, respectively.

8. A method for preparing a mild anticorrosive composition, used to prepare a mild anticorrosive composition as described in any one of claims 1-7, characterized in that, Includes the following steps: Step 1: Add antibacterial oil to the reactor and stir and melt it at 300-400 rpm for 10-20 minutes at a temperature of 50-55℃. Add polyol ester and stir for 4-6 minutes. Then add fatty acid salts that have been pulverized to a particle size D90≤2μm. Maintain the stirring speed and ultrasonically disperse and stir for 8-12 minutes to obtain the oil phase. Step 2: Lower the temperature of the oil phase to 40-45℃, add oil-soluble alcohols and plant extracts, stir at 500-600 rpm for 10-20 minutes, and after cooling and aging, obtain a mild preservative composition.

9. The method for preparing a mild anti-corrosion composition according to claim 8, characterized in that, The frequency of the ultrasonic dispersion is 15-20 kHz.

10. The application of a mild anti-corrosion composition for use with any one of claims 1-7, characterized in that, The application is in pure oils, water-in-oil creams, and oil-in-water creams.

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