CN107519024B

CN107519024B - Alcohol-free mosquito-repelling/itching-relieving composition and preparation method thereof

Info

Publication number: CN107519024B
Application number: CN201710840403.0A
Authority: CN
Inventors: 刘建宁; 郭奕光; 陆志航
Original assignee: Shanghai Jahwa United Co Ltd
Current assignee: Shanghai Jahwa United Co Ltd
Priority date: 2017-09-18
Filing date: 2017-09-18
Publication date: 2020-04-28
Anticipated expiration: 2037-09-18
Also published as: CN107519024A

Abstract

The invention discloses an alcohol-free mosquito repellent/itching relieving composition, which comprises the following components: (a) a low viscosity microgel aqueous structuring solution having a viscosity of less than 200mPa · s and a density of 1 ± 0.01g/cm³The aqueous structuring solution comprises: (i) a high molecular weight polysaccharide polymer, and (ii) an inorganic cation, and (b) an oil phase comprising a mosquito repellent and/or antipruritic active ingredient, the oil phase having a density of 1 + -0.01 g/cm³。

Description

Alcohol-free mosquito-repelling/itching-relieving composition and preparation method thereof

Technical Field

The invention relates to a low-viscosity microgel aqueous structural solution capable of stably suspending millimeter-sized oil drops, and a novel mosquito-repelling and/or itching-relieving aqueous composition containing the low-viscosity microgel aqueous structural solution. The aqueous structuring solution of the invention and/or the aqueous mosquito repellent and/or antipruritic composition of the invention are both free of alcohol. The present invention further relates to methods of preparing the low viscosity microgel aqueous structural solution and novel mosquito repellent and/or antipruritic aqueous compositions comprising the low viscosity microgel aqueous structural solution.

Background

Conventional water-oil two-phase emulsification systems contain a certain amount of surfactant as an emulsifier or solubilizer to stabilize the system. However, the low viscosity aqueous structural solution can form a three-dimensional network structure to stabilize the system by utilizing the coordination crosslinking interaction between the high molecular polysaccharide polymer and the inorganic cation, the low viscosity aqueous structural solution does not need to add a surfactant to reduce the surface tension of the water phase and the oil phase, the microgel system formed by the low viscosity aqueous structural solution can stably suspend millimeter-sized oil drops, and only the densities of the water phase and the oil phase need to be controlled to be 1 +/-0.01 g/cm³And (4) the following steps.

Gellan gum is a polysaccharide polymer having fibrous, viscoelastic properties and good flavor release, and is also an excellent gel. The gellan gum is composed of tetrasaccharide repeating unit D- (1-3) glucopyranose unit, D- (1-4) glucopyranose uronic acid unit, and D- (1-4)) A polymer saccharide compound formed by connecting a glucopyranose unit and an L- (1-4) rhamnopyranose unit sequentially through glycosidic bonds. There are two existing forms of gellan gum products: one is high acyl gellan gum (also known as natural gellan gum) and the other is low acyl gellan gum (also known as deacylated gellan gum). The main molecular structures of the above-mentioned four sugar repeating units are the same, and the relative molecular mass is about 5X 10⁵And D, dalton. Due to their excellent stabilizing and suspending effect, they are becoming more and more widely used in the food and cosmetic field, where low acyl gellan gums have a greater ability to form gels and contribute more to the stability of the system.

Gellan gum solution is a typical pseudoplastic fluid whose solution viscosity decreases significantly with increasing shear rate and recovers with decreasing shear rate. After the gellan gum is dissolved in water, molecules can be automatically gathered to form a double-strand helical structure, two molecular chains form double-strand parallel helices in a dextrorotation mode, acting force for stabilizing the double-helical structure is mainly intermolecular hydrogen bonds, and the double helices are further gathered to form a three-dimensional network structure. The three-dimensional network structure and the double helix can be decomposed by heating or stirring, so that the three-dimensional network structure is decomposed into a random coil structure under the action of high shear rate, and the viscosity of the solution is rapidly reduced. When the shear rate or the thermal action is released, the molecular structure can restore to a three-dimensional network structure. In addition, inorganic cations also help stabilize the double helix structure and accelerate the formation of the double helix into a three-dimensional network.

Xanthan gum is also called Xanthomonas polysaccharide, and is a microbial extracellular polysaccharide with wide application, which is produced by Xanthomonas campestris by taking carbohydrate as a main raw material through fermentation engineering. Xanthan gum is a pentasaccharide repeating unit structural polymer consisting of D-glucose, D-mannose, D-glucuronic acid, acetic acid and pyruvic acid, and the relative molecular mass of the xanthan gum is 2 multiplied by 10⁶-50×10⁶About dalton.

