Bacteriostatic, deodorant and antiperspirant composition containing tetrachloro-hydroxy aluminum zirconium GLY coordination compound and application of antibacterial, deodorant and antiperspirant composition
By adding tetrachlorohydroxyaluminum zirconium GLY coordination compound and cetrium bromide to the antiperspirant, combined with ultrasonic extraction and alkaline amino acid enrichment technology, the body odor problem caused by sweat bacterial decomposition is solved, and the body odor problem is achieved Better antibacterial, deodorant and antiperspirant effects.
Patent Information
- Application Number
- CN202411119569.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-14
- Publication Date
- 2024-12-27
- Estimated Expiration
- 2044-08-14
AI Technical Summary
Existing antiperspirants cannot effectively prevent body odor or sweat odor caused by bacterial decomposition of sweat, causing hyperhidrosis to feel embarrassed in social and work.
A composition containing tetrachlorohydroxyaluminum zirconium GLY coordination compound with cetrium bromide, peony root crust extract, glycerol glucoside, oat β-glucan, PEG-40 hydrogenated castor oil, flavor and citric acid , by ultrasonic extraction and alkaline amino acid enrichment technology, a composition with antibacterial, deodorization and antiperspiration was prepared.
This composition not only significantly improves the antiperspirant effect, but also significantly reduces the production of odor by inhibiting bacterial growth, providing better deodorization effect, especially in patients with hyperhidrosis.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of daily chemical products, and specifically relates to a composition containing a tetrachloroaluminum zirconium hydroxy GLY coordination compound and having antibacterial, deodorizing and antiperspirant effects, and application thereof. Background Art
[0002] Sweat secretion is controlled by temperature and emotions. It is an extremely important physiological function to maintain and control body temperature. It can also promote metabolism and is of great significance to maintaining human health. However, due to physiological reasons, some people's sweat glands are too developed and they are prone to hyperhidrosis. They sweat a lot in a slightly hot environment, under stress or slight exercise. In the hot summer, sweat will be decomposed by bacteria and cause body odor or sweat odor. The above inconveniences often make patients feel embarrassed and affect their normal social life and work.
[0003] ACH, Chinese name Aluminum Chlorohydrate, English name Aluminum Chlorohydrate, molecular formula is Al2(OH)5Cl x ·nH2O. It is an inorganic polymer compound with a higher alkalinity (basicity) than polyaluminium chloride and second only to aluminium hydroxide. It is bridged and polymerised through hydroxyl groups and has the highest number of hydroxyl groups in the molecule. It is a white powdery solid and its solution is a colourless transparent liquid. It has strong bridging adsorption properties and is easily soluble in water. The hydrolysis process is accompanied by physical and chemical processes such as electrochemistry, coagulation, adsorption and precipitation.
[0004] In 1960, people modified the commonly used ACH and proposed a method of adding zirconium salt modification. At the same time, a certain amount of glycine was added to further reduce the irritation, and glycinate aluminum zirconium antiperspirant active agent was prepared. The application results show that the antiperspirant effect of glycinate aluminum zirconium is much stronger than ACH. However, even so, the antiperspirant effect of glycinate aluminum zirconium is still limited, and it still cannot avoid the social problem of body odor or sweat odor caused by sweat being decomposed by bacteria. Summary of the invention
[0005] The purpose of the present invention is to overcome the problems existing in the prior art and provide a composition containing a tetrachloroaluminum zirconium hydroxy GLY coordination compound and having antibacterial, deodorizing and antiperspirant effects and its application. The composition provided by the present invention not only has an antiperspirant effect, but also has an antibacterial effect.
[0006] The purpose of the present invention and the solution to the technical problem are achieved by adopting the following technical solutions.
[0007] In a first aspect, a composition containing a tetrachloroaluminum zirconium GLY coordination compound and having antibacterial, deodorizing and antiperspirant effects is provided. The composition comprises the following components in weight percentage: 5-15% of tetrachloroaluminum zirconium GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 0.1-0.5% of peony root bark extract, 2-5% of glyceryl glucoside, 1-5% of oat β-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1.5% of citric acid, and the remainder of water.
