Preparation method of shampoo capable of responding to release functional components in weak acid environment
Through microsphere wrapping and pH stimulation response technology, the problem that the effective ingredients in existing shampoos cannot be released accurately is solved, and the stable storage and precise release of the effective ingredients are achieved, which improves the effect of the shampoo and the utilization rate of the active ingredients.
Patent Information
- Application Number
- CN202411405723.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-10
- Publication Date
- 2025-03-04
AI Technical Summary
Existing shampoos cannot accurately release the effective ingredients under specific conditions, resulting in poor efficacy and the active ingredients are prone to inactivate and difficult to preserve.
Microsphere wrapping and pH stimulation response technology are used to adjust the pH value of shampoo through phosphate buffered water and pH regulators, so that it accurately releases the effective ingredients in a weak acid environment.
It achieves stable storage and precise release of active ingredients, extends the validity period of shampoo, and improves the utilization rate of active ingredients.
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Figure CN119548435A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of shampoo, and in particular to a method for preparing a shampoo capable of releasing functional ingredients in response to a weakly acidic environment. Background Art
[0002] Due to the high pressure of today's pace of life, the human body's immunity is reduced, the probability of infection with Malassezia increases, and the problems of oily dandruff emerge in an endless stream, seriously affecting people's lives. At present, the common functional shampoos for oily dandruff on the market mainly include ketoconazole, selenium disulfide and Chinese medicine shampoos. Among them, ketoconazole shampoos can only be used in small amounts because they contain hormones, and are prone to drug resistance. Selenium disulfide shampoos have a bad smell and are less accepted. In Chinese medicine shampoos, because they contain more active substances, there are problems such as easy inactivation of effective ingredients and difficulty in preservation. And the above shampoos cannot achieve the effect of precise release of effective ingredients under specific conditions, affecting the efficacy of the shampoo.
[0003] Therefore, solving the problem of oily dandruff cannot be underestimated. Solving the problem of oily dandruff from the root and ensuring that the effective ingredients are not inactivated during storage and are accurately released during use are issues that the present invention urgently needs to solve. Summary of the invention
[0004] In order to solve the problems existing in the above-mentioned background technology, the present invention provides a method for preparing a shampoo that releases functional ingredients in response to a weak acid environment. The method utilizes microsphere encapsulation and pH stimulation response technology to effectively solve the problems of unstable functional ingredients being easily inactivated and difficult to preserve, and allows the functional ingredients to be accurately released under specific conditions to exert their effects, which can not only reduce the dosage of active functional ingredients, but also improve the utilization rate of active ingredients.
[0005] In order to achieve the above technical objectives, the present invention mainly adopts the following technical solutions:
[0006] The invention discloses a shampoo for releasing effective ingredients in response to a weak acid environment. The shampoo comprises the following raw materials in parts by weight: 0.2-0.3 parts of chlorogenic acid, 3-4 parts of polyvinyl alcohol, 100-150 parts of phosphate buffered water, 20-40 parts of Tween 80, 1-2 parts of methyl parahydroxybenzoate solution, 10 parts of N-[3-(dimethylamino)propyl]octadecylamide, 30-40 parts of citric acid solution, 500-600 parts of sodium hydroxide solution, 1-2 parts of lemon juice, 80-100 parts of gelatin solution and 0.1-0.2 parts of rose essential oil.
[0007] In a preferred embodiment of the present invention, the pH of the phosphate buffered water is 4.7, the mass fraction of the methyl parahydroxybenzoate solution is 0.05%, the mass fraction of the citric acid solution is 1%, the concentration of the sodium hydroxide solution is 1 mol / L, and the mass fraction of the gelatin solution is 10%.
[0008] The present invention also discloses a method for preparing the shampoo that releases functional ingredients in response to a weak acid environment, comprising the following steps:
[0009] Step 1, preparing chlorogenic acid-containing microspheres;
[0010] Step 2, preparing pH responsive hydrogel;
[0011] Step 3: Prepare a shampoo that releases effective ingredients in response to a weak acid environment.
