A feminine intimate care fluid and method of making the same

Abstract

This invention relates to the field of feminine hygiene products, and discloses a feminine hygiene product and its preparation method. The feminine hygiene product is prepared from a functional phase solution, a gel matrix solution, an aqueous lactic acid solution, and an aqueous sodium lactate solution. The functional phase solution is obtained by mixing deionized water, glycerin, fructooligosaccharides, and chitosan quaternary ammonium salt. The chitosan quaternary ammonium salt is obtained by mixing an aqueous acetic acid solution, chitosan, and an aqueous 2,3-epoxypropyltrimethylammonium chloride solution. The gel matrix solution is obtained by mixing deionized water and poloxamer 407 powder. This invention uses poloxamer 407 as a temperature-sensitive gel matrix. When body temperature is reached, the hydrophobic polyoxypropylene segments in its molecules dehydrate and self-assemble to form a three-dimensional network gel structure, thereby transforming the liquid product into a semi-solid gel that can adhere tightly to the mucous membrane, prolonging the action time of the active ingredients.

Description

Technical Field

[0001] This invention relates to the field of feminine hygiene products, specifically to a feminine intimate hygiene product and its preparation method. Background Technology

[0002] The female genital area is a complex and delicate micro-ecosystem, and its health depends on the balance of flora, the integrity of the mucous membrane, and a suitable acid-base environment. A healthy female genital area is usually maintained in a slightly acidic environment with a pH of 3.8-4.5, dominated by beneficial bacteria such as lactobacilli. These bacteria can inhibit the growth of harmful microorganisms. At the same time, the genital mucosa needs to be kept moist to maintain its barrier function and resist external stimuli and infections.

[0003] Patent CN107007515A discloses a feminine intimate care solution comprising the following components by weight percentage: 0.1%-1% cationic thickener, 1%-20% moisturizer, 1%-20% surfactant, 1%-30% active ingredient, 0.1%-1% pH adjuster, and the remainder being purified water. The preparation method includes the following steps: (1) weighing the cationic thickener, adding purified water and stirring to form a homogeneous liquid; (2) adding the moisturizer, surfactant, and active ingredient to the homogeneous liquid and stirring until homogeneous; (3) adding the pH adjuster to the product obtained in step (2) to adjust the pH of the solution to 4-5. However, the existing technology still has some shortcomings: the product is quickly lost after application due to changes in body position, dilution by body fluids, or simple rinsing, failing to form an effective physical barrier, resulting in a short-lived interaction between the active ingredient and the mucous membrane, making it difficult to achieve a sustained protective or regulatory effect. Summary of the Invention

[0004] The purpose of this invention is to provide a feminine intimate care solution and its preparation method to solve the problems existing in the prior art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: A feminine hygiene wash, comprising a functional phase solution, a gel matrix solution, an aqueous lactic acid solution, and an aqueous sodium lactate solution; the functional phase solution is prepared by mixing deionized water, glycerin, fructooligosaccharides, and chitosan quaternary ammonium salt; the chitosan quaternary ammonium salt is prepared by mixing aqueous acetic acid solution, chitosan, and an aqueous 2,3-epoxypropyltrimethylammonium chloride solution; and the gel matrix solution is prepared by mixing deionized water and poloxamer 407 powder.

[0006] Furthermore, chitosan has a degree of deacetylation of 85-95% and a number-average molecular weight of 100,000-200,000 Da.

[0007] Furthermore, the mass fraction of the aqueous solution of 2,3-epoxypropyltrimethylammonium chloride is 50-70%.

[0008] Furthermore, the mass fraction of the acetic acid aqueous solution is 1-3%.

