CN113332191A

CN113332191A - Shampoo and preparation method thereof

Info

Publication number: CN113332191A
Application number: CN202110497819.3A
Authority: CN
Inventors: 吴知情; 万岳鹏; 胡根华; 龚盛昭; 胡兴国
Original assignee: Guangzhou Huanya Cosmetic Science and Technology Co Ltd
Current assignee: Guangzhou Huanya Cosmetic Science and Technology Co Ltd
Priority date: 2017-12-08
Filing date: 2017-12-08
Publication date: 2021-09-03
Also published as: CN107802551A

Abstract

The invention provides shampoo and a preparation method thereof, wherein the shampoo comprises the following components in percentage by mass: 10-40% of potassium cocoyl hydrolyzed oat protein, 1-10% of disodium cocoyl glutamate, 0.1-2.0% of conditioner, 0.1-1.0% of pH regulator, 0.1-0.4% of preservative synergist and the balance of deionized water. The shampoo disclosed by the invention is prepared by reasonably compounding the potassium cocoyl hydrolyzed oat protein, the disodium cocoyl glutamate and a conditioner and then adding a proper amount of an antiseptic synergist, and is a silicone oil-free shampoo which is mild in property and does not contain an antiseptic.

Description

Shampoo and preparation method thereof

The application is a divisional application with the application date of 2017, 12 months and 08 days, the application number of 201711291798.X and the name of the invention of 'shampoo and a preparation method thereof'.

Technical Field

The invention belongs to the field of daily cosmetics, relates to shampoo and a preparation method thereof, and particularly relates to silicone oil-free shampoo and a preparation method thereof.

Background

In recent years, with the improvement of living standard of people, the demand of consumers for hair care is higher, and green, healthy and natural hair care products are favored by consumers. At present, silicone oil-free washing and protecting products gradually become mainstream consumer products, but most silicone oil-free washing and protecting products only simply remove silicone oil, the formula is not reasonable, and the market demand cannot be really met.

CN 105796421A discloses a silicone oil-free balance repair shampoo, which comprises the main active components and the mass parts of 20-28 parts of surfactant, 100.2-0.4 part of polyquaternium, 0.2-0.4 part of cationic guar gum, 1-3 parts of ethylene glycol distearate and 0.3-0.8 part of di (hydrogenated tallow) p-benzene dicarboxamide, the shampoo has mild formula, does not contain silicone oil, and can remove dandruff and relieve itching, but the sulfate surfactant adopted by the shampoo has certain irritation and toxicity.

CN 106265378A discloses silicone oil-free shampoo with scalp care effect, which comprises the following components in percentage by mass: 5-20 parts of surfactant, 0.1-0.5 part of cationic conditioner, 1-8 parts of humectant, 1-3 parts of moisturizing conditioner, 0.1-0.2 part of anti-dandruff agent, 2-5 parts of pure natural vegetable oil and 0.1-5 parts of scalp care agent, the shampoo adopts camellia oil compounded with star anise oil to replace silicone oil, and simultaneously adopts the combination of the surfactant and the scalp care agent, so that the shampoo has scalp care effect, but the star anise oil adopted by the shampoo can cause burden on scalp.

Therefore, the shampoo with mild properties and no burden on the scalp is a problem to be solved urgently.

Disclosure of Invention

Aiming at the defects of the prior art, the shampoo provided by the invention is a silicone oil-free shampoo which is mild in property and does not contain preservatives, and is prepared by reasonably compounding potassium oat cocoyl hydrolysate, disodium cocoyl glutamate and a conditioner and then adding a proper amount of an antiseptic synergist.