[0012] In a preferred embodiment of the present invention, in step 1, the method for preparing chlorogenic acid microspheres is:
[0013] Step 1.1, preparing an internal aqueous phase: dissolving chlorogenic acid in a polyvinyl alcohol solution and a phosphate buffer to obtain an internal aqueous phase W1;
[0014] Step 1.2, preparing a primary emulsion: pouring lW1 into a polyvinyl alcohol solution, emulsifying, and obtaining a primary emulsion W1 / O;
[0015] Step 1.3, preparing double emulsion W1 / O / W2: adding the primary emulsion W1 / O dropwise to a polyvinyl alcohol solution containing a surfactant Tween 80, emulsifying, and obtaining double emulsion W1 / O / W2;
[0016] Step 1.4, preparing chlorogenic acid-containing microspheres: stirring the double emulsion W1 / O / W2, centrifuging, and washing to obtain chlorogenic acid-containing microspheres.
[0017] In a preferred embodiment of the present invention, in step 1.1, the mass fraction of the polyvinyl alcohol solution is 1%, in step 1.2, the mass fraction of the polyvinyl alcohol solution is 0.3%, and in step 1.3, the mass fraction of the polyvinyl alcohol solution is 2%.
[0018] In a preferred embodiment of the present invention, in step 1.2 and step 1.3, emulsification is performed at 24,000 rpm using a Helldorf VR homogenizer; in step 1.4, the stirring time is 3 hours, centrifuged at 9,000 rpm for 15 minutes, and washed with distilled water.
[0019] In a preferred embodiment of the present invention, in step 2, the method for preparing the pH responsive hydrogel is:
[0020] Step 2.1: Add N-[3-(dimethylamino)propyl]octadecylamide to deionized water and dissolve under heating conditions to obtain an aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide;
[0021] Step 2.2: Add citric acid to the aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide, and then adjust the pH value of the system to pH=7 with a sodium hydroxide solution to obtain a gel system;
[0022] Step 2.3: Add the chlorogenic acid-containing microspheres to the prepared gel system, and freeze-dry the mixture and grind it into powder to obtain a pH-responsive hydrogel.
[0023] Preferably, in step 2.1, the heating condition is 70° C.; in step 2.2, the molar ratio of N-[3-(dimethylamino)propyl]octadecylamide to citric acid is 3:1; in step 2.3, the powder is sieved through a 200-mesh sieve.
[0024] In a preferred embodiment of the present invention, in step 3, the method for preparing a shampoo that releases functional ingredients in response to a weakly acidic environment is:
[0025] The freeze-dried powder of the pH-responsive hydrogel was added to a portion of the gelatin solution, and the mixture was shaken and mixed. Lemon juice and methyl paraben were added under stirring, followed by citric acid solution and rose essential oil, and finally the gelatin solution was added until the final solution volume was 100 ml to obtain shampoo.
[0026] Compared with the prior art, the present invention has the following beneficial effects:
[0027] The preparation method of the shampoo for releasing functional ingredients in response to a weak acid environment provided by the present invention can provide a stable environment for the functional ingredients: the microsphere encapsulation technology used in the preparation process of the shampoo can provide a stable environment for the unstable and easily inactivated functional ingredients, so that the functional ingredients can remain active and stable, and the shelf life of the shampoo can be extended; the functional ingredients can be accurately released when used;
[0028] The shampoo adopts pH stimulation response technology in the preparation process, so that when the shampoo contacts the weak acid environment of the human scalp, it can accurately release the active ingredients through acid response and exert its effect, which can not only reduce the amount of active ingredients used, but also improve the utilization rate of active ingredients;
[0029] The design concept of the present invention can not only be used for the precise release of chlorogenic acid, but can also be used for the design and application of other similar ingredients. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 A flow chart of a method for preparing a shampoo that releases functional ingredients in response to a weak acid environment provided by an embodiment of the present invention;
[0031] Figure 2 The diagram is a reaction mechanism diagram of the shampoo of the present invention that releases effective ingredients in response to a weak acid environment. DETAILED DESCRIPTION
[0032] The following will combine the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are 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] In the present invention:
[0034] The polyvinyl alcohol solution with a mass fraction of 1% is prepared by dissolving 1 part by weight of polyvinyl alcohol in 100 parts by weight of water;
[0035] The polyvinyl alcohol solution with a mass fraction of 0.3% is prepared by dissolving 0.3 parts by weight of polyvinyl alcohol in 100 parts by weight of water;
[0036] The polyvinyl alcohol solution with a mass fraction of 2% is prepared by dissolving 2 parts by weight of polyvinyl alcohol in 100 parts by weight of water.
