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CN115645316A - Anti-hair loss shampoo containing rosemary - Google Patents

Anti-hair loss shampoo containing rosemary Download PDF

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Publication number
CN115645316A
CN115645316A CN202210793848.9A CN202210793848A CN115645316A CN 115645316 A CN115645316 A CN 115645316A CN 202210793848 A CN202210793848 A CN 202210793848A CN 115645316 A CN115645316 A CN 115645316A
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rosemary
chitosan
hair loss
shampoo
modified chitosan
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CN115645316B (en
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林俊达
卢绮华
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Full Core Biotechnology Macau Co ltd
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Full Core Biotechnology Macau Co ltd
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Abstract

The invention relates to an anti-hair loss shampoo containing rosemary. The anti-hair loss shampoo containing rosemary comprises raw materials such as cocamidopropyl betaine, sodium lauroyl-methyl aminopropionate, cocamidomethyl MEA (Mea-MEA), AOS (AOS), rosemary, modified chitosan 1, modified chitosan 2, functional additives and the like, wherein the modified chitosan 1 is prepared by reacting polyalcohol monomethyl ether with chitosan; the modified chitosan 2 is prepared by reacting amino acid with chitosan. Surprisingly, the components have good dispersing and compatibilization effects on additives of various natural components under a specific surfactant system, can effectively prevent the components from rapidly losing functions under a high-temperature environment, and have good anti-alopecia performance.

Description

Anti-hair loss shampoo containing rosemary
Technical Field
The invention relates to the technical field of daily chemical products, and particularly relates to rosemary-containing anti-hair loss shampoo.
Background
In modern society, many urban people, especially urban men, face the trouble of alopecia due to factors such as environmental pollution, huge working pressure, irregular life and the like. The direct causes of alopecia are endocrine disorders, genetic factors, or vascular disorders. In addition to medical conditioning, daily hair care is also a very important method of preventing hair loss.
In the prior art, for example, patents CN106214583A, CN107019789A, CN110179732A and the like report shampoo compositions for preventing hair loss and growing hair, but all of them bring unfavorable experience to consumers in terms of color, smell or irritation, so that there is a disadvantage. Daily chemical manufacturers and consumers prefer to replace artificially synthesized raw materials with natural functional components without side effects, so that the shampoo product has the effect of preventing alopecia.
Rosemary (Rosmarinus officinalis L.) belongs to Rosmarinus of Labiatae, and is known as Everfew, native to the coastal countries of Mediterranean sea, and is widely cultivated in all countries of the world, mainly produced in France, italy, spain, etc. Rosemary was first introduced abroad by the institute of Chinese academy of sciences and Beijing plantations in the end of 1981, and the plant cultivation test was successful. At present, seeds are widely cut in the south of China and are successful. The main chemical components of the composition comprise terpenes, flavonoids, organic acids, essential oils and the like.
Rosemary has strong oxidation resistance, is a natural substance, and has good safety. The antioxidant mechanism is caused by the effects of the components of rosmanol, carnosol and rosemary dialdehyde in the rosemary extract. Compared to other artificially prepared antioxidants, rosemary is a favored target for daily chemical manufacturers due to its strong antioxidant properties (reported to be about 5 times as potent as BHT and BHA), natural non-toxicity, and wide source.
Also, in the prior art, a shampoo product added with rosemary has a synergistic effect with other functional components, and has nourishing and cleaning effects on hair and scalp, so that the shampoo product has a certain anti-hair loss effect.
However, rosemary is a complex organic substance, and is liable to produce unknown reaction or change under a liquid environment coexisting with other organic components, such as amino acids, plant extracts and the like, for a long time; in addition, the shampoo is usually a composition with coexisting anionic and cationic surfactants, and the composition is a system easy to agglomerate; in addition, the shampoo is usually placed at a place close to a hot water source in a bathroom, and the preservation temperature is high, so that the stability of the shampoo containing rosemary faces a greater test.