In order to achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the invention provides shampoo, which comprises the following components in percentage by mass:

according to the invention, two amino acid type surfactants, namely potassium cocoyl hydrolyzed oat protein and disodium cocoyl glutamate, are used as main surfactants, so that the wet combing, washing and dry combing effects of hair can be obviously improved, and compared with the traditional fatty alcohol sulfate surfactant, the amino acid surfactant has the advantages of large surface tension, strong wettability, strong permeability, rich and fine foam, low irritation, low toxicity, strong softness, strong antibacterial property, good decontamination capability, excellent corrosion inhibition, biodegradability and the like; according to the invention, the coconut acyl hydrolyzed oat protein potassium and the coconut acyl disodium glutamate are reasonably compounded with the conditioner, and then the preservative synergist is added, so that the prepared shampoo is mild in property, free of preservative, low in irritation and free of silicone oil, and the moisture retention and the soothing degree of the scalp after use are obviously improved.

Preferably, the content of the potassium cocoyl hydrolyzed oat protein in the shampoo is 10-40% by mass, for example, 10%, 12%, 15%, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38% or 40%, preferably 20-30%, and more preferably 30%.

Preferably, the content of the cocoyl glutamic acid disodium in the shampoo is 1-10% by mass, for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%, preferably 8-10%, and more preferably 10%.

Preferably, the conditioner is 0.1 to 2.0% by mass in the shampoo, and may be, for example, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.25%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2.0%, preferably 0.9 to 1.6%, and more preferably 1.25%.

Preferably, the pH adjuster is 0.1 to 1.0% by mass in the shampoo, and may be, for example, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.55%, 0.6%, 0.7%, 0.8%, 0.9%, or 1.0%, preferably 0.55%.

Preferably, the preservative synergist is 0.1-0.4% by mass in the shampoo, for example, 0.1%, 0.2%, 0.3% or 0.4%, preferably 0.4%.

Preferably, the conditioning agent comprises any one of or a combination of at least two of polyquaternium-10, sorbitan caprylate or hydrolyzed corn starch, preferably a combination of polyquaternium-10, sorbitan caprylate and hydrolyzed corn starch.

Preferably, the pH adjusting agent is a citric acid-sodium citrate buffer.

Preferably, the preservative synergist comprises any one or a combination of at least two of glyceryl caprylate, glyceryl laurate or olive leaf extract, preferably the combination of glyceryl caprylate, glyceryl laurate and olive leaf extract.

The traditional shampoo usually adopts methylchloroisothiazolinone, methylisothiazolinone or DMDM hydantoin as a preservative, has high irritation, is easy to cause allergic symptoms, and is not beneficial to scalp care. According to the invention, the preservative synergist consisting of the glyceryl caprylate, the glyceryl laurate and the olive leaf extract is adopted to act synergistically with the sorbitan caprylate, so that the antibacterial spectrum of the system is widened, the preservative property of the system is improved, the secondary pollution resistance effect is achieved, and the irritation of the shampoo to the scalp is effectively reduced while the preservative property of the shampoo is ensured.

The shampoo also comprises cocoamide methyl MEA and/or essence.

Preferably, the cocoamide methyl MEA is present in the shampoo in a mass percentage of 0.5-0.8%, for example 0.5%, 0.6%, 0.7% or 0.8%.

Preferably, the mass percentage of the essence in the shampoo is 0.2%.

Preferably, the shampoo comprises the following components in percentage by mass:

in a second aspect, the present invention provides a method for preparing a shampoo according to the first aspect, comprising the following steps:

(1) adding the potassium cocoyl hydrolyzed oat protein, the disodium cocoyl glutamate, the conditioner, the anticorrosion synergist and the deionized water into an emulsifying pot according to a formula proportion, heating, stirring and mixing uniformly;

(2) and (3) after cooling, adding a pH regulator into the emulsifying pot to regulate the pH value of the mixture, and performing vacuum defoaming to obtain the shampoo.

Preferably, the temperature of the addition in step (1) is 70-90 ℃, for example 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃, preferably 80 ℃.

Preferably, the temperature for reducing the temperature in the step (2) is 37-40 ℃, for example, 37 ℃, 38 ℃, 39 ℃ or 40 ℃.

Preferably, the pH of the mixture of step (2) is 5.0 to 7.0, and may be, for example, 5.0, 5.68, 6.0 or 7.0, preferably 5.68.