[0037] Example 1
[0038] A shampoo that releases functional ingredients in response to a weak acid environment is made from the following raw material ratios:
[0039] 0.2 parts of chlorogenic acid, 3.3 parts of polyvinyl alcohol, 100 parts of phosphate buffered water with a pH of 4.7, 20 parts of Tween 80, 1 part of 0.05% methyl p-hydroxybenzoate solution, 10 parts of N-[3-(dimethylamino)propyl]octadecylamide, 40 parts of citric acid solution, 500 parts of 1 mol / L sodium hydroxide solution, 1 part of lemon juice, 80 parts of 10% gelatin solution, and 0.1 part of rose essential oil.
[0040] A method for preparing a shampoo that releases functional ingredients in response to a weak acid environment comprises the following steps:
[0041] (1) dissolving chlorogenic acid (CGA) in a 1% by mass polyvinyl alcohol (PVA) solution and phosphate buffered water (pH = 4.7) to obtain an internal aqueous phase W1;
[0042] (2) Pour lW1 into a 0.3% polyvinyl alcohol (PVA) solution and emulsify it with a Helldorf VR homogenizer at 24000 rpm to obtain a primary emulsion W1 / O;
[0043] (3) adding the primary emulsion (W1 / O) dropwise into a 2% W / V polyvinyl alcohol (PVA) solution containing a surfactant Tween 80, and emulsifying the solution at 24,000 rpm using a Heildorf VR homogenizer to obtain a double emulsion (W1 / O / W2);
[0044] (4) The double emulsion (W1 / O / W2) was stirred at 7000 rpm for 3 h (to evaporate the organic solvent and tighten the microspheres), and the mixture was centrifuged at 9000 rpm for 15 min. After centrifugation, it was washed with distilled water to obtain microspheres containing chlorogenic acid;
[0045] (5) adding N-[3-(dimethylamino)propyl]octadecylamide (NDPO) to 90 parts of deionized water and dissolving the mixture at 70° C. to obtain an aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO);
[0046] (6) adding citric acid (CA) to the aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO) according to the molar ratio of organic carboxylic acid to N-[3-(dimethylamino)propyl]octadecylamide (NDPO) (1:3);
[0047] (7) adjusting the pH value of the solution system to pH=7 with a 1 mol / L sodium hydroxide (NaOH) solution to obtain a gel system;
[0048] (8) adding the chlorogenic acid-containing microspheres prepared in step (4) to the prepared gel system, freeze-drying the mixture and grinding it into a 200 mesh powder;
[0049] (9) adding the lyophilized powder prepared in step (8) to the 10% gelatin solution and shaking for 20 minutes to mix;
[0050] (10) Add lemon juice and methyl paraben while stirring;
[0051] (11) adding sufficient 1% citric acid solution to adjust the pH value of the solution;
[0052] (12) Add rose essential oil to adjust the smell;
[0053] (13) Finally, gelatin solution was added to a final solution volume of 100 ml to obtain shampoo.
[0054] Example 2
[0055] A shampoo that releases functional ingredients in response to a weak acid environment is made from the following raw material ratios:
[0056] 0.3 parts of chlorogenic acid, 3.3 parts of polyvinyl alcohol, 100 parts of phosphate buffered water with a pH of 4.7, 20 parts of Tween 80, 1 part of 0.05% methyl p-hydroxybenzoate solution, 10 parts of N-[3-(dimethylamino)propyl]octadecylamide, 40 parts of citric acid solution, 500 parts of 1 mol / L sodium hydroxide solution, 1 part of lemon juice, 80 parts of 10% gelatin solution, and 0.1 part of rose essential oil.