[0008] As an optional embodiment of the composition of the first aspect, the peony root bark extract is prepared according to the following steps:
[0009] The dried root bark of peony is crushed and ground, and then passed through a 100-200 mesh sieve to obtain peony root bark powder;
[0010] The peony root bark powder and the extraction solvent are mixed in a mass volume ratio of 1 g: 20-40 mL and ultrasonicated, then soaked for 4-10 hours, and finally the distillate is collected by refluxing in a water bath to obtain a crude extract;
[0011] Add a basic amino acid / ethanol mixture to the obtained crude extract at a volume ratio of 1:20-30, and continue stirring at 40-60° C. for 1-5 hours. After standing for 18-24 hours, filter out the precipitate, and vacuum freeze-dry the precipitate to obtain a peony root bark extract.
[0012] As an optional implementation of the composition of the first aspect, the extraction solvent is a mixture of ethanol, chloroform and water in a volume ratio of 1:0.5:10-30.
[0013] As an optional implementation of the composition of the first aspect, the ultrasonic conditions are: frequency 80-120 kHz, and ultrasonic time 40-60 min.
[0014] As an optional embodiment of the composition of the first aspect, the basic amino acid is selected from any one of lysine, arginine and histidine.
[0015] As an optional embodiment of the composition of the first aspect, the alkaline amino acid / ethanol mixed solution is prepared by mixing the alkaline amino acid with an ethanol solution having a volume fraction of 75% in a mass-to-volume ratio of 1 g: 50-150 mL.
[0016] In a second aspect, a method for preparing a composition is provided, characterized in that the preparation method comprises the following steps:
[0017] Preparation of Paeonia suffruticosa Root Bark Extract:
[0018] The dried root bark of peony is crushed and ground, and then passed through a 100-200 mesh sieve to obtain peony root bark powder;
[0019] The peony root bark powder and the extraction solvent are mixed in a mass volume ratio of 1 g: 20-40 mL and ultrasonicated, then soaked for 4-10 hours, and finally the distillate is collected by refluxing in a water bath to obtain a crude extract;
[0020] Adding a basic amino acid / ethanol mixture to the obtained crude extract in a volume ratio of 1:20-30, stirring continuously at 40-60° C. for 1-5 hours, letting it stand for 18-24 hours, filtering out the precipitate, and vacuum freeze-drying the obtained precipitate to obtain a peony root bark extract;
[0021] Weigh the raw materials according to weight percentage: 5-15% of aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 0.1-0.5% of peony root bark extract, 2-5% of glyceryl glucoside, 1-5% of oat β-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1.5% of citric acid, and the balance of water;
[0022] First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved; then peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly; finally, PEG-40 hydrogenated castor oil and essence that have been pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0023] As an optional implementation of the preparation method described in the second aspect, the extraction solvent is a mixture of ethanol, chloroform and water in a volume ratio of 1:0.5:10-30.
[0024] As an optional implementation of the preparation method described in the second aspect, the ultrasonic conditions are: frequency 80-120 kHz, and ultrasonic time 40-60 min.
[0025] As an optional implementation of the preparation method described in the second aspect, the alkaline amino acid / ethanol mixed solution is prepared by mixing the alkaline amino acid and an ethanol solution with a volume fraction of 75% in a mass-to-volume ratio of 1 g: 50-150 mL.
[0026] As an optional implementation of the preparation method described in the second aspect, the basic amino acid is selected from any one of lysine, arginine and histidine.
[0027] By means of the above technical solution, the present invention has at least the following advantages:
[0028] 1. Tetrachloroaluminum zirconium GLY coordination compound is a common antiperspirant active substance with the characteristics of low skin irritation and is one of the metal salts with better antiperspirant effect. Cetrimonium bromide is white or light yellow crystals to powder, easily soluble in isopropanol, soluble in water, produces a large amount of foam when shaken, and has good compatibility with cationic, nonionic and amphoteric surfactants. It has excellent penetration, softening, emulsification, antistatic, biodegradability and bactericidal properties. However, the use of tetrachloroaluminum zirconium GLY coordination compound alone will limit its antiperspirant effect, and excessive sweating will promote bacterial reproduction and produce odor. Based on the above, the present invention provides a composition containing tetrachloroaluminum zirconium GLY coordination compound and antibacterial deodorant and antiperspirant and its application, and the antibacterial deodorant and antiperspirant composition uses tetrachloroaluminum zirconium GLY coordination compound and cetrimonium bromide as main active ingredients. The present invention unexpectedly discovered during the experiment that the tetrachloroaluminum zirconium GLY coordination compound combined with cetrimonium bromide can not only synergistically reduce sweat odor, but also cetrimonium bromide can inhibit bacterial growth, thereby achieving the purpose of reducing odor generation. It has been verified that the combined use of the tetrachloroaluminum zirconium GLY coordination compound and cetrimonium bromide is significantly better than the use of the tetrachloroaluminum zirconium GLY coordination compound and cetrimonium bromide alone. The present invention provides a direction for the treatment of patients with hyperhidrosis or the development of deodorant and antiperspirant products.
