CN106727255B

CN106727255B - Shampoo containing natural surfactant and preparation method thereof

Info

Publication number: CN106727255B
Application number: CN201710123265.4A
Authority: CN
Inventors: 王书敏
Original assignee: Individual
Current assignee: Individual
Priority date: 2017-03-03
Filing date: 2017-03-03
Publication date: 2020-09-15
Anticipated expiration: 2037-03-03
Also published as: CN106727255A

Abstract

The repairing shampoo comprises the following components in percentage by weight: 6.0-40.0% of surfactant, 2.0-8.0% of yak bone small molecular peptide, 0.01-2.0% of thickening agent, 0.5-3.0% of pearling agent, 0.01-0.5% of preservative, 0.05-2.0% of humectant, 1.0-20.0% of plant extract, 0.1-3.0% of essence and the balance of water; the surfactant contains 0.5-80 wt% of natural surfactant. The natural surfactant enables the shampoo to be mild and non-irritating while effectively controlling oil, and has anti-inflammatory and other effects.

Description

Shampoo containing natural surfactant and preparation method thereof

Technical Field

The invention relates to the field of daily chemicals, and particularly relates to shampoo containing a natural surfactant and a preparation method of the shampoo.

Background

With the increase of age, the increase of working pressure, environmental pollution and other reasons, people's hair becomes rough and dull, and in addition, because of frequent hair dyeing, perm, shaping and the like, the hair or scalp is inevitably contacted with chemical substances, so that the problems of dry hair, rough hair, dull and dull hair and the like are also caused, and the hair is oily and greasy. Therefore, the ordinary anti-dandruff and decontamination shampoo with single functions of removing dandruff, preventing alopecia and the like in the market at present cannot meet the requirements of consumers, and the shampoo with good oil control effect, no stimulation and damaged cell repairing effect is urgently needed to be developed.

The natural surfactant is superior to other existing surfactants in dermatology, toxicology, mild compatibility to skin and the like, and is widely applied in daily life, for example, lecithin is a natural surfactant, is one of components of organism cells, is widely distributed in animals and plants, and has an amphiphilic structure consisting of a lipophilic structure formed by combining two acyl groups in glycerol through ester bonding and a quaternary ammonium group hydrophilic structure formed by combining the two acyl groups in the glycerol through taking a phosphate group as a medium. Natural surfactants can improve the wetting and spreading properties, dispersion stability and storage resistance of oils and fats in skin care products.

CN101880307A discloses a method for extracting tea saponin by using microorganisms, which comprises the steps of mixing and fermenting high starch substances added from outside sources, complex enzyme and alcohol yeast to enable starch in the high starch substances to be fully utilized by the alcohol yeast to generate alcohol to form mash, then soaking a certain amount of crushed oil-tea camellia cake powder into the fermented mash, uniformly mixing and culturing, carrying out solid-liquid separation after a few days, and then concentrating and drying supernatant liquid of the separated liquid to obtain the final product tea saponin.

CN102670447A discloses a natural plant extract for hair care and a preparation method and application thereof, wherein the natural plant extract is prepared from the following raw materials in parts by mass: 40-65 parts of polygonum multiflorum, 30-50 parts of angelica sinensis, 20-35 parts of cacumen biotae, 10-25 parts of soapberry, 20-50 parts of tea seeds and 25-40 parts of golden sapree.

CN103479539A discloses a shampoo containing natural saponin and natural thickener, which contains natural saponin, natural thickener and water, wherein the natural saponin at least comprises one of sapindus saponin and theasaponin or a mixture of the two; the natural thickener at least comprises one or more of natural plant starch, xanthan gum, Arabic gum, guar gum, carrageenan and seaweed gel. According to the invention, through the matching use of the natural saponin and the natural thickener, the shampoo in the formula has viscosity suitable for daily life, and can be used for mildly cleaning hair without stimulating and damaging scalp.

CN1370515A discloses a shampoo, which is composed of all natural plant components, such as soapberry fruit pulp extract, shrubalthea leaf extract, clove, rhubarb and pepper extract.