[0057] A method for preparing a shampoo that releases functional ingredients in response to a weak acid environment comprises the following steps:
[0058] (1) dissolving chlorogenic acid (CGA) in a 1% by mass polyvinyl alcohol (PVA) solution and phosphate buffered water (pH = 4.7) to obtain an internal aqueous phase W1;
[0059] (2) Pour lW1 into a 0.3% polyvinyl alcohol (PVA) solution and emulsify it with a Helldorf VR homogenizer at 24000 rpm to obtain a primary emulsion W1 / O;
[0060] (3) adding the primary emulsion (W1 / O) dropwise into a 2% W / V polyvinyl alcohol (PVA) solution containing a surfactant Tween 80, and emulsifying the solution at 24,000 rpm using a Heildorf VR homogenizer to obtain a double emulsion (W1 / O / W2);
[0061] (4) The double emulsion (W1 / O / W2) was stirred at 7000 rpm for 3 h (to evaporate the organic solvent and tighten the microspheres), and the mixture was centrifuged at 9000 rpm for 15 min. After centrifugation, it was washed with distilled water to obtain microspheres containing chlorogenic acid;
[0062] (5) adding N-[3-(dimethylamino)propyl]octadecylamide (NDPO) to 90 parts of deionized water and dissolving the mixture at 70° C. to obtain an aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO);
[0063] (6) adding citric acid (CA) to the aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO) according to the molar ratio of organic carboxylic acid to N-[3-(dimethylamino)propyl]octadecylamide (NDPO) (1:3);
[0064] (7) adjusting the pH value of the solution system to pH=7 with a 1 mol / L sodium hydroxide (NaOH) solution to obtain a gel system;
[0065] (8) adding the chlorogenic acid-containing microspheres prepared in step (4) to the prepared gel system, freeze-drying the mixture and grinding it into a 200 mesh powder;
[0066] (9) adding the lyophilized powder prepared in step (8) to the 10% gelatin solution and shaking for 20 minutes to mix;
[0067] (10) Add lemon juice and methyl paraben while stirring;
[0068] (11) adding sufficient 1% citric acid solution to adjust the pH value of the solution;
[0069] (12) Add rose essential oil to adjust the smell;
[0070] (13) Finally, gelatin solution was added to a final solution volume of 100 ml to obtain shampoo.
[0071] Example 3
[0072] A shampoo that releases functional ingredients in response to a weak acid environment is made from the following raw material ratios:
[0073] 0.3 parts of chlorogenic acid, 3.3 parts of polyvinyl alcohol, 150 parts of phosphate buffered water with a pH of 4.7, 40 parts of Tween 80, 2 parts of 0.05% methyl p-hydroxybenzoate solution, 10 parts of N-[3-(dimethylamino)propyl]octadecylamide, 40 parts of citric acid solution, 600 parts of 1 mol / L sodium hydroxide solution, 22 parts of lemon juice, 80 parts of 10% gelatin solution, and 0.2 parts of rose essential oil.
[0074] A method for preparing a shampoo that releases functional ingredients in response to a weak acid environment comprises the following steps:
[0075] (1) dissolving chlorogenic acid (CGA) in a 1% by mass polyvinyl alcohol (PVA) solution and phosphate buffered water (pH = 4.7) to obtain an internal aqueous phase W1;
[0076] (2) Pour lW1 into a 0.3% polyvinyl alcohol (PVA) solution and emulsify it with a Helldorf VR homogenizer at 24000 rpm to obtain a primary emulsion W1 / O;
[0077] (3) adding the primary emulsion (W1 / O) dropwise into a 2% W / V polyvinyl alcohol (PVA) solution containing a surfactant Tween 80, and emulsifying the solution at 24,000 rpm using a Heildorf VR homogenizer to obtain a double emulsion (W1 / O / W2);
[0078] (4) The double emulsion (W1 / O / W2) was stirred at 7000 rpm for 3 h (to evaporate the organic solvent and tighten the microspheres), and the mixture was centrifuged at 9000 rpm for 15 min. After centrifugation, it was washed with distilled water to obtain microspheres containing chlorogenic acid;
[0079] (5) adding N-[3-(dimethylamino)propyl]octadecylamide (NDPO) to 90 parts of deionized water and dissolving the mixture at 70° C. to obtain an aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO);
[0080] (6) adding citric acid (CA) to the aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide (NDPO) according to the molar ratio of organic carboxylic acid to N-[3-(dimethylamino)propyl]octadecylamide (NDPO) (1:3);
[0081] (7) adjusting the pH value of the solution system to pH=7 with a 1 mol / L sodium hydroxide (NaOH) solution to obtain a gel system;
[0082] (8) adding the chlorogenic acid-containing microspheres prepared in step (4) to the prepared gel system, freeze-drying the mixture and grinding it into a 200 mesh powder;
[0083] (9) adding the lyophilized powder prepared in step (8) to the 10% gelatin solution and shaking for 20 minutes to mix;
[0084] (10) Add lemon juice and methyl paraben while stirring;
[0085] (11) adding sufficient 1% citric acid solution to adjust the pH value of the solution;
[0086] (12) Add rose essential oil to adjust the smell;
[0087] (13) Finally, gelatin solution was added to a final solution volume of 100 ml to obtain shampoo.