[0029] 2. Paeonia suffruticosa root bark is the dry root bark of the Ranunculaceae plant peony. Studies have shown that peony root bark extract contains phenol and phenolic glycosides, monoterpenes and glycoside compounds, triterpenes, sterols and their glycosides. In addition, peony root bark extract decoction has a strong inhibitory effect on some microorganisms such as Escherichia coli, Shigella dysenteriae, Staphylococcus aureus, hemolytic streptococci, etc., and its effects are clearing away heat and cooling blood, promoting blood circulation and removing blood stasis, and have anti-inflammatory, anti-tumor, hypoglycemic, anti-allergic, cardiovascular protection and other effects. Conventional peony root bark extraction adopts solvents such as water and ethanol, combined with distillation and other technologies, but the active substances in the extract are relatively abundant, and the loss of active substances is easily caused during the extraction process, which greatly reduces the active substance content in the extract, thereby further reducing the efficacy of the extract. Therefore, the present invention maximizes the extraction of active substances contained therein by combining ultrasonic solvents and distillation, and enriches and precipitates active substances by adding basic amino acids on the other hand to improve the content of active substances.
[0030] 3. As a more preferred embodiment of the present invention, the composition of the present invention also includes a microcarrier capable of enriching the active substances in the composition. The microcarrier of the present invention is a three-dimensional ordered macroporous metal-organic framework material as a carrier matrix, and a sulfonated modified three-dimensional ordered macroporous metal-organic framework material is obtained by the modification of 2,3-dihydroxynaphthalene-6-sodium sulfonate, and then a coupling group is added to the modified three-dimensional ordered macroporous metal-organic framework material under the action of a silane coupling agent, which can connect organic matter and inorganic matter together through the action of a coupling agent, so that the effective active substances in the composition can be enriched on the microcarrier and play a greater role. It has been verified by experiments that the effect of the effective active substances can be improved by the enrichment of microcarriers.
[0031] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the preferred embodiments of the present invention are described in detail as follows. DETAILED DESCRIPTION
[0032] In order to make the technical means, creative features, objectives and effects of the present invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0033] Unless otherwise specified, the sources of the products used in the following examples are as follows: tetrachloroaluminum zirconium GLY coordination compound was purchased from Guangzhou Tenusi Chemical Co., Ltd.; cetrimonium bromide was purchased from Guangzhou Tenusi Chemical Co., Ltd.; peony root bark and oat β-glucan were purchased from Guangzhou Tenusi Chemical Co., Ltd.; PEG-40 hydrogenated castor oil was purchased from Evonik, Germany; flavor was purchased from IFF; citric acid was purchased from Anhui Fengyuan Biochemical Co., Ltd.; other materials and reagents of unspecified origin can be obtained from commercial channels.
[0034] Unless otherwise specified, the preparation method of the three-dimensional ordered macroporous metal-organic framework material in the following Examples 4-7 is as follows: the polystyrene emulsion is centrifuged at a speed of 5000r / h for 6h, and then the supernatant is removed to obtain the bottom precipitate. After drying at 90°C overnight, an ordered polystyrene template is obtained. It is immersed in a 0.05g / mL zinc nitrate / methanol dispersion for 2 hours, and then the polystyrene template is fished out and dried overnight. The polystyrene template immersed in zinc nitrate / methanol solution is immersed in a 0.1g / mL 2-methylimidazole / methanol solution and allowed to stand for 48 hours to obtain a polystyrene / organic framework composite material. The polystyrene / organic framework composite material is immersed in N,N-dimethylformamide, and the polystyrene is removed after stirring for 24 hours to obtain a three-dimensional ordered macroporous metal-organic framework material.
[0035] Unless otherwise specified, the experimental methods used in the following examples are all conventional methods.