[0009] A method for preparing a feminine hygiene wash includes the following steps: (1) Add deionized water to the reactor, and slowly add poloxamer 407 powder over 20-30 minutes at a stirring speed of 200-300 rpm at 10-15℃. Then continue stirring for 4-6 hours, and then let it stand at 10-15℃ for 10-12 hours to obtain a gel matrix solution. (2) Mix acetic acid aqueous solution and chitosan, and stir at 300-400 rpm for 30-40 minutes to obtain chitosan solution; add chitosan solution to reaction vessel, and slowly add 2,3-epoxypropyltrimethylammonium chloride aqueous solution at 40-50℃ and 200-400 rpm for 30-60 minutes. Adjust the pH value to 8-9 with sodium hydroxide aqueous solution with a mass fraction of 9-11%, and continue stirring for 6-10 hours. Then precipitate the reaction solution in acetone, filter, wash 2-4 times with ethanol aqueous solution with a mass fraction of 70-80%, and finally vacuum dry at 50-60℃ for 8-12 hours to obtain chitosan quaternary ammonium salt. (3) Add deionized water to the reactor, add glycerol and fructooligosaccharide at 40-45℃ and 300-400rpm, then continue stirring for 10-20 minutes, then add chitosan quaternary ammonium salt, and continue stirring for 60-90 minutes to obtain the functional phase solution. (4) At 10-15℃ and a stirring speed of 300-400rpm, the functional phase solution is slowly added to the gel matrix solution over 30-60 minutes. Then, 85-90% lactic acid aqueous solution and 50-60% sodium lactate aqueous solution are added. Stirring is continued for 10-20 minutes. The pH value is then adjusted to 3.9-4.1 with 9-11% citric acid aqueous solution or 9-11% sodium hydroxide aqueous solution. The solution is stirred at 300-400rpm for 1-2 hours at 10-15℃ to obtain the feminine intimate care solution.

[0010] Furthermore, in step (1), the mass ratio of deionized water to poloxamer 407 powder is 100:18-22.

[0011] Furthermore, in step (3), the mass ratio of deionized water, glycerol, fructooligosaccharide and chitosan quaternary ammonium salt is 100:2-4:1-3:0.5-1.5.

[0012] Furthermore, in step (2), the mass ratio of acetic acid aqueous solution to chitosan is 100:2-4.

[0013] Furthermore, in step (2), the mass ratio of chitosan solution, 2,3-epoxypropyltrimethylammonium chloride aqueous solution and acetone is 100:40-60:350-450.

[0014] Furthermore, in step (4), the mass ratio of the functional phase solution, gel matrix solution, lactic acid aqueous solution and sodium lactate aqueous solution is 30-33:65-70:0.3-0.7:0.1-0.3.

[0015] Compared with the prior art, the beneficial effects achieved by the present invention are: 1. In this invention, the primary amino group of chitosan acts as a nucleophile, attacking the epoxy ring of 2,3-epoxypropyltrimethylammonium chloride to undergo a ring-opening reaction, grafting a positively charged trimethyl quaternary ammonium group onto the chitosan molecular chain to obtain a chitosan quaternary ammonium salt; glycerol serves to keep the mucous membrane moist, and fructooligosaccharides provide nutrients for beneficial bacteria; a buffer system composed of lactic acid and sodium lactate maintains the product's pH within a healthy weakly acidic range; when the product is at ambient temperature, due to the predominantly hydrophilic nature of poloxamer 407 molecules, it exhibits a readily flowing liquid state, facilitating handling and application; when the product comes into contact with the human body at temperatures exceeding poloxamer... At the phase transition temperature of 407, the hydrophobic segments of polyoxypropylene in poloxamer 407 molecules undergo dehydration. Intermolecular forces self-assemble through hydrophobic interactions to form a micelle network with hydrophobic segments as the core and hydrophilic segments as the shell. This transforms the product from a solution state to a semi-solid gel state, effectively retaining active ingredients such as chitosan quaternary ammonium salt and fructooligosaccharides at the site of action, potentially prolonging their local residence and action time. Chitosan quaternary ammonium salt binds to the negatively charged microbial cell membrane through electrostatic adsorption, interfering with membrane potential, disrupting the bilayer lipid structure and integrity of the cell membrane, leading to leakage of cell contents and thus inactivating the microorganisms. Detailed Implementation

[0016] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0017] A feminine hygiene wash, comprising a functional phase solution, a gel matrix solution, an aqueous lactic acid solution, and an aqueous sodium lactate solution; the functional phase solution is prepared by mixing deionized water, glycerin, fructooligosaccharides, and chitosan quaternary ammonium salt; the chitosan quaternary ammonium salt is prepared by mixing aqueous acetic acid solution, chitosan, and an aqueous 2,3-epoxypropyltrimethylammonium chloride solution; and the gel matrix solution is prepared by mixing deionized water and poloxamer 407 powder.