Claims
1. A shampoo that releases functional ingredients in response to a weak acid environment, characterized in that: The invention comprises the following raw materials in parts by weight: 0.2-0.3 parts of chlorogenic acid, 3-4 parts of polyvinyl alcohol, 100-150 parts of phosphate buffered water, 20-40 parts of Tween 80, 1-2 parts of methyl parahydroxybenzoate solution, 10 parts of N-[3-(dimethylamino)propyl]octadecylamide, 30-40 parts of citric acid solution, 500-600 parts of sodium hydroxide solution, 1-2 parts of lemon juice, 80-100 parts of gelatin solution and 0.1-0.2 parts of rose essential oil.
2. The shampoo for releasing functional ingredients in response to weak acid environment according to claim 1, characterized in that: The pH value of the phosphate buffered water is 4.7, the mass fraction of the methyl parahydroxybenzoate solution is 0.05%, the mass fraction of the citric acid solution is 1%, the concentration of the sodium hydroxide solution is 1 mol / L, and the mass fraction of the gelatin solution is 10%.
3. A method for preparing the shampoo that releases functional ingredients in response to a weak acid environment as claimed in claim 1, characterized in that: The steps include: Step 1, preparing chlorogenic acid-containing microspheres; Step 2, preparing pH responsive hydrogel; Step 3: prepare a shampoo that releases effective ingredients in response to a weak acid environment.
4. The preparation method according to claim 3, characterized in that: In step 1, the method for preparing chlorogenic acid microspheres is: Step 1.1, preparing an internal aqueous phase: dissolving chlorogenic acid in a polyvinyl alcohol solution and a phosphate buffer to obtain an internal aqueous phase W1; Step 1.2, preparing a primary emulsion: pouring lW1 into a polyvinyl alcohol solution, emulsifying, and obtaining a primary emulsion W1 / O; Step 1.3, preparing double emulsion W1 / O / W2: adding the primary emulsion W1 / O dropwise to a polyvinyl alcohol solution containing a surfactant Tween 80, emulsifying, and obtaining double emulsion W1 / O / W2; Step 1.4, preparing chlorogenic acid-containing microspheres: stirring the double emulsion W1 / O / W2, centrifuging, and washing to obtain chlorogenic acid-containing microspheres.
5. The preparation method according to claim 4, characterized in that: In step 1.1, the mass fraction of the polyvinyl alcohol solution is 1%, in step 1.2, the mass fraction of the polyvinyl alcohol solution is 0.3%, and in step 1.3, the mass fraction of the polyvinyl alcohol solution is 2%.
6. The preparation method according to claim 4, characterized in that: In step 1.2 and step 1.3, emulsification was performed using a Helldorf VR homogenizer at 24,000 rpm; in step 1.4, the stirring time was 3 hours, the mixture was centrifuged at 9,000 rpm for 15 minutes, and washed with distilled water.
7. The preparation method according to claim 3, characterized in that: In step 2, the method for preparing the pH responsive hydrogel is: Step 2.1: Add N-[3-(dimethylamino)propyl]octadecylamide to deionized water and dissolve under heating conditions to obtain an aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide; Step 2.2: Add citric acid to the aqueous solution of N-[3-(dimethylamino)propyl]octadecylamide, and then adjust the pH value of the system to pH=7 with a sodium hydroxide solution to obtain a gel system; Step 2.3: Add the chlorogenic acid-containing microspheres to the prepared gel system, and freeze-dry the mixture and grind it into powder to obtain a pH-responsive hydrogel.
8. The preparation method according to claim 7, characterized in that: In step 2.1, the heating condition is 70° C.; in step 2.2, the molar ratio of N-[3-(dimethylamino)propyl]octadecylamide to citric acid is 3:1; in step 2.3, the powder is sieved through a 200-mesh sieve.
9. The preparation method according to claim 3, characterized in that: In step 3, the method for preparing a shampoo that releases functional ingredients in response to a weak acid environment is: The freeze-dried powder of the pH-responsive hydrogel was added to a portion of the gelatin solution, and the mixture was shaken and mixed. Lemon juice and methyl paraben were added under stirring, followed by citric acid solution and rose essential oil, and finally the gelatin solution was added until the final solution volume was 100 ml to obtain shampoo.