[0036] Embodiment 1:
[0037] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 150 mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water in a volume ratio of 1:0.5:20) in a mass volume ratio of 1g:30mL and ultrasonicated at 100kHz for 50min, then soaked for 7h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. A histidine / ethanol mixture (composed of histidine and a 75% ethanol solution in a mass volume ratio of 1g:100mL) is added to the obtained crude extract in a volume ratio of 1:25 and stirred continuously at 50°C for 3h. After standing for 21h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0038] S2: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0039] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0040] Embodiment 2:
[0041] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 100-mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water in a volume ratio of 1:0.5:30) in a mass volume ratio of 1g:20mL and ultrasonicated at 80kHz for 60min, then soaked for 4h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. Lysine / ethanol mixed solution (composed of lysine and 75% ethanol solution in a mass volume ratio of 1g:50mL) is added to the obtained crude extract in a volume ratio of 1:20 and stirred continuously at 60°C for 1h. After standing for 24h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0042] S2: Weigh the raw materials according to weight percentage: 15% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.15% cetrimonium bromide, 0.5% peony root bark extract, 2% glyceryl glucoside, 5% oat β-glucan, 2% PEG-40 hydrogenated castor oil, 0.5% flavor, 1.5% citric acid, and the balance water.
[0043] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0044] Embodiment 3:
[0045] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 200 mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water in a volume ratio of 1:0.5:10) in a mass volume ratio of 1g:40mL and ultrasonicated at 120kHz for 40min, then soaked for 10h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. Arginine / ethanol mixed solution (composed of arginine and 75% ethanol solution in a mass volume ratio of 1g:150mL) is added to the obtained crude extract in a volume ratio of 1:30 and stirred continuously at 40°C for 5h. After standing for 18h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0046] S2: Weigh the raw materials according to weight percentage: 5% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.05% cetrimonium bromide, 0.1% peony root bark extract, 5% glyceryl glucoside, 1% oat β-glucan, 1% PEG-40 hydrogenated castor oil, 1% essence, 0.5% citric acid, and the balance water.
[0047] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0048] Embodiment 4:
[0049] As a more preferred embodiment of the present invention, the composition of the present invention also includes a microcarrier capable of enriching the active substance in the composition. It has been verified by experiments that the enrichment of the microcarrier can improve the efficacy of the effective active substance. Therefore, according to the weight percentage, the composition comprises the following components: 5-15% of tetrachlorohydroxyaluminum zirconium GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 1-5% of microcarrier, 0.1-0.5% of peony root bark extract, 2-5% of glycerol glucoside, 1-5% of oat beta-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1.5% of citric acid, and the balance of water.
[0050] The preparation method of the composition is:
[0051] Preparation of Paeonia suffruticosa Root Bark Extract: The method is the same as the above method and will not be repeated here.
[0052] Preparation of microcarriers: crushing and grinding a three-dimensional ordered macroporous metal-organic framework material and then passing it through a 500-1000 mesh sieve to obtain an ultrafine three-dimensional ordered macroporous metal-organic framework material powder; then dispersing the obtained ultrafine three-dimensional ordered macroporous metal-organic framework material powder in N,N-dimethylformamide, adding a 2,3-dihydroxynaphthalene-6-sodium sulfonate solution (mixed with 2,3-dihydroxynaphthalene-6-sodium sulfonate, sodium chloride, and 10-30wt% hydrochloric acid solution in a mass volume ratio of 1g:0.05-0.1g:30-80mL), stirring and reacting at 100-150°C for 2-3h, filtering, washing, and drying after the reaction is completed to obtain a modified three-dimensional ordered macroporous metal. The modified three-dimensional ordered macroporous metal-organic framework material is immersed in an ethanol solution of 40-60wt% silane coupling agent and stirred at room temperature for 10-12h, then filtered, and the obtained solid product is washed and dried to obtain a microcarrier; in the above reaction process, three-dimensional ordered macroporous metal-organic framework material powder, N,N-dimethylformamide and 2,3-dihydroxynaphthalene-6-sodium sulfonate solution are added in a mass volume ratio of 1g: 5-10mL: 10-30mL; the silane coupling agent is selected from any one of methyltrimethoxysilane, tetramethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, ethyltriethoxysilane and tetrapropoxysilane.
[0053] Weigh the raw materials according to weight percentage: 5-15% of aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 1-5% of microcarrier, 0.1-0.5% of peony root bark extract, 2-5% of glycerol glucoside, 1-5% of oat β-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1.5% of citric acid, and the balance of water;
[0054] First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 30-35° C. for 1-3 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0055] Embodiment 5:
[0056] S1: Preparation of Paeonia suffruticosa Root Bark Extract: The process is the same as described in Example 1 and will not be repeated herein.