[0018] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0019] In the embodiments, the unit of rotational speed is revolutions per minute (rpm), and the unit of molecular weight is Dalton (Da).

[0020] Example 1

[0021] (1) Add deionized water to the reactor, and slowly add poloxamer 407 powder over 20 minutes at 10°C and 200 rpm. Then continue stirring for 4 hours, and then let it stand at 10°C for 10 hours to obtain a gel matrix solution. The mass ratio of deionized water to poloxamer 407 powder is 100:18.

[0022] (2) A 1% acetic acid aqueous solution and chitosan were mixed at a mass ratio of 100:2 and stirred at 300 rpm for 30 minutes to obtain a chitosan solution. The chitosan solution was added to a reaction vessel, and a 50% 2,3-epoxypropyltrimethylammonium chloride aqueous solution was slowly added over 30 minutes at 40°C and 200 rpm. The pH was adjusted to 8 with a 9% sodium hydroxide aqueous solution, and stirring was continued for 6 hours. The reaction solution was then precipitated in acetone, filtered, washed twice with a 70% ethanol aqueous solution, and finally vacuum dried at 50°C for 8 hours to obtain chitosan quaternary ammonium salt. The mass ratio of chitosan solution, 2,3-epoxypropyltrimethylammonium chloride aqueous solution and acetone was 100:40:350. The degree of deacetylation of chitosan was 85%, and the number average molecular weight was 100,000 Da.

[0023] (3) Add deionized water to the reactor, add glycerol and fructooligosaccharide at 40°C and 300 rpm, and continue stirring for 10 minutes. Then add chitosan quaternary ammonium salt and continue stirring for 60 minutes to obtain a functional phase solution. The mass ratio of deionized water, glycerol, fructooligosaccharide and chitosan quaternary ammonium salt is 100:2:1:0.5.

[0024] (4) Under a stirring speed of 300 rpm and 10°C, the functional phase solution was slowly added to the gel matrix solution over 30 minutes. Then, an 85% (w / w) lactic acid aqueous solution and a 50% (w / w) sodium lactate aqueous solution were added. The mixture was stirred for another 10 minutes. The pH was then adjusted to 3.9 with a 9% (w / w) citric acid aqueous solution or a 9% (w / w) sodium hydroxide aqueous solution. The mixture was stirred at 300 rpm for 1 hour at 10°C to obtain the feminine hygiene solution. The mass ratio of the functional phase solution, gel matrix solution, lactic acid aqueous solution, and sodium lactate aqueous solution was 30:65:0.3:0.1.

[0025] Example 2

[0026] (1) Add deionized water to the reactor, and slowly add poloxamer 407 powder over 25 minutes at a stirring speed of 250 rpm at 12°C. Then continue stirring for 5 hours and let it stand at 12°C for 11 hours to obtain a gel matrix solution. The mass ratio of deionized water to poloxamer 407 powder is 100:20.

[0027] (2) A 2% acetic acid aqueous solution and chitosan were mixed at a mass ratio of 100:3 and stirred at 350 rpm for 35 minutes to obtain a chitosan solution. The chitosan solution was added to a reaction vessel, and a 60% 2,3-epoxypropyltrimethylammonium chloride aqueous solution was slowly added over 45 minutes at 45°C and 300 rpm. The pH was adjusted to 8.5 with a 10% sodium hydroxide aqueous solution, and stirring was continued for 8 hours. The reaction solution was then precipitated in acetone, filtered, washed three times with a 75% ethanol aqueous solution, and finally vacuum dried at 55°C for 10 hours to obtain chitosan quaternary ammonium salt. The mass ratio of chitosan solution, 2,3-epoxypropyltrimethylammonium chloride aqueous solution and acetone was 100:50:400. The degree of deacetylation of chitosan was 90%, and the number average molecular weight was 150,000 Da.

[0028] (3) Add deionized water to the reactor, add glycerol and fructooligosaccharide at 42°C and 350 rpm, and continue stirring for 15 minutes. Then add chitosan quaternary ammonium salt and continue stirring for 75 minutes to obtain a functional phase solution. The mass ratio of deionized water, glycerol, fructooligosaccharide and chitosan quaternary ammonium salt is 100:3:2:1.