CN105431154A discloses a topical antibacterial composition and a method of use thereof, which relates to a topical antibacterial composition comprising a quaternized chitosan derivative comprising a polymerizable organic moiety and an amphoteric surfactant.

The initial research on the foaming performance of a natural surfactant in space station bathing, green-blue and the like, manned space, 2016 and 22(4), designs a bathing product taking the natural surfactant as a main effective component and a natural preservative and a bacteriostatic agent as main auxiliary materials according to the requirements of space station astronauts, screens a low-foam easy-to-wash and high-cleanliness product formula by using the foaming performance and sensory evaluation of the product as indexes by using an orthogonal optimization method, performs further reaction condition optimization and physicochemical stability detection on the product in the formula, obtains an optimal compound formula product, and achieves the effects of natural non-irritation, low foam easy-to-wash and high cleanliness.

However, in the above-mentioned prior art, completely using a synthetic surfactant has a feeling of stimulation, and dandruff is easily generated, and it is known that the surface activation effect of the natural surfactant used is not significant, and further, the conventional shampoo is insufficient for deeply nourishing hair. Therefore, the shampoo which has strong surface activity, is mild and non-irritant and has deep nourishing efficacy is needed in the field.

Disclosure of Invention

In order to solve the technical problems, the invention provides a formula and a production process of a repair shampoo containing a natural surfactant and yak bone small molecular peptide.

In one aspect of the invention, the repair shampoo containing the natural surfactant and the preparation method thereof are provided, and the repair shampoo comprises the following components in parts by weight: by weight percentage, 6.0-40.0% of surfactant, 2.0-8.0% of yak bone small molecular peptide, 0.01-2.0% of thickening agent, 0.5-3.0% of pearling agent, 0.01-0.5% of preservative, 0.05-2.0% of humectant, 1.0-20.0% of plant extract, 0.1-3.0% of essence and the balance of water.

The surfactant comprises 0.5-100 wt%, preferably 5-80 wt%, preferably 20-90 wt%, preferably 50-80 wt% of natural surfactant.

The natural surface active ingredient is preferably a natural compound represented by the following formula (I):

the natural compound shown in the formula (I) is extracted from carambola leaves, has a surface activity in shampoo, and also has antibacterial and anti-inflammatory effects due to a flavone structure. The compound can be extracted by the following method: sun drying carambola leaf, pulverizing, reflux heating in distilled water for 10-30min, cooling to room temperature, filtering to obtain aqueous extract, concentrating, enriching with macroporous adsorbent resin, eluting and purifying, wherein the eluent is hydrophilic solvent such as ethanol or mixture of ethanol and water (preferably 1: 1 volume), concentrating the eluate under vacuum degree of-0.01 to-0.1 MPa at 40-60 deg.C, purifying the concentrated purified solution with ion exchange chromatography column (such as macroporous ion exchange resin, such as Amberlite series resin) for the second time, using hydrophilic solvent as mobile phase, the natural compound content shown in the formula (I) is distinguished and collected, the collected liquid is concentrated, the temperature is controlled to be 10-50 ℃, so as to ensure that the compound is not degraded, and then the concentrated solution containing the natural compound shown in the formula (I) is obtained. The concentrated solution can be directly used for preparing shampoo. That is, the natural compound may be used in the form of a (aqueous) concentrate in the formulation of a shampoo.

In addition, the inventor finds that a large amount of small molecular peptides (small peptides) can be generated after yak bone collagen is treated by a specific enzymolysis method and the like, the small peptides are processed by taking the yak bone collagen as a raw material and are peptides with much smaller molecular weight than the collagen, wherein the mass fraction of the small peptides with the molecular weight of less than 1000 daltons is about 85%, the small peptides of the yak bone collagen are easy to dissolve in water and can be quickly absorbed by a human body more easily, the small peptides can directly reach the cell tissues of the human body without digestion, and the daily chemical products prepared by the small peptides have the effects of deeply nourishing cells, repairing damaged cells and delaying cell senescence.

