WO2020073368A1

WO2020073368A1 - Formulation and process for preparing body wash employing xinhui tangerine peels and blossom extract

Info

Publication number: WO2020073368A1
Application number: PCT/CN2018/112392
Authority: WO
Inventors: 温伟成
Original assignee: 温伟成
Priority date: 2018-10-10
Filing date: 2018-10-29
Publication date: 2020-04-16
Also published as: CN108938505A

Abstract

Disclosed are a formulation and a process for preparing a body wash employing Xinhui tangerine peels and flower extracts. The formulation comprises the following ingredients, in mass percentage: 5-10% of sodium laureth sulfate, 1-5% of lauryl ammonium sulfate, 0.2-0.5% of polyquaternium-7, 0.1-0.3% of PEG-120 methyl glucose dioleate, 0.1% of methyl paraben, 0.1-0.4% of polyoxyethylene sorbitan tristearate, 2-7% of cocamidopropyl betaine, 1-6% of coconut oil fatty acid diethanolamide, 0.5-1% of Xinhui tangerine peel extract, 0.5-1% of Xinhui tangerine blossom extract, 1-5% of glycerin, 0.1-0.5% of chitosan, and 0.1-0.2% of disodium EDTA, the balance being water. Xinhui tangerine peel and flower extracts, used in combination with other moisturizing ingredients, offer a mild and non-irritating body wash that can accelerate self-renewal and repair of skin cells, having the effects of repairing and moisturizing the skin while also cleaning the skin.

Description

Formula and process for preparing shower gel of Xinhui citrus peel and citrus flower extract

Technical field

The invention belongs to the technical field of cosmetics, and particularly relates to a formula and a process for preparing shower gel of Xinhui citrus peel and citrus flower extract.

Background technique

There are various factors for skin damage, including external physical factors, genetic factors, biological factors, health factors, iatrogenic factors and so on. For example, excessive ultraviolet radiation can damage the skin and make the skin age and become rough; too cold, too hot, and excessive mechanical irritation will cause damage to the skin. As the environment deteriorates, people's skin and even the physiological functions of young girls' skin are easily damaged.

Xinhui mandarin, also known as Xinhui Guangchen mandarin or tangerine peel mandarin, is a famous local product in Xinhui District, Jiangmen City, Guangdong Province, and is a Chinese geographical indication product. Xinhui mandarin has both skin and meat, and has the same origin as medicine and food. It is an excellent variety selected from the big red mandarin of Rutaceae citrus in the long cultivation history of Guangchen orange farmers. Its unique quality, popular in the Ming and Qing Dynasties, and was classified as a "tribute", tribute every year.

Citrus peel is the most important by-product that remains after citrus fruit processing. It contains nutrients other than amino acids, and the rest are higher than the pulp. Especially rich in certain functional ingredients, such as flavonoids, limonoids, carotenoids , Phenolic acid, pectin and dietary fiber. These substances have many physiological activities such as anti-cancer, anti-oxidation, bacteriostasis, etc., and have important health care effects on human health. Among them, the content of flavonoids in citrus peel is particularly rich, and its content is much higher than that of fruit juice.

At present, the shower gels on the market are mainly used to clean the body's skin such as sweat and dirt. People expect to be able to develop a shower gel with repair and moisturizing function, which can repair damaged skin and moisturize the whole body skin while cleansing the skin. For such products, the market is currently blank.

Summary of the invention

The purpose of the present invention is to provide a formula and process for making shower gel of Xinhui citrus peel and citrus flower extract. It uses Xinhui citrus peel and xinhui citrus flower extract in combination with other moisturizing and moisturizing ingredients. Accelerate the self-renewal and repair of skin cells. While cleaning the skin, it can also play a role in skin repair and moisturizing.