[0029] (4) Under a stirring speed of 350 rpm and 12°C, the functional phase solution was slowly added to the gel matrix solution over 45 minutes. Then, an 87% (w / w) lactic acid aqueous solution and a 55% (w / w) sodium lactate aqueous solution were added, and stirring was continued for 15 minutes. The pH value was then adjusted to 4.0 with a 10% (w / w) citric acid aqueous solution or a 10% (w / w) sodium hydroxide aqueous solution. The solution was stirred at 350 rpm for 1.5 hours at 12°C to obtain the feminine hygiene solution. The mass ratio of the functional phase solution, gel matrix solution, lactic acid aqueous solution, and sodium lactate aqueous solution was 31.5:67.5:0.5:0.2.

[0030] Example 3

[0031] (1) Add deionized water to the reactor, and slowly add poloxamer 407 powder over 30 minutes at 15°C and 300 rpm. Then continue stirring for 6 hours, and then let it stand at 15°C for 12 hours to obtain a gel matrix solution. The mass ratio of deionized water to poloxamer 407 powder is 100:22.

[0032] (2) A 3% acetic acid aqueous solution and chitosan were mixed at a mass ratio of 100:4 and stirred at 400 rpm for 40 minutes to obtain a chitosan solution. The chitosan solution was added to a reaction vessel, and a 70% 2,3-epoxypropyltrimethylammonium chloride aqueous solution was slowly added over 60 minutes at 50°C and 400 rpm. The pH was adjusted to 9 with an 11% sodium hydroxide aqueous solution, and stirring was continued for 10 hours. The reaction solution was then precipitated in acetone, filtered, washed four times with an 80% ethanol aqueous solution, and finally vacuum dried at 60°C for 12 hours to obtain chitosan quaternary ammonium salt. The mass ratio of chitosan solution, 2,3-epoxypropyltrimethylammonium chloride aqueous solution, and acetone was 100:60:450. The degree of deacetylation of chitosan was 95%, and the number average molecular weight was 200,000 Da.

[0033] (3) Add deionized water to the reactor, add glycerol and fructooligosaccharide at 45°C and 400 rpm, and continue stirring for 20 minutes. Then add chitosan quaternary ammonium salt and continue stirring for 90 minutes to obtain a functional phase solution. The mass ratio of deionized water, glycerol, fructooligosaccharide and chitosan quaternary ammonium salt is 100:4:3:1.5.

[0034] (4) Under stirring at 15℃ and 400 rpm, the functional phase solution was slowly added to the gel matrix solution over 60 minutes. Then, a 90% (w / w) lactic acid aqueous solution and a 60% (w / w) sodium lactate aqueous solution were added, and stirring was continued for 20 minutes. The pH was then adjusted to 4.1 with an 11% (w / w) citric acid aqueous solution or an 11% (w / w) sodium hydroxide aqueous solution. The solution was stirred at 400 rpm for 2 hours at 15℃ to obtain the feminine hygiene solution. The mass ratio of the functional phase solution, gel matrix solution, lactic acid aqueous solution, and sodium lactate aqueous solution was 33:70:0.7:0.3.

[0035] Comparative Example 1 The only difference between Comparative Example 1 and Example 1 is that the chitosan quaternary ammonium salt is omitted.

[0036] Comparative Example 2 The only difference between Comparative Example 2 and Example 1 is that poloxamer 407 powder was not added.

[0037] The physical state of the samples was observed at 25℃ and 37℃, respectively.

[0038] The inhibition rates against Candida albicans (ATCC10231), Escherichia coli (ATCC25922), and Staphylococcus aureus (ATCC6538) were tested according to the suspension quantitative method in the "Disinfection Technical Specifications" (2002 edition). The contact time was 30 minutes, and the results were repeated three times to calculate the average value. Table 1 below shows the performance analysis results of the embodiments and comparative examples of the present invention.

[0039] Table 1

[0040] Experimental data from the examples and comparative examples show that the present invention uses poloxamer 407 as a thermosensitive gel matrix. When it reaches body temperature, the hydrophobic polyoxypropylene segments in its molecules dehydrate and self-assemble to form a gel structure, thereby transforming the liquid product into a semi-solid gel that can adhere tightly to the mucous membrane, thus prolonging the action time of the active ingredients. Chitosan quaternary ammonium salt is used as an antibacterial agent. The quaternary ammonium cations on its molecular chain bind to the negatively charged microbial cell membrane through electrostatic adsorption, disrupting the integrity of its lipid bilayer and causing leakage of cell contents, thereby achieving a broad-spectrum antibacterial effect.