Preferably, the shampoo comprises the following components in percentage by weight: 10.0-40.0% of surfactant, 2.0-8.0% of yak bone small molecular peptide, 0.1-2.0% of thickening agent, 1.5-3.0% of pearling agent, 0.1-0.5% of preservative, 0.5-2.0% of humectant, 4.0-16.0% of plant extract, 0.5-3.0% of essence and the balance of water.

Preferably, the shampoo comprises the following components in percentage by weight: 15.0-35.0% of surfactant, 1.0-6.0% of yak bone small molecular peptide, 0.5-2.0% of thickening agent, 1.0-3.0% of pearling agent, 0.2-0.5% of preservative, 0.5-2.0% of humectant, 6.0-20.0% of plant extract, 0.5-2.0% of essence and the balance of water.

Preferably, the shampoo comprises the following components in percentage by weight: 26.0% of surfactant, 8.0% of yak bone small molecular peptide, 1.0% of thickening agent, 2.0% of pearling agent, 0.4% of preservative, 1.0% of humectant, 16.0% of plant extract, 1.5% of essence and the balance of water.

The surfactant may further include a combination of any two or more selected from the group consisting of sodium laureth sulfate, ammonium laureth sulfate, cocamidopropyl betaine, laureth-4, laureth-23, PEG-55 stearate, and dodecylbenzene sulfonate TEA salt, and the combination ratio is not particularly limited.

The thickening agent is coconut oil amide MEA, guar gum hydroxypropyl trimethyl ammonium chloride, cetearyl alcohol, styrene/acrylic acid (ester) copolymer; the pearling agent is titanium dioxide; the preservative is one or more of polyquaternium-10, methyl chloro isothiazolinone and methyl isothiazolinone propionic acid.

The humectant is a dimethiconol humectant; the essence is one or more of lavender essence, rose essence, mint essence and the like; the plant extract is one or more of dendrobium officinale extract and ginseng extract.

The invention also aims to provide a method for preparing the repairing shampoo, which comprises the following steps:

(1) weighing water in the formula, heating to 80-85 ℃, adding a surfactant under stirring, and stirring until the surfactant is completely dissolved;

(2) adding pearling agent, stirring to dissolve completely, cooling to below 65 deg.C;

(3) then sequentially adding the yak bone small molecular peptide, the plant extract, the preservative, the thickening agent, the humectant and the essence;

(4) after stirring uniformly, adjusting the pH value of the shampoo to 5.5-6.5 by using a pH regulator, and aging for 18 hours to obtain the yak bone small molecule peptide repairing shampoo.

In another aspect of the present invention, there is provided a method for extracting the above small molecule peptide from yak bone, namely yak bone small molecule peptide, which comprises the steps of defatting, decalcification and purification treatment, more specifically or more preferably, the method comprises the steps of:

(1) drying yak bone with the meat, muscle, membrane and cartilage attached to the surface removed, then crushing, and sieving with a 30-mesh sieve to obtain yak bone powder;

(2) adding 5-10 times of degreasing solution A by weight of yak bone powder, wherein the degreasing solution A is a mixture of chloroform, methanol and acetone in a volume ratio of (2.0-3.0) to (3.0-6.0) to (0.5-1.0), preferably 1: 2: 0.8, stirring and degreasing at 0-4 ℃ for 16-48h, filtering the degreasing solution A, and adding the yak bone powder into ethanol containing a surfactant: in the degreasing solution B which is water mixed solution (preferably 1: 1 volume ratio), the concentration of the surfactant in the degreasing solution B is 0.01-0.1mol/L, and the degreasing is carried out for 4-10h under stirring at the temperature of 5-10 ℃;