As a preferred technical solution, the present invention provides a method for preparing a shampoo according to the first aspect, including the following steps:

(1) adding the potassium cocoyl hydrolyzed oat protein, the disodium cocoyl glutamate, the conditioner, the preservative synergist and the deionized water into an emulsifying pot according to the formula proportion, heating to 70-90 ℃, and stirring and mixing uniformly;

(2) and cooling to 37-40 ℃, adding a pH regulator into the emulsifying pot to regulate the pH value of the mixture to 5.0-7.0, and performing vacuum defoaming to obtain the shampoo.

Compared with the prior art, the invention has the following beneficial effects:

(1) the shampoo disclosed by the invention adopts two amino acid type surfactants, namely potassium oat protein hydrolysate and disodium cocoyl glutamate, as main surfactants, so that the shampoo is rich and fine in foam, mild in property, and lower in possibility of causing skin irritation reaction by being reasonably compounded with a conditioner;

(2) the shampoo disclosed by the invention adopts a green and safe preservative synergist, has a remarkable inhibition effect on bacteria and fungi under the synergistic effect with sorbitan caprylate, and effectively reduces the stimulation of the shampoo on the scalp while ensuring the preservative property of the shampoo;

(3) the shampoo disclosed by the invention has the advantages of strong scalp moisturizing capability and good scalp soothing performance, and does not cause dandruff and itching.

Detailed Description

To further illustrate the technical means and effects of the present invention, the present invention is further described with reference to the following examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention.

The specific techniques or conditions not specified in the examples of the present invention are performed according to the techniques or conditions described in the literature in the art or according to the product specification. The reagents or apparatus used are conventional products commercially available from normal sources, not indicated by the manufacturer.

In the invention, the pH value is measured according to the method specified in the national standard GB/T13531.1-2008, and the foaming power is measured according to the national standard GB/T13173-2008 by using a Roche foamer. Experimental methods without specifying specific conditions, according to conventional conditions or manufacturers

Example 1

The formulation of the shampoo is shown in table 1.

TABLE 1

The preparation method comprises the following steps:

(1) adding cocoyl hydrolyzed oat protein potassium, cocoyl disodium glutamate, polyquaternium-10, sorbitan caprylate, hydrolyzed corn starch, glyceryl caprylate, glyceryl laurate, olive leaf extract, cocoamide methyl MEA (methyl MEA), essence and deionized water into an emulsifying pot according to a formula proportion, heating to 80 ℃, and stirring and mixing uniformly;

(2) and cooling to 40 ℃, adding citric acid and sodium citrate into the emulsifying pot to adjust the pH value of the mixture to 5.68, and performing vacuum defoaming to obtain the shampoo.

Example 2

The formulation of the shampoo is shown in table 2.

TABLE 2

The preparation method comprises the following steps:

Example 3

The formulation of the shampoo is shown in table 3.

TABLE 3

The preparation method comprises the following steps:

Example 4

The formulation of the shampoo is shown in table 4.

TABLE 4

The preparation method comprises the following steps:

(1) adding cocoyl hydrolyzed oat protein potassium, cocoyl disodium glutamate, polyquaternium-10, sorbitan caprylate, hydrolyzed corn starch, glyceryl caprylate, glyceryl laurate, olive leaf extract, cocoamide methyl MEA (methyl MEA), essence and deionized water into an emulsifying pot according to a formula proportion, heating to 90 ℃, and stirring and mixing uniformly;

(2) and cooling to 40 ℃, adding citric acid and sodium citrate into the emulsifying pot to adjust the pH value of the mixture to 5.0, and defoaming in vacuum to obtain the shampoo.

Comparative example 1

Compared to example 1, the formulation and preparation conditions were the same as in example 1 except that potassium cocoyl oat protein was not included.

Comparative example 2

The formulation and preparation conditions were the same as in example 1, except that disodium cocoyl glutamate was not included, as compared to example 1.

Comparative example 3

Compared to example 1, the formulation and preparation conditions were the same as in example 1 except that no conditioning agent was included.