[0057] S2: Preparation of microcarriers: The three-dimensional ordered macroporous metal-organic framework material is crushed and ground, and then passed through an 800-mesh sieve to obtain ultrafine three-dimensional ordered macroporous metal-organic framework material powder. The obtained ultrafine three-dimensional ordered macroporous metal-organic framework material powder is then dispersed in N,N-dimethylformamide, and then 2,3-dihydroxynaphthalene-6-sulfonic acid sodium solution (mixed by 2,3-dihydroxynaphthalene-6-sulfonic acid sodium, sodium chloride, and 20wt% hydrochloric acid solution according to a mass volume ratio of 1g:0.075g:55mL) is added, and the reaction is stirred at 125°C for 2.5h. After the reaction is completed, it is filtered, washed, and dried to obtain a modified three-dimensional ordered macroporous metal-organic framework material. The obtained modified three-dimensional ordered macroporous metal-organic framework material is immersed in a 50wt% methyltrimethoxysilane ethanol solution and stirred for 11h at room temperature, then filtered, and the obtained solid product is washed and dried to obtain a microcarrier. In the above reaction process, three-dimensional ordered macroporous metal-organic framework material powder, N,N-dimethylformamide and sodium 2,3-dihydroxynaphthalene-6-sulfonate solution are added in a mass volume ratio of 1g:7.5mL:20mL.
[0058] S3: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 3% microcarrier, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0059] S4: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 32° C. for 2 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0060] Embodiment 6:
[0061] S1: Preparation of Paeonia suffruticosa Root Bark Extract: The process is the same as described in Example 1 and will not be repeated herein.
[0062] S2: Preparation of microcarriers: The three-dimensional ordered macroporous metal-organic framework material is crushed and ground, and then passed through a 1000-mesh sieve to obtain ultrafine three-dimensional ordered macroporous metal-organic framework material powder. Then the obtained ultrafine three-dimensional ordered macroporous metal-organic framework material powder is dispersed in N,N-dimethylformamide, and then a sodium 2,3-dihydroxynaphthalene-6-sulfonate solution (obtained by mixing sodium 2,3-dihydroxynaphthalene-6-sulfonate, sodium chloride, and 10wt% hydrochloric acid solution in a mass volume ratio of 1g:0.1g:80mL) is added, and the reaction is stirred at 100°C for 3 hours. After the reaction is completed, it is filtered, washed, and dried to obtain a modified three-dimensional ordered macroporous metal-organic framework material; the obtained modified three-dimensional ordered macroporous metal-organic framework material is immersed in a 40wt% tetramethoxysilane ethanol solution and stirred at room temperature for 12 hours, then filtered, and the obtained solid product is washed and dried to obtain a microcarrier; during the above reaction process, the three-dimensional ordered macroporous metal-organic framework material powder, N,N-dimethylformamide and sodium 2,3-dihydroxynaphthalene-6-sulfonate solution are added in an amount of 1g:5mL:10mL in a mass volume ratio.
[0063] S3: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 3% microcarrier, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0064] S4: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 32° C. for 2 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0065] Embodiment 7:
[0066] S1: Preparation of Paeonia suffruticosa Root Bark Extract: The process is the same as described in Example 1 and will not be repeated herein.
[0067] S2: Preparation of microcarriers: The three-dimensional ordered macroporous metal-organic framework material is crushed and ground, and then passed through a 500-mesh sieve to obtain ultrafine three-dimensional ordered macroporous metal-organic framework material powder. Then the obtained ultrafine three-dimensional ordered macroporous metal-organic framework material powder is dispersed in N,N-dimethylformamide, and then a 2,3-dihydroxynaphthalene-6-sulfonic acid sodium solution (obtained by mixing 2,3-dihydroxynaphthalene-6-sulfonic acid sodium, sodium chloride, and 30wt% hydrochloric acid solution in a mass volume ratio of 1g:0.05g:30mL) is added, and the reaction is stirred at 150°C for 2h. After the reaction is completed, the modified three-dimensional ordered macroporous metal-organic framework material is filtered, washed, and dried to obtain the modified three-dimensional ordered macroporous metal-organic framework material; the obtained modified three-dimensional ordered macroporous metal-organic framework material is immersed in a 60wt% methyltriethoxysilane ethanol solution and stirred at room temperature for 10h, then filtered, and the obtained solid product is washed and dried to obtain a microcarrier; during the above reaction process, the three-dimensional ordered macroporous metal-organic framework material powder, N,N-dimethylformamide and the 2,3-dihydroxynaphthalene-6-sulfonic acid sodium solution are added in a mass volume ratio of 1g:10mL:30mL.