To achieve its purpose, the present invention adopts the following technical solutions:

A formula of Xinhui citrus peel and citrus flower extract for making shower gel, which contains the following components in mass percentage:

Sodium laureth sulfate 5-10%, ammonium lauryl sulfate 1-5%, polyquaternium-7 0.2-0.5%, PEG-120 methyl glucose dioleate 0.1-0.3%, hydroxybenzene Methyl ester 0.1% ～ 0.3%, polyoxyethylene sorbitan tristearate 0.1 ～ 0.4%, cocamidopropyl betaine 2 ～ 7%, coconut oil fatty acid diethanolamide 1 ～ 6%, Xinhui Citrus peel extract 0.5-1%, Xinhui citrus flower extract 0.5-1%, glycerin 1-5%, chitosan 0.1-0.5%, disodium EDTA 0.1-0.2%, water balance.

The above-mentioned Xinhui citrus peel and citrus flower extracts are used to prepare a shower gel, which contains the following components in mass percentage:

Sodium laureth sulfate 7-9%, ammonium lauryl sulfate 2-3%, polyquaternium-7 0.2-0.3%, PEG-120 methyl glucose dioleate 0.1-0.3%, hydroxybenzene Methyl ester 0.1% ～ 0.3%, Polyoxyethylene sorbitan tristearate 0.3 ～ 0.4%, Cocamidopropyl betaine 2 ～ 5%, Coconut oil fatty acid diethanolamide 5 ～ 6%, New Huigan peel extract 0.8-1%, Xinhui citrus flower extract 0.8-1%, glycerin 3-5%, chitosan 0.3-0.5%, disodium EDTA 0.1-0.2%, water balance.

The above-mentioned Xinhui citrus peel and citrus flower extract are used to prepare a shower gel. The preparation method of the Xinhui citrus flower extract is:

1) Take fresh Xinhui citrus flowers, dry at 50-60 ° C with hot air, grind them into powder, and pass through a 10-100 mesh sieve;

2) Carry out carbon dioxide supercritical extraction of the powder obtained in step 1), the extraction temperature is 40-60 ℃, the extraction pressure is 200-500 BAR, wherein, according to the material-liquid ratio g / mL is 1: (0.5-2), add 95% Ethanol, static extraction 20-30min, then add 95% ethanol at 0.2-0.6mL / min, dynamic extraction 1-3h;

3) The liquid obtained in step 2) is concentrated under reduced pressure to obtain the Xinhui citrus flower extract.

The above-mentioned Xinhui citrus peel and citrus flower extract are used to prepare a shower gel. The Xinhui citrus peel extract uses carbon dioxide supercritical extraction technology.

The above-mentioned Xinhui citrus peel and citrus flower extract are used to make a shower gel. The preparation method of the Xinhui citrus peel extract is:

1) Cut the fresh Xinhui citrus peel into thin strips, dry it at 50-60 ° C with hot air, grind it into powder, and sieve;

2) Add an entrainer and perform supercritical CO2 extraction of the Xinhui citrus peel powder prepared in step 1). The extraction temperature is 40-60 ° C, the extraction pressure is 200-500 BAR, and the extraction time is 1-3h. After pressure concentration, the Xinhui orange peel extract is obtained.

Further, in step 2), the entraining agent is 70% ethanol, 95% ethanol, absolute ethanol, or methanol; preferably, the entraining agent is methanol.

When selecting the entrainer, choose 70% ethanol, 95% ethanol and absolute ethanol. Since the polarity of methanol in organic solvents is greater than ethanol, and the boiling point of methanol is lower than that of absolute ethanol. Therefore, the choice of methanol may be more conducive to the extraction and separation of flavonoids.

Further, in step 2), the entraining agent is added at a feed liquid ratio of g / mL of 1: (0.5-2), static extraction is performed for 20 minutes, and then the entraining agent is added at 0.2-0.6 mL / min. Extraction for 2h; preferably, the entrainer is added according to a material-liquid ratio of 1: 1, static extraction is performed for 20min, and then the entrainer is added at 0.4mL / min, and dynamic extraction is performed for 2h.