(3) filtering the degreasing solution B after the step (2) is completed, adding 0.1moL/L hydrochloric acid solution containing 0.2-0.5moL/L EDTA in an amount of 10-15 times the weight of the yak bone powder, stirring at 5-10 deg.C for 16-32h, removing the hydrochloric acid solution (e.g. by centrifugation), adding 10-15ml of 4moL/L moroxydine hydrochloride per g of yak bone, stirring at 5-10 deg.C for 8-24h, centrifuging, washing the precipitate with Tris-HCl (pH7.4) buffer solution and 0.5-1.0moL/L acetic acid solution, adding 5-20ml of pepsin digestive juice and 1-10ml of neutral protease digestive juice (preferably containing 0.5moL/L acetic acid) per g of yak bone, suspending, stirring at 2-4 deg.C for 12-36h, centrifuging and collecting supernatant;

(4) adjusting the pH of the supernatant to about 7.5 with 3.0-5.0mol/L NaOH, adding NaCl to make the concentration of NaCl 2.0mol/L, salting out overnight at 4 ℃, and centrifuging to obtain a supernatant Q1 and a precipitate P1; continuously adding NaCl into the supernatant Q1 to adjust the NaCl concentration to 4.0mol/L.4 ℃, salting out overnight, and centrifuging to obtain a supernatant Q2 and a precipitate P2; mixing the precipitate P1 and P2, dissolving with 0.1-0.3moL/L acetic acid, neutralizing with 1.0-2.0moL/L NaOH to pH7.5, dialyzing with 0.005moL/LTris-HCl (pH7.4) and distilled water, and balancing to obtain small molecular peptide primary extract E1;

(5) mixing small molecule peptide primary extract E1 and Tris-HCl (pH7.4) buffer solution with the volume of 3 times, placing the mixture into a beaker, adding an anion exchanger (preferably anion exchange resin) balanced by the buffer solution, wherein the volume ratio of the resin to the small molecule peptide primary extract E1 is about 1: 5-1: 10, uniformly mixing, slowly stirring for 60-120min, performing centrifugal separation, and collecting supernatant; adding sodium chloride into the supernatant to make the concentration of the sodium chloride be 2.0moL/L, salting out at 4 ℃ overnight, centrifuging for 30min, collecting the precipitate, dissolving the precipitate with 0.1-0.3moL/L acetic acid, dialyzing and balancing with 0.05moL/L acetic acid, 0.01moL/L acetic acid and distilled water respectively to obtain a small molecular peptide solution, and freeze-drying to obtain the small molecular peptide protein freeze-dried powder.

The proportion of the small molecular peptide with the molecular weight less than 1000 daltons in the small molecular peptide protein freeze-dried powder is more than 95 wt%, preferably more than 98 wt%, more preferably more than 99 wt%, and more preferably almost all small molecular peptide eggs.

For the purposes of the present invention, the acetic acid solution and hydrochloric acid solution, etc., are both referred to as aqueous solutions, as is generally understood by those skilled in the art.

The surfactant in the degreasing solution B in the step (2) is preferably a zwitterionic surfactant. More preferably a betaine type zwitterion represented by the following formula (II):

by using the specific surfactant, the content of oil or fat in the collagen can be reduced to 0.001% by weight or less, preferably 0.0001% by weight or less. The surfactant has many unique properties in the aspects of critical micelle concentration, interfacial property and the like, such as higher surface activity, lower Krafft temperature, better solubility and unique rheological property, so that the surfactant has particularly good effect in the aspect of extremely reducing the fat content, thereby reducing the greasy feeling of the shampoo to a lower level.

In addition, the acetone solvent is added into the degreasing liquid A, so that the degreasing effect is improved, and meanwhile, the protein denaturation can be effectively prevented, and the generation of denatured impurities can be effectively prevented. This has not been reported in the literature before.

The mass fraction of small peptides with a molecular weight of less than 1000 daltons in the small peptides obtained by the method of the present invention is about 85%, preferably more than 85%, more preferably more than 90%.

The invention has the beneficial effects that: the natural surfactant is mild and non-irritant, has the effects of resisting bacteria and diminishing inflammation, contains yak bone small-molecular peptide and natural plant components, is high in proportion of low-molecular-weight small peptide, good in nourishing effect, low in impurity content, especially low in ester content, free of greasy feeling, soft in texture, safe and non-irritant, contains the yak bone small-molecular peptide and the natural plant components, is rich in foam, mild and non-irritant, strong in decontamination capability, and good in hair brightness, dryness and wet combing property after use, has an obvious effect of repairing damaged hair, has herbal fragrance and refreshing effect, and is a multi-effect shampoo integrating hair washing, hair care and restoration.