Therefore, how to ensure that the shampoo containing rosemary still has the hair loss prevention and hair care functions in a long period of time in a high-temperature storage environment is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a shampoo containing rosemary aiming at the defects of the prior art. The shampoo containing rosemary is compounded with several kinds of amphoteric surfactants, anionic surfactants, cationic surfactants, polyquaternium-10 and several kinds of natural component additives. In addition, the invention compounds the poly-polyol monomethyl ether grafted chitosan and the amino acid grafted chitosan, and surprisingly discovers that the components have good dispersing and compatibilization effects on additives of various natural components under a specific surfactant system, can effectively prevent the components from quickly attenuating under a high-temperature environment, and have good anti-alopecia performance.
The invention provides rosemary-containing anti-hair loss shampoo which comprises the following components in parts by weight:
Figure BDA0003734838290000021
wherein,
the modified chitosan 1 is prepared by the reaction of poly-polyol monomethyl ether and chitosan;
the modified chitosan 2 is prepared by reacting amino acid with chitosan.
Further, the amino acid is selected from one or more of tryptophan, methionine, threonine, valine, lysine, histidine, leucine, isoleucine, alanine, phenylalanine, cystine, cysteine, arginine, glycine, serine, tyrosine, glutamic acid, aspartic acid, proline, hydroxyproline, citrulline and ornithine.
Further, the poly-polyol monomethyl ether is selected from one or more of poly-ethylene glycol monomethyl ether and polypropylene glycol monomethyl ether.
Further, the auxiliary agent comprises EDTA sodium salt, essence, a thickening agent, a dispersing agent, a pH regulator, citric acid, DMDM hydantoin and amino acid.
Further, the pH value of the anti-hair loss shampoo containing rosemary is 6.5-7.0.
Further, the thickening agent is selected from one or more of coconut oil fatty acid diethanolamide, coconut oil fatty acid monoethanolamide, sodium carboxymethylcellulose, sodium hydroxyethylcellulose, polyvinylpyrrolidone, acrylate copolymer, carbomer and sodium chloride.
Further, the preparation method of the modified chitosan 1 comprises the following steps:
s1, adding chitosan and polyatomic alcohol monomethyl ether into a solvent, then adding formaldehyde, and stirring for 10-20 hours to obtain a crude product;
and S2, dialyzing and freeze-drying the crude product, washing, filtering, and repeatedly dialyzing and freeze-drying to obtain the modified chitosan 1.
Further, the preparation method of the modified chitosan 2 comprises the following steps:
l1, adding amino acid into MES buffer solution containing a coupling agent and a condensing agent, and reacting to obtain an intermediate product;
and L2, adding the intermediate product into MES buffer solution containing chitosan, reacting, adjusting the pH value, and dialyzing to obtain the modified chitosan 2.
Further, the mass ratio of the chitosan to the poly-polyol monomethyl ether is 1 (1-6).
Further, the coupling agent is N-hydroxysuccinimide (NHS) and the condensing agent is 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC).
Compared with the prior art, the invention has the following beneficial effects:
1. in the anti-hair loss shampoo product containing rosemary, main components in the rosemary, such as terpenes, phenols and other natural extracts, are organic matters, have similar polarity with the modified chitosan 1 containing grafted long EO and PO chain segments, and have good compatibility; the modified chitosan 2 has better dispersibility and biocompatibility, and can promote the dissolution and dispersion of active ingredients such as amino acid and the like in the product; the modified chitosan 1 and the modified chitosan 2 are compounded, are mutually attracted and can load other effective components, so that agglomeration of anionic and cationic surfactant systems with opposite charges in the formula is effectively slowed down, and massive precipitates are formed, so that the condition of unstable appearance can not occur when the formula is placed in a bathroom environment at a higher temperature for a long time.