In dynamic extraction, when the amount of entrainer added is about 0.4mL / min, the extraction rate is the highest. With the increase of the amount of entrainer, it is conducive to the dissolution of flavonoids in citrus peel and the extraction rate is increased; however, when the amount is too large, the contact time of flavonoids in citrus peel with entrainer becomes shorter, resulting The use efficiency of the entraining agent is reduced. In dynamic extraction, the longer the time, the higher the extraction rate of flavonoids. But after 120min, the total flavonoid leaching amount is very small, because under normal circumstances, if the extraction time is too short, the supercritical carbon dioxide fluid does not reach good contact with the solute, the extraction amount is small; The compound gradually approaches the equilibrium of dissolution, and then the extraction time is increased. The extraction yield is limited to increase, and with the extension of time, the energy consumption of supercritical extraction also increases.

In addition, the invention also provides a process for preparing a shower gel of the Xinhui citrus peel and citrus flower extract, which includes the following steps:

1) Weigh the raw materials of each component, put deionized water in a jacket heating barrel and heat up to 50 ～ 60 ℃;

2) Emulsification: Put the raw materials of Group A into a stirring pot in sequence, heat to 80 ° C, stirring speed 30 rpm / min until the raw materials are completely dissolved; the raw materials of Group A include: water, sodium laureth sulfate, lauryl Ammonium sulfate, polyquaternium-7, PEG-120 methyl glucose dioleate, methylparaben, polyoxyethylene sorbitan tristearate;

3) Insulation: Insulation for 20 minutes, vacuuming 0.05mmHg to defoam;

4) Cooling: stirring speed 35 rpm and cooling to 50 ℃;

5) Feeding: add Group B raw materials and mix evenly (agitating speed 30 rpm), cool to 40 ° C, add Group C raw materials, and mix evenly for 10 minutes; the Group B raw materials include: cocamidopropyl betaine 2 ～ 7%, coconut oil fatty acid diethanolamide; the Group C raw materials include: Xinhui orange peel extract, Xinhui orange flower extract, glycerin, chitosan, disodium EDTA;

6) Discharging: Discharging at a temperature of 40 ° C; a small amount of pH adjuster (citric acid) can be added to control the pH value at 5.5-7.0, and a small amount of sodium chloride can be added to adjust the viscosity.

With the above technical solutions, the present invention has the following advantages and beneficial technical effects:

1. In the specific formula system provided by the present invention, the three components of glycerin, chitosan, Xinhui citrus peel and citrus flower extract are combined in a specific ratio, and are combined with other specific components in the formula to obtain The body wash not only has a good skin cleansing effect, but also greatly reduces the irritation of the surfactant on the skin in the formula system, can promote the repair of the skin surface lipid film, and help restore the normal physiological function of the skin.

2. The present invention uses a combination of Xinhui citrus peel and citrus flower extract and other moisturizing ingredients. It contains a variety of anti-aging and moisturizing ingredients. The active ingredients in it can inhibit the generation of free radicals and accelerate the removal of free radicals; The active ingredients are combined in a certain proportion, which can synergistically reduce skin free radicals. It has a gentle effect and no irritation. It can accelerate the self-renewal and repair of skin cells. It has significant anti-aging and moisturizing effects. It can quickly improve skin texture, increase skin elasticity and smoothness. wrinkle.

3. The present invention utilizes a combination of glycerin, chitosan, Xinhui citrus peel and citrus flower extract to repair damaged skin from three aspects of promoting skin regeneration, activating immune function and reducing external irritation, so that the skin can quickly recover to a healthy state.

detailed description

The present invention will be further described in detail below in conjunction with specific preferred embodiments. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not intended to limit the present invention.

Among them, the carbon dioxide supercritical extraction technology is used to extract the peel of Xinhui citrus. The total flavonoid content of the extract is greater than 10%. Lactobacillus acidophilus and E. coli have different degrees of inhibition and can be used as a natural antibacterial active substance;

Xinhui citrus flower extract is rich in flavonoids, flavonoids have significant physiological activity, flavonoids have good antioxidant activity, can reduce the harm of free radicals to varying degrees. A large number of studies have shown that the flavonoids SOD and GSH-Px not only remove the active oxidized free radicals in the body and prevent the biofilm lipids from being oxidized by superoxide and hydroxyl radicals, but also have a similar effect to vitamin E.