Detailed Description

The invention is further illustrated by the following examples and comparative examples:

examples 1 to 4

Examples 1-4 are examples of a yak bone small molecule peptide deep shampoo. The formula of the deep shampoo containing the yak bone small-molecule peptide in the embodiment is shown in the following table 1:

table 1: formulation table (by weight percentage content)

The small-molecule peptide of the hair ox bone is extracted from the yak bone according to the method, wherein the proportion of the small-molecule peptide with the molecular weight of less than 1000 daltons is 98.5 percent by weight.

The method for preparing the shampoos of examples 1-4 comprises the following steps: weighing water in the formula, heating to 80-85 ℃, adding a surfactant under stirring, and stirring until the surfactant is completely dissolved; adding pearling agent, stirring to dissolve completely, cooling to below 65 deg.C; then sequentially adding the yak bone small molecular peptide, the plant extract, the preservative, the thickening agent, the humectant and the essence; after stirring evenly, adjusting the pH value of the shampoo to 5.5-6.5 by using a pH regulator, and aging for 18 hours.

Comparative example 1

This comparative example 1 is different from example 1 only in that the compound represented by formula (I) is replaced with ordinary laureth-23 and the yak bone small molecule peptide is replaced with ordinary bone peptide (available from pharmaceutical group chemical agents, ltd.).

The shampoo of examples 1 to 4 shows that it has a good oil control effect, shows that the surface active effect is fully exerted, and it is mild and non-irritating, does not easily produce dandruff, has a pleasant and elegant smell, and enables the effective ingredients to permeate into the hair, and the small molecular peptides can help repair damaged hair proteins and isolate the cuticle which has been peeled off, thereby helping to repair the surface of hair, protecting the hair from damage, and in addition, can provide a more refreshing feeling of care to the hair without feeling heavy hair. In contrast, the shampoo of comparative example 1 has a strong degreasing ability, but has a certain stimulation to the scalp, a certain scurf phenomenon, and also has a poor hair quality restoration ability, and the user has a greasy feeling, feels heavy hair, and has no sense of relaxation.

This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to make and use the invention. The patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims. All citations referred to herein are incorporated herein by reference to the extent that no inconsistency is made.

Claims

1. A method of preparing a restorative shampoo containing a natural surfactant, comprising the steps of:

(1) weighing water in the formula, heating to 85 ℃, adding a surfactant under the stirring condition, and stirring until the surfactant is completely dissolved;

(4) after stirring uniformly, adjusting the pH value of the shampoo to 6.5 by using a pH regulator, and aging for 18 hours to obtain a repair shampoo containing a natural surfactant;

the repairing shampoo comprises the following components in percentage by weight 1-4:

the surfactant comprises a natural surfactant component, and is a compound shown in the following formula (I):

formula (I)

The compound shown in the formula (I) is extracted by the following method: drying carambola leaves in the sun, crushing, then heating in distilled water under reflux for 10-30min, cooling to room temperature, filtering to obtain an aqueous extract, concentrating, enriching, eluting and purifying by using macroporous adsorption resin, wherein the eluent is ethanol or a mixture of ethanol and water, then concentrating the eluent under the conditions of vacuum degree of-0.01 to-0.1 MPa and temperature of 40-60 ℃, performing secondary refining on the concentrated purified liquid by using an ion exchange chromatography column, using a hydrophilic solvent as a mobile phase, performing differential collection according to the content of the compound shown in the formula (I), concentrating the collected liquid, and controlling the temperature to be 10-50 ℃ so as to ensure that the compound is not degraded, thus obtaining the concentrated liquid containing the compound shown in the formula (I).

2. The method of claim 1, wherein the yak bone small molecule peptide is extracted by a method comprising the steps of defatting, decalcification and purification.