2. The surfactant system in the product, as well as the thickening agent contained in the adjuvant, has excellent suspending and thickening effects on rosemary and other natural extracts, mainly because the dispersing agent in the formula has longer branched chains, which promotes the degree of intertwining with the components of other formulas, so that the relative positions of the components in the system are not easy to change.
3. The surfactant and other components in the product have certain protection effect on functional components in the system, and the negative influence of part of external temperature change on the functional components is shielded, so that the shelf life of the product is prolonged.
Detailed Description
In order to more clearly illustrate the technical aspects of the present invention, the following examples are given, but the present invention is not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Rosemary in embodiments of the invention were purchased from a local market.
The surfactant in the embodiment of the invention is common raw materials in the market, and the essence adopts fruit-flavor essence produced by domestic chemical companies in certain countries.
The chitosan in the examples of the present invention is commercially available, and the degree of deacetylation is 85%.
The ginger extract and the sophora flavescens root extract in the embodiment of the invention are common raw materials sold in the market.
The Amino acid designation in the examples of the present invention is Amino acid liquid 607 produced by CM Bridge.
The preparation method of the modified chitosan 1 in the embodiment of the invention comprises the following steps:
s1, dissolving 0.25g of chitosan in 10mL of formic acid, then adding 1.5g of polyethylene glycol monomethyl ether, stirring for 15min, then adding 5mL of 37% formaldehyde, and stirring for 12h to obtain a crude product;
s2, adding the crude product into a dialysis bag, dialyzing with deionized water for 3d, freeze-drying, washing with chloroform, filtering, drying, dialyzing with deionized water for 3d again, and freeze-drying to obtain the modified chitosan 1.
The preparation method of the modified chitosan 2 in the embodiment of the invention comprises the following steps:
l1, adding methionine into an MES buffer solution containing NHS and EDC (with the MES concentration of 25mmol/L, the pH of 4.5 and the molar ratio of methionine, NHS and MES of 1;
and L2, adding the intermediate product into a MES buffer solution containing chitosan (with the MES concentration of 25mmol/L and the pH of 4.5, and the mass ratio of hydroxypropyl chitosan to methionine in the step S1 of 1), reacting for 24 hours, adding 25mg of hydroxylamine hydrochloride to terminate the reaction, adjusting the pH to 9 after the reaction, and then filling into a dialysis bag for dialysis for 48 hours to obtain the modified chitosan 2.
The components and the corresponding parts by mass of the anti-hair loss shampoo containing rosemary in the examples 1 to 3 are shown in table 1.
TABLE 1 ingredients and parts by weight in rosemary-containing hair loss reducing shampoo of examples 1-3
Figure BDA0003734838290000041
Figure BDA0003734838290000051
The preparation methods of the anti-hair loss shampoo containing rosemary in the embodiments 1 to 3 are as follows:
according to the mass parts, stirring and premixing a small amount of water, modified chitosan 1 and modified chitosan 2 with rosemary, ginger extract, sophora flavescens root extract, polyethylene glycol distearate, cocamidopropyl betaine, sodium lauroyl methyl aminopropionate, cocamidomethyl MEA and AOS in a reaction kettle at 30 ℃ for 30min; adding polyquaternium-10 and other residual components, adding water, and stirring for 30min to obtain the final product.
A comparative example thereof was set based on example 1. The ingredients of the comparative examples are shown in table 2.
TABLE 2 ingredients and parts by mass in the shampoo for preventing alopecia containing rosemary of example 1 and comparative examples 1 to 3
Figure BDA0003734838290000052
Figure BDA0003734838290000061
Comparative examples 1-3 were prepared in the same manner as in example 1 except that the specified ingredients in Table 1 were replaced with other ingredients.
Test example section
Test example 1 stability test
The test method comprises the following steps:
the anti-hair loss shampoos containing rosemary prepared in examples 1-3 and comparative examples 1-3 were tested for stability by the following specific test methods:
200g of each of the samples of examples 1 to 3 and comparative examples 1 to 3 was taken, and filled in a transparent PE bottle, and then placed in an oven at 40 ℃ for 120 hours, and then the appearance change of the sample was visually evaluated.