Glycerin has a high moisturizing effect. Chitosan has good antibacterial activity and can inhibit the growth and reproduction of some fungi, bacteria, and viruses. It is believed that there are three possible mechanisms: one is due to the polycation of chitosan, which is susceptible to the action of negatively charged groups on the surface of fungal cells, thereby changing the fluidity and permeability of pathogenic cell membranes; ; The third is to block the metabolism of pathogenic bacteria. Chitosan has good hygroscopic and moisturizing effects. It can form a thin protective film on the skin surface, which slows down the evaporation of skin moisture and protects the skin from external irritation.

All kinds of test instruments and reagents are commercially available products, all of which can be purchased through commercial channels.

Preparation of raw materials:

Preparation of Huigan peel extract: Cut the fresh Xinhui orange peel into thin strips, dry at 55 ° C with hot air, grind it into a powder, and sieve; take out 100g of dry powder and add 100mL of methanol, at an extraction temperature of 50 ° C, the extraction pressure is Under the conditions of 300 BAR, static extraction was performed for 20 minutes, then methanol was added at 0.4 mL / min, dynamic extraction was performed for 2 hours, and after concentration under reduced pressure, 22.2 g of Xinhui citrus peel extract was obtained.

Preparation of Xinhui citrus flower extract: take 100g fresh Xinhui citrus flower, dry at 55 ℃ with hot air, grind it into powder and pass through a 40 mesh sieve; subject the obtained powder to supercritical carbon dioxide extraction with an extraction temperature of 55 ℃ and extraction pressure It is 300BAR, in which, 95% ethanol is added according to the material-liquid ratio g / mL 1: 1, static extraction is performed for 25min, then 95% ethanol is added at 0.4mL / min, and dynamic extraction is performed for 2h; the resulting liquid is concentrated under reduced pressure , That is, Xinhui Orange Flower Extract.

The percentages in the following examples are all weight percentages.

Examples 1-4

The formulation of the Xinhui citrus peel and citrus flower extract of Example 1-4 to prepare a shower gel, which contains the following components in the following mass percentages, is shown in Table 1 below:

Table 1 Formulation components (%) of the Xinhui citrus peel and citrus flower extract of Example 1-4 for making shower gel

The preparation process of Examples 1-4 is as follows.

A process for making shower gel of Xinhui citrus peel and citrus flower extract is prepared as follows:

3) Insulation: Insulation for 20 minutes, vacuuming 0.05mmHg to defoam;

4) Cooling: stirring speed 35 rpm and cooling to 50 ℃;

Comparative Example 1

A shower gel product, prepared as follows:

3) Insulation: Insulation for 20 minutes, vacuuming 0.05mmHg to defoam;

4) Cooling: stirring speed 35 rpm and cooling to 50 ℃;

5) Feeding: add Group B raw materials and mix well (agitating speed 30 rpm), after cooling to 40 ° C; the Group B raw materials include: cocamidopropyl betaine 2-7 percent, coconut oil fatty acid diethanolamide ;

Effect Test Example 1

Test article: shower gels prepared in Examples 1 to 4 and Comparative Example 1 of the present invention and a commercially available moisturizing shower gel.

Subject population: The subjects had healthy skin and no history of skin allergies, which met the volunteer's voluntary inclusion criteria. A total of 35 people were divided into 7 groups on average, with 4 women and 3 men in each group.

Test method: Draw a test area on the inner side of the volunteer's right hand forearm at 4 square centimeters. Use a skin moisture tester to test the moisture content of the skin before washing and the moisture content of the skin after washing for 2 hours to calculate the increase in moisture content. percentage. The results are shown in Table 2.

Table 2 Examples 1 to 4 and Comparative Example 1 and comparison of shower gel test of commercially available products

A	实施例1Example 1	实施例2Example 2	实施例3Example 3	实施例4Example 4	对比例1Comparative Example 1	市售品Commercial products
洗前皮肤含水量Skin moisture before washing	30.43％30.43%	30.07％30.07%	30.66％30.66%	30.50％30.50%	30.25％30.25%	30.56％30.56%
洗后皮肤含水量Skin moisture after washing	35.84％35.84%	35.97％35.97%	35.16％35.16%	35.37％35.37%	31.21％31.21%	33.62％33.62%
含水量增加(％)Increased water content (%)	17.78％17.78%	19.62％19.62%	14.68％14.68%	15.97％15.97%	3.17％3.17%	10.01％10.01%

* Compared with commercially available products and Comparative Example 1, p <0.05.