Comparative example 4

Compared with the example 1, the conditioner has the mass percentage of 2.5 percent, and other formulas and preparation conditions are the same as those of the example 1.

Comparative example 5

Compared to example 1, the formulation and preparation conditions were the same as in example 1 except that sorbitan octanoate was not contained.

Comparative example 6

Compared with example 1, the other formulation and preparation conditions are the same as example 1 except that the preservative synergist is not contained.

Experiment of corrosion prevention challenge

The test was conducted with reference to the American society for Cosmetic and Toiletries (CTFA) standards for preservation challenge testing. Preservative challenge experiments required 99.9% reduction in bacterial content and 90% reduction in fungal content at day 7, and continued reduction in bacterial content over days 14, 21 and 28 (N.I ═ no increase), with specific criteria as shown in table 5.

TABLE 5 Corrosion protection challenge criteria

The results of the preservation challenge experiments are shown in tables 6-7.

TABLE 6 bacterial challenge experiments

TABLE 7 fungal challenge experiments

Therefore, the preservative synergist in the shampoo in the embodiments 1 to 4 is reasonably compounded with sorbitan caprylate, and through a challenge experiment, the bacterial content is reduced by 99.999% and the fungal content is reduced by 99.99% at the 7 th day, and the bacterial content is continuously reduced within 14, 21 and 28 days, so that the preservative synergist has a good preservative effect; compared with the shampoo of the example 1, the shampoo of the comparative example 3 and the shampoo of the comparative example 5 do not contain sorbitan caprylate, the conditioner in the shampoo of the comparative example 4 is unreasonable in mass percentage, so that the preservative synergist and the sorbitan caprylate cannot play a good synergistic effect, the shampoo of the comparative example 6 does not contain the preservative synergist, the bacteriostatic effect of the shampoo of the comparative examples 3 to 6 is not ideal, and the preservative challenge cannot be passed. Therefore, the preservative synergist and the sorbitan caprylate have a synergistic effect, and the preservative synergist plays a crucial role in the overall preservative effect.

Haemolysis test of erythrocytes

The erythrocyte hemolysis test is an alternative method of the rabbit eye stimulation test (Draize test), and the basic principle is to evaluate the damage of chemicals to eye tissue cells by measuring the amount of dissolved hemoglobin and the degree of denaturation. The irritation of cosmetics and raw materials thereof to eyes is evaluated internationally mainly through erythrocyte hemolysis experiments.

In the present invention, the ratio L/D of 2 variables (L50/DI) was obtained by calculating the weight concentration of the test substance (HC50, mg/L) at 410nm which causes hemolysis of 50% erythrocytes and the denaturation rate (DI) of hemoglobin at 575nm and 540 nm. Three commercially available shampoos which are ten times of the domestic shampoo sale market in nearly 5 years are selected in the experiment, and the main surface active agents of the three shampoos are sodium laureth sulfate.

The results are shown in Table 8.

TABLE 8 foam height and L/D ratio

Experimental data show that the shampoo prepared in the embodiment 1-4 can obviously reduce the irritation of the formula by compounding the cocoyl hydrolyzed oat protein potassium and the cocoyl disodium glutamate and performing synergistic action with a conditioner; comparative examples 1-2 used a single potassium cocoyl hydrolyzed oat protein or disodium cocoyl glutamate, and the conditioner formulations of comparative examples 3-4 were not reasonable and had slightly higher irritancy; the three commercially available shampoos use sodium laureth sulfate as a primary surfactant, and have high irritation.

Patch test

Safety evaluation tests were performed using example 1, comparative examples 1 to 2, and a commercially available shampoo. 30 volunteers aged 22-40 years were selected, a spot test tape containing 0.02mL of sample was applied to normal skin on the back of the volunteer, the spot tester was removed after 24 hours, and the patch was removed and examined according to CTFA guidelines (1981) within a second half hour. The identification criteria are shown in Table 9 and the results are shown in Table 10.