[0068] S3: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 3% microcarrier, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0069] S4: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 32° C. for 2 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0070] Comparative Example 1:
[0071] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 150 mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water mixed in a volume ratio of 1:0.5:20) in a mass volume ratio of 1g:30mL and ultrasonicated at 100kHz for 50min, then soaked for 7h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. A 75% ethanol solution is added to the obtained crude extract in a volume ratio of 1:25 and stirred continuously at 50°C for 3h. After standing for 21h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0072] S2: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0073] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0074] Comparative Example 2:
[0075] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 150 mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water in a volume ratio of 1:0.5:20) in a mass volume ratio of 1g:30mL and ultrasonicated at 100kHz for 50min, then soaked for 7h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. A histidine / ethanol mixture (composed of histidine and a 75% ethanol solution in a mass volume ratio of 1g:100mL) is added to the obtained crude extract in a volume ratio of 1:25 and stirred continuously at 50°C for 3h. After standing for 21h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0076] S2: Weigh the raw materials according to weight percentage: 0.1% cetrimonium bromide, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0077] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0078] Comparative Example 3:
[0079] S1: Preparation of peony root bark extract: The dried root bark of peony is crushed and ground and then passed through a 150 mesh sieve to obtain peony root bark powder. The peony root bark powder is mixed with an extraction solvent (composed of ethanol, chloroform, and water in a volume ratio of 1:0.5:20) in a mass volume ratio of 1g:30mL and ultrasonicated at 100kHz for 50min, then soaked for 7h, and finally the distillate is collected by reflux in a water bath to obtain a crude extract. A histidine / ethanol mixture (composed of histidine and a 75% ethanol solution in a mass volume ratio of 1g:100mL) is added to the obtained crude extract in a volume ratio of 1:25 and stirred continuously at 50°C for 3h. After standing for 21h, the precipitate is filtered and the obtained precipitate is vacuum freeze-dried to obtain a peony root bark extract.
[0080] S2: Weigh the raw materials according to weight percentage: 10% of tetrachloroaluminum zirconium GLY coordination compound, 0.3% of peony root bark extract, 3.5% of glyceryl glucoside, 3% of oat β-glucan, 1.5% of PEG-40 hydrogenated castor oil, 0.75% of flavor, 0.1% of citric acid, and the balance of water.
[0081] S3: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved. Then, peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly. Finally, PEG-40 hydrogenated castor oil and essence that are pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
[0082] Comparative Example 4:
[0083] S1: Preparation of Paeonia suffruticosa Root Bark Extract: The process is the same as described in Example 1 and will not be repeated herein.
[0084] S2: Preparation of microcarriers: The three-dimensional ordered macroporous metal-organic framework material is crushed and ground, and then passed through an 800-mesh sieve to obtain ultrafine three-dimensional ordered macroporous metal-organic framework material powder. The obtained three-dimensional ordered macroporous metal-organic framework material powder is soaked in a 50wt% methyltrimethoxysilane ethanol solution and stirred at room temperature for 11 hours, then filtered, and the obtained solid product is washed and dried to obtain a microcarrier.
[0085] S3: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 3% microcarrier, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0086] S4: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 32° C. for 2 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0087] Comparative Example 5:
[0088] S1: Preparation of Paeonia suffruticosa Root Bark Extract: The process is the same as described in Example 1 and will not be repeated herein.
[0089] S2: Preparation of microcarriers: The three-dimensional ordered macroporous metal-organic framework material is crushed and ground, and then passed through an 800-mesh sieve to obtain ultrafine three-dimensional ordered macroporous metal-organic framework material powder. The obtained ultrafine three-dimensional ordered macroporous metal-organic framework material powder is then dispersed in N,N-dimethylformamide, and then 2,3-dihydroxynaphthalene-6-sulfonic acid sodium solution (mixed with 2,3-dihydroxynaphthalene-6-sulfonic acid sodium, sodium chloride, and 20wt% hydrochloric acid solution according to a mass volume ratio of 1g:0.075g:55mL) is added, and the reaction is stirred at 125°C for 2.5h. After the reaction is completed, it is filtered, washed, and dried to obtain microcarriers.