Effect Test Example 2

The test was conducted with reference to the literature method (Human Skin Patch Test 2007, Cosmetic Hygiene Specification).

Test substance: The samples obtained in Examples 1 to 5 obtained in the preparation examples.

Participants: A total of 26 people, half male and female, aged 20 to 30 years old, in line with the subject's voluntary selection criteria.

Test method: Put the test substance into the spot tester, the dosage is 0.021g. The control well is a blank control (without any substance). Place the spot tester with the test substance on the back of the subject or the curved side of the forearm with non-stimulating tape, and gently press it with the palm of the hand to evenly apply it to the skin for 3 minutes. 30 minutes after removing the spot tester, observe the skin reaction after the indentation disappears. If the result is negative, observe again 24h and 48h after the patch test. Record the results of the reactions in accordance with Table 3 (Standard Table for Classification of Adverse Skin Reactions).

Table 3 Classification Standard Table of Adverse Skin Reactions

The test results are shown in Table 4:

Table 4 Evaluation results after removing the test substance

A	--	±±	++	++++	++++++
实施例1Example 1	26人26 people	00	00	00	00
实施例2Example 2	26人26 people	00	00	00	00
实施例3Example 3	26人26 people	00	00	00	00
实施例4Example 4	26人26 people	00	00	00	00
实施例5Example 5	26人26 people	00	00	00	00

The results of re-observation 24 hours and 48 hours after the patch test are the same as in Table 4. The above results show that the shower gel prepared by the Xinhui citrus peel and citrus flower extract of the present invention has no irritating effect on human skin. Volunteers prefer the formula shower gel of Example 1, not only does it feel refreshing after cleansing, but also the skin is more moisturized. The effects of the products of Examples 2 and 3 are basically the same as those of Example 1, and are not repeated here. It can be seen that the shower gel of the present invention can provide consumers with both a refreshing skin feel and a high moisturizing effect on the skin.

It can be seen from the above results that the present invention adds a specific amount of Xinhui citrus peel extract and Xinhui citrus flower extract to the formulation system, and through the coordination with other components of the formulation system, the prepared shower gel product has not only It has a good skin cleansing effect, and has the dual effects of moisturizing and antibacterial, and the pH value is neutral, the texture is mild and non-irritating, and there is no skin tightness after use.

The above is only the preferred embodiments of the present invention, and does not limit the present invention in any form, so any simple modifications to the above embodiments based on the technical essence of the present invention are made without departing from the technical solution content of the present invention. , Equivalent changes and modifications are still within the scope of the technical solution of the present invention.

Claims

A formula for making shower gel of Xinhui citrus peel and citrus flower extract is characterized in that the formula contains the following components in mass percentage:

Sodium laureth sulfate 5-10%, ammonium lauryl sulfate 1-5%, polyquaternium-7 0.2-0.5%, PEG-120 methyl glucose dioleate 0.1-0.3%, hydroxybenzene Methyl ester 0.1% ～ 0.3%, polyoxyethylene sorbitan tristearate 0.1 ～ 0.4%, cocamidopropyl betaine 2 ～ 7%, coconut oil fatty acid diethanolamide 1 ～ 6%, Xinhui Citrus peel extract 0.5-1%, Xinhui citrus flower extract 0.5-1%, glycerin 1-5%, chitosan 0.1-0.5%, disodium EDTA 0.1-0.2%, water balance.
The formula of Xinhui citrus peel and citrus flower extract for making shower gel according to claim 1, characterized in that the formula contains the following components in mass percentage:

Sodium laureth sulfate 7-9%, ammonium lauryl sulfate 2-3%, polyquaternium-7 0.2-0.3%, PEG-120 methyl glucose dioleate 0.1-0.3%, hydroxybenzene Methyl ester 0.1% ～ 0.3%, Polyoxyethylene sorbitan tristearate 0.3 ～ 0.4%, Cocamidopropyl betaine 2 ～ 5%, Coconut oil fatty acid diethanolamide 5 ～ 6%, New Huigan peel extract 0.8-1%, Xinhui citrus flower extract 0.8-1%, glycerin 3-5%, chitosan 0.3-0.5%, disodium EDTA 0.1-0.2%, water balance.
The formula of Xinhui citrus peel and citrus flower extract for making shower gel according to claim 1, wherein the preparation method of the Xinhui citrus flower extract is:

1) Take fresh Xinhui citrus flowers, dry at 50-60 ° C with hot air, grind them into powder, and pass through a 10-100 mesh sieve;

2) Carry out carbon dioxide supercritical extraction of the powder obtained in step 1), the extraction temperature is 40-60 ℃, the extraction pressure is 200-500 BAR, wherein, according to the material-liquid ratio g / mL is 1: (0.5-2), add 95% Ethanol, static extraction 20-30min, then add 95% ethanol at 0.2-0.6mL / min, dynamic extraction 1-3h;

3) The liquid obtained in step 2) is concentrated under reduced pressure to obtain the Xinhui citrus flower extract.
The formula of Xinhui citrus peel and citrus flower extract for making shower gel according to claim 1, characterized in that: the Xinhui citrus peel extract uses carbon dioxide supercritical extraction technology.
The formula of Xinhui citrus peel and citrus flower extract for making shower gel according to claim 4, wherein the preparation method of the Xinhui citrus peel extract is:

1) Cut the fresh Xinhui citrus peel into thin strips, dry it at 50-60 ° C with hot air, grind it into powder, and sieve;

2) Add an entrainer and perform supercritical CO2 extraction of the Xinhui citrus peel powder prepared in step 1). The extraction temperature is 40-60 ° C, the extraction pressure is 200-500 BAR, and the extraction time is 1-3h. After pressure concentration, the Xinhui orange peel extract is obtained.
The formula of Xinhui mandarin peel and mandarin flower extract as claimed in claim 5, wherein in step 2), the entrainer is 70% ethanol, 95% ethanol, absolute ethanol or methanol .
The formula of Xinhui mandarin peel and mandarin flower extract as claimed in claim 5 is characterized in that: in step 2), the material / liquid ratio g / mL is 1: (0.5-2) The entrainer was statically extracted for 20 minutes, then the entrainer was added at 0.2-0.6 mL / min, and dynamic extraction was performed for 2 hours.
The formula of Xinhui citrus peel and citrus flower extract as claimed in claim 5, wherein the total flavonoid content of the Xinhui citrus peel extract is greater than 10%.
A process for preparing a shower gel of Xinhui mandarin peel and mandarin flower extract as claimed in any one of claims 1 to 8, which comprises the following steps:

1) Weigh the raw materials of each component, put deionized water in a jacket heating barrel and heat up to 50 ～ 60 ℃;

2) Emulsification: Put the raw materials of Group A into a stirring pot in sequence, heat to 80 ° C, stirring speed 30 rpm / min until the raw materials are completely dissolved; the raw materials of Group A include: water, sodium laureth sulfate, lauryl Ammonium sulfate, polyquaternium-7, PEG-120 methyl glucose dioleate, methylparaben, polyoxyethylene sorbitan tristearate;

3) Insulation: Insulation for 20 minutes, vacuuming 0.05mmHg to defoam;

4) Cooling: stirring speed 35 rpm and cooling to 50 ℃;

5) Feeding: add Group B raw materials and mix evenly (agitating speed 30 rpm), cool to 40 ° C, add Group C raw materials, and mix evenly for 10 minutes; the Group B raw materials include: cocamidopropyl betaine 2 ～ 7%, coconut oil fatty acid diethanolamide; the Group C raw materials include: Xinhui orange peel extract, Xinhui orange flower extract, glycerin, chitosan, disodium EDTA;

6) Discharging: Discharging at a temperature of 40 ° C; a small amount of pH adjuster (citric acid) can be added to control the pH value at 5.5-7.0, and a small amount of sodium chloride can be added to adjust the viscosity.