TABLE 9 identification standards

Grade	(symbol)	Identification criteria
			0	﹣	Negative reaction: no irritation and erythema
1	±	And (3) suspicious reaction: mild erythema
			2	﹢	Weak positive reaction: erythema
3	﹢﹢	Strong positive reaction: erythema, papules, blisters
			4	﹢﹢﹢	Very positive reaction: serious edema and cannon

TABLE 10 Patch test results

The results show that 1 suspicious reaction appears in the shampoo of the example 1, 5 suspicious reactions appear in the shampoo of the comparative example 1, 3 suspicious reactions appear in the shampoo of the comparative example 2, and 6 suspicious reactions appear in the shampoo sold in market. According to the regulations of the cosmetic hygiene code (2015 edition), it can be judged that none of example 1, comparative examples 1-2 and commercially available shampoos caused adverse reactions on the skin of the subjects of the batch. However, statistically, it can be seen that the shampoo of example 1 is less likely to cause skin irritation, and the shampoo of example 1 is milder in nature.

Population test evaluation

The use mildness evaluation test was performed using example 1, comparative examples 1 to 2, and a commercially available shampoo. And selecting 50 volunteers to perform half-head comparison test, wherein the period is 28 days, and effect return visits are performed every 2 weeks. The scalp moisture retention and scalp soothing degree are respectively graded, the questionnaire is filled according to the use feeling, the grading standard is 1 point without effect, 2 points with effect and weak, 3 points with effect and obvious effect, 4 points with effect and good effect, and 5 points with effect and good effect. The score of more than or equal to 3 is judged as obvious effect, the total number of people with the score of more than or equal to 3 is counted, the number of people causing dandruff and head itching is counted, and the investigation result is shown in a table 11.

TABLE 11 shampoo sensory test evaluation

The results show that the shampoo in the embodiment 1 is prepared by compounding potassium cocoyl hydrolyzed oat protein and disodium cocoyl glutamate, and is superior to single potassium cocoyl hydrolyzed oat protein and disodium cocoyl glutamate in terms of scalp moisture retention and scalp soothing; after 28 days of using the shampoo of comparative examples 1-2, 2 volunteers showed dandruff and itching; the shampoo sold in the market is weaker than the shampoo of the invention in terms of scalp moisture retention and scalp soothing, and 5 subjects showed dandruff and itching after using the shampoo for 28 days.

In conclusion, the shampoo provided by the invention adopts two amino acid type surfactants, namely potassium oat protein hydrolysate and disodium cocoyl glutamate, as the main surfactants, is reasonably compounded with the conditioner, and is supplemented with the preservative synergist, so that the prepared shampoo is rich and fine in foam, mild in property, strong in scalp moisturizing capability, good in scalp soothing performance, and free of dandruff and itching.

The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims

1. The shampoo is characterized by comprising the following components in percentage by mass:

the balance of deionized water;

the conditioner is a combination of polyquaternium-10, sorbitan caprylate and hydrolyzed corn starch;

the preservative synergist is a combination of glyceryl caprylate, glyceryl laurate and olive leaf extract.

2. The shampoo of claim 1, wherein the pH adjuster is a citric acid-sodium citrate buffer.

3. Shampoo according to claim 1, characterized in that it further comprises cocamide methyl MEA and/or perfume.

4. The shampoo according to claim 3, characterized by comprising the following components in percentage by mass:

the balance being deionized water.

5. The shampoo according to claim 4, wherein the shampoo comprises the following components in percentage by mass:

the balance being deionized water.

6. The shampoo according to claim 5, wherein the shampoo comprises the following components in percentage by mass:

7. a process for preparing a shampoo as defined in claim 1 or claim 2, comprising the steps of:

8. The method of claim 7, wherein the temperature of the addition in step (1) is 70-90 ℃.

9. The method of claim 7, wherein the temperature of the temperature reduction in step (2) is 37-40 ℃.

10. The method of claim 7, wherein the pH of the mixture of step (2) is 5.0-7.0.