[0090] S3: Weigh the raw materials according to weight percentage: 10% aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.1% cetrimonium bromide, 3% microcarrier, 0.3% peony root bark extract, 3.5% glyceryl glucoside, 3% oat β-glucan, 1.5% PEG-40 hydrogenated castor oil, 0.75% flavor, 0.1% citric acid, and the balance water.
[0091] S4: First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then the peony root bark extract is added and stirred evenly; then the microcarrier is added and stirred continuously at 32° C. for 2 hours; then citric acid, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly, and finally the pre-mixed PEG-40 hydrogenated castor oil and essence are added and stirred until completely uniform to obtain the composition.
[0092] Test Example 1: Antiperspirant and deodorant effect testing of different compositions
[0093] Test object: Compositions of Examples 1-3, Examples 5-7 and Comparative Examples 1-5
[0094] Experimental method: 110 subjects with excessive sweating and odor in the armpits were randomly recruited, half of them were male and half were female, aged between 18 and 40 years old, and the physical health of the volunteers did not affect the test results. The volunteers were divided into 11 groups, 10 people in each group, numbered 1-11, and no topical drugs were used 3 days before the test.
[0095] 3. Test method: After the bodies of the test volunteers were cleaned and dried, the compositions of Examples 1-3, Examples 5-7 and Comparative Examples 1-5 were sprayed evenly on the armpits of groups 1-11 of test volunteers in equal amounts, and the subjects were tested at 28-30°C for 8 hours under normal activity conditions. The antiperspirant and deodorant effects of the test volunteers in each group on the antiperspirant and deodorant liquid were statistically analyzed, and the antiperspirant effect scores were statistically analyzed. The scoring criteria are shown in Table 1. The deodorization rate was calculated according to the odor scoring criteria (see Table 2), and the results were averaged. The statistical results are shown in Table 3.
[0096] Deodorization rate = (score before using the composition - score after using the sample) / score before using the sample × 100%.
[0097] Table 1 Antiperspirant effect scoring criteria
[0098]
[0099]
[0100] Table 2 Odor scoring standards
[0101] score Degree of odor 0 No odor within 1 meter social distance 1 There is a slight odor within 1 meter of social distance 2 There is a bad smell within 1 meter social distance 3 Strong odor within 1 meter social distance 4 Strong odor within 1 meter social distance 5 The odor is very strong within the 1-meter social distance
[0102] Table 3 Statistics of antiperspirant and deodorant effects of different compositions
[0103]
[0104]
[0105] Groups 1-11 in the table correspond to the compositions of spraying Examples 1-3, Examples 5-7 and Comparative Examples 1-5, respectively. It can be seen from the results of Table 3 that compared with the test group spraying the composition of Comparative Examples 1-5, the test group spraying the compositions of Examples 1-3 and 5-7 of the present invention showed a more obvious antiperspirant effect and a higher deodorization rate. At the same time, compared with the test group spraying the composition of Examples 1-3, the subjects spraying the composition of Examples 5-7 had better antiperspirant and deodorization effects, which indicates that the antiperspirant and deodorization effects of the combination can be improved in the presence of microcarriers.
[0106] Test Example 2: Antibacterial effect detection of different compositions
[0107] Experimental subjects: Compositions of Examples 1, 5 and Comparative Examples 1-5
[0108] Experimental method: The antibacterial effect was tested using the inhibition zone method. The specific steps are as follows:
[0109] One day in advance, Staphylococcus aureus CMCC (B) 26112, Escherichia coli CMCC 44102, and Candida albicans ATCC 14053 were activated and diluted to 10 7 100 μL of each bacterium was added to LB nutrient agar medium and spread evenly.
[0110] The sterilized and dried filter paper was added to the composition of Examples 1, 5 and Comparative Examples 1-5 and soaked for 1 hour. The soaked filter paper was placed on the culture medium inoculated with bacteria and left to stand for 30 minutes, and then placed in an incubator for constant temperature and wet culture (36°C for bacteria, 24 hours; 30°C for fungi, 24 hours).
[0111] The plate that reached the incubation time was taken out, and the diameter (mm) of the transparent inhibition zone around the filter paper was measured with a vernier caliper. The test was repeated three times. The results are shown in Table 4.
[0112] Table 4 Statistics of antibacterial effects of different compositions
[0113]
[0114] It can be seen from the results in Table 4 that, compared with Comparative Examples 1-5, the compositions of Examples 1 and 5 of the present invention have better antibacterial effects.