[0041] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A feminine intimate care fluid, characterized in that, The feminine intimate care solution is prepared from a functional phase solution, a gel matrix solution, an aqueous lactic acid solution, and an aqueous sodium lactate solution. The functional phase solution is prepared by mixing deionized water, glycerin, fructooligosaccharides, and chitosan quaternary ammonium salt. The chitosan quaternary ammonium salt is prepared by mixing aqueous acetic acid solution, chitosan, and an aqueous 2,3-epoxypropyltrimethylammonium chloride solution. The gel matrix solution is prepared by mixing deionized water and poloxamer 407 powder.

2. The feminine intimate care solution according to claim 1, characterized in that... Chitosan has a degree of deacetylation of 85-95% and a number-average molecular weight of 100,000-200,000 Da.

3. The feminine intimate care solution according to claim 1, characterized in that... The mass fraction of the aqueous solution of 2,3-epoxypropyltrimethylammonium chloride is 50-70%.

4. The feminine intimate care solution according to claim 1, characterized in that... The mass fraction of the acetic acid aqueous solution is 1-3%.

5. A method for preparing a feminine intimate care solution, applicable to the feminine intimate care solution according to any one of claims 1-4, characterized in that, Includes the following steps: (1) Add deionized water to the reactor, and slowly add poloxamer 407 powder over 20-30 minutes at a stirring speed of 200-300 rpm at 10-15℃. Then continue stirring for 4-6 hours, and then let it stand at 10-15℃ for 10-12 hours to obtain a gel matrix solution. (2) Mix acetic acid aqueous solution and chitosan, and stir at 300-400 rpm for 30-40 minutes to obtain chitosan solution; add chitosan solution to reaction vessel, and slowly add 2,3-epoxypropyltrimethylammonium chloride aqueous solution at 40-50℃ and 200-400 rpm for 30-60 minutes. Adjust the pH value to 8-9 with sodium hydroxide aqueous solution with a mass fraction of 9-11%, and continue stirring for 6-10 hours. Then precipitate the reaction solution in acetone, filter, wash 2-4 times with ethanol aqueous solution with a mass fraction of 70-80%, and finally vacuum dry at 50-60℃ for 8-12 hours to obtain chitosan quaternary ammonium salt. (3) Add deionized water to the reactor, add glycerol and fructooligosaccharide at 40-45℃ and 300-400rpm, then continue stirring for 10-20 minutes, then add chitosan quaternary ammonium salt, and continue stirring for 60-90 minutes to obtain the functional phase solution. (4) At 10-15℃ and a stirring speed of 300-400rpm, the functional phase solution is slowly added to the gel matrix solution over 30-60 minutes. Then, 85-90% lactic acid aqueous solution and 50-60% sodium lactate aqueous solution are added. Stirring is continued for 10-20 minutes. The pH value is then adjusted to 3.9-4.1 with 9-11% citric acid aqueous solution or 9-11% sodium hydroxide aqueous solution. The solution is stirred at 300-400rpm for 1-2 hours at 10-15℃ to obtain the feminine intimate care solution.

6. The method for preparing a feminine intimate care solution according to claim 5, characterized in that... In step (1), the mass ratio of deionized water to poloxamer 407 powder is 100:18-22.

7. The method for preparing a feminine intimate care solution according to claim 5, characterized in that... In step (3), the mass ratio of deionized water, glycerol, fructooligosaccharide and chitosan quaternary ammonium salt is 100:2-4:1-3:0.5-1.

5.

8. The method for preparing a feminine intimate care solution according to claim 5, characterized in that... In step (2), the mass ratio of acetic acid aqueous solution to chitosan is 100:2-4.

9. The method for preparing a feminine intimate care solution according to claim 5, characterized in that... In step (2), the mass ratio of chitosan solution, 2,3-epoxypropyltrimethylammonium chloride aqueous solution and acetone is 100:40-60:350-450.

10. A method for preparing a feminine intimate care solution according to claim 5, characterized in that... In step (4), the mass ratio of the functional phase solution, gel matrix solution, lactic acid aqueous solution and sodium lactate aqueous solution is 30-33:65-70:0.3-0.7:0.1-0.3.

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