The results are shown in Table 3.
TABLE 3 high temperature stability test of examples 1-3, comparative examples 1-3
Figure BDA0003734838290000062
From the stability test in table 3, it can be seen that the stability of examples 1-3 is significantly better than that of comparative example 1, which indicates that the effect of stabilizing and dispersing functional components is more ideal and superior to that of general chitosan by compounding two modified chitosan components as an auxiliary agent; in comparative examples 2 to 3, due to the use of the single modified chitosan, a synergistic effect of promoting stabilization and compatibilization cannot be formed, and the protective performance of the modified chitosan on functional components is lower than that of examples 1 to 3.
Test example 2
The above samples were tested for anti-hair loss effect. The tests were divided into two groups, the first being the test for the anti-alopecia effect of the newly prepared product, and the second being the test for the anti-alopecia effect of the product after being placed in an oven at 40 ℃ for two weeks.
The test method comprises the following steps: 40 socially recruited volunteers, males between the ages of 35-45, were selected to have symptoms of seborrheic or physiological alopecia. All volunteers did not undergo any other treatment for targeted alopecia within 1 month and voluntarily tried the product on time and quantity.
40 volunteers are divided into two groups, wherein each group comprises 20 volunteers, fixed volunteers are arranged in each group, and specific products are tried out respectively. The volunteers of the first large group used each newly prepared product separately; the second large group of volunteers used the same respective products after two weeks in an oven at 40℃ for 56 days each (as the first large group of volunteers A themselves, who only tried the product of example 1 for 56 days) and then during the trial, the hair was combed three times a day, morning, evening and the shed hair was collected. The total number of hair loss for each person was recorded over the three day period 54-56 days, and the number of hair loss was recorded for each of the three days. The statistical results obtained are shown in Table 4 as the results of the alopecia preventing effect.
Table 4 test results of alopecia prevention effects of the anti-alopecia shampoos containing rosemary of examples 1 to 3 and comparative examples 1 to 3
Figure BDA0003734838290000071
As can be seen from Table 4, the alopecia preventing effects of the newly prepared samples of examples 1 to 3 and comparative examples 1 to 3 were all at the same level, and the number of alopecia was about 110 to 125 per person. After long-term storage at high temperature, the anti-falling effects of the first and second groups show obvious difference: after the embodiment 1-3 is stored at high temperature, the anti-hair-loss effect is still remarkable, and the hair loss number is only increased in a small range in the same time period; in the comparative example, the number of hair loss is greatly increased, particularly in the comparative example 1, because no dispersible component is added in the comparative example 1, the functions of rosemary, extract and the like are easily degraded; the formulation systems in comparative examples 2 and 3 also have poor stability, which causes obvious decline of the functions of rosemary, the extract and the like.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (10)

1. The anti-hair loss shampoo containing rosemary is characterized by comprising the following components in parts by weight:
Figure FDA0003734838280000011
auxiliary agent
Water;
wherein,
the modified chitosan 1 is prepared by reacting polyol monomethyl ether with chitosan;
the modified chitosan 2 is prepared by reacting amino acid with chitosan.
2. The rosemary-containing anti-hair loss shampoo according to claim 1, wherein the amino acid is selected from one or more of tryptophan, methionine, threonine, valine, lysine, histidine, leucine, isoleucine, alanine, phenylalanine, cystine, cysteine, arginine, glycine, serine, tyrosine, glutamic acid, aspartic acid, proline, hydroxyproline, citrulline and ornithine.
3. The rosemary-containing anti-hair loss shampoo according to claim 1, wherein the poly-polyol monomethyl ether is selected from one or more of poly-ethylene glycol monomethyl ether and poly-propylene glycol monomethyl ether.