[0115] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technician familiar with this profession can make some changes or modifications to equivalent embodiments of equivalent changes by using the methods and technical contents disclosed above without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still fall within the scope of the technical solution of the present invention.
Claims
1. A composition containing a tetrachloroaluminum zirconium hydroxy GLY coordination compound and having antibacterial, deodorizing and antiperspirant properties, characterized in that: The composition comprises the following components in weight percentage: 5-15% of aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 0.1-0.5% of peony root bark extract, 2-5% of glyceryl glucoside, 1-5% of oat beta-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1% of citric acid, and the balance of water.
2. The composition according to claim 1, characterized in that The peony root bark extract is prepared according to the following steps: The dried root bark of peony is crushed and ground, and then passed through a 100-200 mesh sieve to obtain peony root bark powder; The peony root bark powder and the extraction solvent are mixed in a mass volume ratio of 1 g: 20-40 mL and ultrasonicated, then soaked for 4-10 hours, and finally the distillate is collected by refluxing in a water bath to obtain a crude extract; Add a basic amino acid / ethanol mixture to the obtained crude extract at a volume ratio of 1:20-30, and continue stirring at 40-60° C. for 1-5 hours. After standing for 18-24 hours, filter out the precipitate, and vacuum freeze-dry the precipitate to obtain a peony root bark extract.
3. The composition according to claim 2, characterized in that The extraction solvent is prepared by mixing ethanol, chloroform and water in a volume ratio of 1:0.5:10-30.
4. The composition according to claim 2, characterized in that The ultrasonic conditions are: frequency 80-120 kHz, and ultrasonic time 40-60 min.
5. The composition according to claim 2, characterized in that The basic amino acid is selected from any one of lysine, arginine and histidine.
6. The composition according to claim 2, characterized in that The alkaline amino acid / ethanol mixed solution is prepared by mixing the alkaline amino acid with an ethanol solution having a volume fraction of 75% in a mass-to-volume ratio of 1 g: 50-150 mL.
7. A method for preparing the composition according to any one of claims 1 to 6, characterized in that: The preparation method comprises the following steps: Preparation of Paeonia suffruticosa Root Bark Extract: The dried root bark of peony is crushed and ground, and then passed through a 100-200 mesh sieve to obtain peony root bark powder; The peony root bark powder and the extraction solvent are mixed in a mass volume ratio of 1 g: 20-40 mL and ultrasonicated, then soaked for 4-10 hours, and finally the distillate is collected by refluxing in a water bath to obtain a crude extract; Adding a basic amino acid / ethanol mixture to the obtained crude extract in a volume ratio of 1:20-30, stirring continuously at 40-60° C. for 1-5 hours, letting it stand for 18-24 hours, filtering out the precipitate, and vacuum freeze-drying the obtained precipitate to obtain a peony root bark extract; Weigh the raw materials according to weight percentage: 5-15% of aluminum zirconium tetrachlorohydrate GLY coordination compound, 0.05-0.15% of cetrimonium bromide, 0.1-0.5% of peony root bark extract, 2-5% of glyceryl glucoside, 1-5% of oat β-glucan, 1-2% of PEG-40 hydrogenated castor oil, 0.5-1% of essence, 0.5-1.5% of citric acid, and the balance of water; First, cetrimonium bromide and aluminum zirconium tetrachlorohydroxide GLY coordination compound are stirred until completely dissolved in water, and then citric acid is added and stirred until completely dissolved; then peony root bark extract, glyceryl glucoside, and oat glucan are added in sequence and stirred evenly; finally, PEG-40 hydrogenated castor oil and essence that have been pre-mixed evenly are added and stirred until completely uniform to obtain the composition.
8. The preparation method according to claim 7, characterized in that: The extraction solvent is prepared by mixing ethanol, chloroform and water in a volume ratio of 1:0.5:10-30.
9. The preparation method according to claim 7, characterized in that: The ultrasonic conditions are: frequency 80-120 kHz, and ultrasonic time 40-60 min.
10. The preparation method according to claim 7, characterized in that: The alkaline amino acid / ethanol mixed solution is prepared by mixing the alkaline amino acid with an ethanol solution having a volume fraction of 75% in a mass-to-volume ratio of 1 g:50-150 mL; the alkaline amino acid is selected from any one of lysine, arginine and histidine.
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