4. The rosemary-containing anti-hair loss shampoo according to claim 1, wherein the auxiliaries comprise sodium EDTA, essence, a thickening agent, a dispersing agent, a pH regulator, citric acid, DMDM hydantoin and amino acid.
5. The shampoo for preventing hair loss containing rosemary according to claim 1, wherein the pH of the shampoo for preventing hair loss containing rosemary is 6.5 to 7.0.
6. Rosemary-containing anti-alopecia shampoo according to claim 4, wherein the thickening agent is selected from one or more of coconut oil fatty acid diethanolamide, coconut oil fatty acid monoethanolamide, sodium carboxymethylcellulose, sodium hydroxyethylcellulose, polyvinylpyrrolidone, acrylate copolymers, carbomer, and sodium chloride.
7. The rosemary-containing anti-alopecia shampoo as claimed in claim 1, wherein the preparation method of the modified chitosan 1 comprises the following steps of:
s1, adding chitosan and polyatomic alcohol monomethyl ether into a solvent, then adding formaldehyde, and stirring for 10-20 hours to obtain a crude product;
and S2, dialyzing and freeze-drying the crude product, washing, filtering, and repeatedly dialyzing and freeze-drying to obtain the modified chitosan 1.
8. The rosemary-containing anti-hair loss shampoo as claimed in claim 1, wherein the preparation method of the modified chitosan 2 comprises the following steps:
l1, adding amino acid into MES buffer solution containing a coupling agent and a condensing agent, and reacting to obtain an intermediate product;
and L2, adding the intermediate product into MES buffer solution containing chitosan, reacting, adjusting the pH value, and dialyzing to obtain the modified chitosan 2.
9. The rosemary-containing anti-hair loss shampoo as claimed in claim 7, wherein the mass ratio of the chitosan to the poly-polyol monomethyl ether is 1 (1-8).
10. The rosemary-containing anti-alopecia shampoo as in claim 8, wherein the coupling agent is N-hydroxysuccinimide and the condensing agent is 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride.
CN202210793848.9A 2022-07-07 2022-07-07 Anti-hair loss shampoo containing rosemary Active CN115645316B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118978687A (en) * 2024-08-05 2024-11-19 广州飞思合成材料有限公司 A preparation method of a modified mercaptan curing agent and its application in epoxy resin

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150021271A (en) * 2013-08-20 2015-03-02 을지대학교 산학협력단 Ppg-chitosan hydrogel mask sheet comprising esculin and method for preparing the same
KR102192004B1 (en) * 2019-06-24 2020-12-16 김영지 Shampoo composition for preventing hair loss and improving state of hair
CN112206188A (en) * 2020-09-23 2021-01-12 禹州森茂迷迭香生物科技有限公司 Rosemary anti-hair loss shampoo and preparation method thereof
CN114376940A (en) * 2022-02-21 2022-04-22 佛山奕安赛医药科技有限公司 Amino acid ice crystal shower gel and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150021271A (en) * 2013-08-20 2015-03-02 을지대학교 산학협력단 Ppg-chitosan hydrogel mask sheet comprising esculin and method for preparing the same
KR102192004B1 (en) * 2019-06-24 2020-12-16 김영지 Shampoo composition for preventing hair loss and improving state of hair
CN112206188A (en) * 2020-09-23 2021-01-12 禹州森茂迷迭香生物科技有限公司 Rosemary anti-hair loss shampoo and preparation method thereof
CN114376940A (en) * 2022-02-21 2022-04-22 佛山奕安赛医药科技有限公司 Amino acid ice crystal shower gel and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118978687A (en) * 2024-08-05 2024-11-19 广州飞思合成材料有限公司 A preparation method of a modified mercaptan curing agent and its application in epoxy resin
CN118978687B (en) * 2024-08-05 2025-04-01 广州飞思合成材料有限公司 A preparation method of modified mercaptan curing agent and its application in epoxy resin

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