The secondary structure of xanthan gum is that the side chain is reversely wound around the main chain skeleton, a rod-shaped double-spiral structure is formed through hydrogen bond maintenance, and the tertiary structure of xanthan gum is a spiral complex formed by combining the rod-shaped double-spiral structures by weak non-covalent bonds. Because the xanthan gum has the characteristics of good thickening property, pseudoplastic rheological property, water solubility, suspension property, emulsion stability, acid and alkali resistance, salt resistance, excellent complex property and the like, the application coverage of the xanthan gum can reach more than twenty industries, and the xanthan gum is widely applied to the fields of cosmetics, foods, medicines, spices and the like.

Hydroxypivalate, chemical name: 1-piperidinecarboxylic acid-2- (2-hydroxyethyl) -1-methylpropyl ester, is a highly effective and slightly toxic mosquito repellent, is sold as Saltidin, is colorless and odorless liquid, is insoluble in water, soluble in alcohol and vegetable oil, and has a density of 1.036g/cm³. The hydroxypipedate is an effective component of an insect repellent applied to the skin, has good cosmetic properties, is friendly to the skin, has no toxic or side effect, has no irritation, can completely replace DEET, has good stability in a formula, has good compatibility with various synthetic components, and can protect the bites of various arthropods.

The bisabolol is a component existing in chamomile, and the anti-inflammatory effect of chamomile is mainly from bisabolol, a monocyclic unsaturated half-fold terpene alcohol. Bisabolol has not only anti-inflammatory and detumescence effects, but also antibacterial activity, anti-irritation, skin protection and repair effects, and is generally added in an amount of 0.2 to 1.0%, and in most cases 0.2 to 0.5%; there is an optimum concentration for bisabolol. Beyond this concentration, the effectiveness is rather reduced (3% is rather weaker than 1%); bisabolol is insoluble in water and glycerol, soluble in fatty alcohol and paraffin, and has density of 0.92g/cm³。

The inventors tried to find out a microgel aqueous structural solution realizing low viscosity, and found out that a high molecular polysaccharide polymer gellan gum and inorganic cations form a three-dimensional network structure through coordination interaction, thereby realizing a microgel aqueous structural solution realizing low viscosity using the effect, which has excellent suspension stability and can stably suspend millimeter-sized oil droplets (e.g., essential oil droplets) which may contain effective active ingredients of hydroxypipedate or bisabolol under the condition of low viscosity.

Disclosure of Invention

It is an object of the present invention to provide an alcohol-free aqueous structural solution of microgel having low viscosity, which is capable of stably suspending oil droplets of millimeter order. The present invention also provides a mosquito repellent/antipruritic composition comprising the low viscosity microgel aqueous structural solution. The greatest difference between the mosquito repellent/itching relieving composition and the conventional mosquito repellent/itching relieving toilet water and other products is that the composition is alcohol-free and is milder, and an oil phase component containing a mosquito repellent active ingredient hydroxypipedate or an oil phase component containing an anti-inflammatory itching relieving active ingredient bisabolol can be stably suspended in a low-viscosity microgel aqueous structural solution.

In one aspect, the present invention provides an alcohol-free mosquito repellent/antipruritic composition comprising:

(a) a low viscosity microgel aqueous structuring solution having a viscosity of less than 200mPa · s and a density of 1 ± 0.01g/cm³The aqueous structuring solution comprises:

(i) a high-molecular polysaccharide polymer, a polysaccharide polymer,

(ii) an inorganic cation, wherein the cation is selected from the group consisting of,

(b) an oil phase comprising mosquito repellent and/or antipruritic active ingredients, the density of the oil phase being 1 + -0.01 g/cm³。

In a preferred embodiment, the high molecular weight polysaccharide polymer is a combination of gellan gum and xanthan gum.

In a preferred embodiment, the total amount of gellan gum and xanthan gum is from 0.1 to 0.5 wt% based on the total weight of the composition.

In a preferred embodiment, the inorganic cation is selected from: k⁺，Ca²⁺Or Mg²⁺。

In a preferred embodiment, the inorganic cation is used in an amount of 0.02 to 0.2 wt%, based on the total weight of the composition.

In a preferred embodiment, the oily phase comprises the mosquito repellent active ingredient hydroxypipedate and has a density of less than 1g/cm³The oil or fat of (2). In a preferred embodiment, the density is less than 1g/cm³The oil and fat are selected from: isooctyl palmitate, isopropyl palmitateEsters, dioctyl carbonate, cetearyl ethyl hexanoate, and combinations thereof.

In a preferred embodiment, the oil phase comprises the anti-itch active ingredient bisabolol and has a density greater than 1g/cm³The oil or fat of (2). In a preferred embodiment, the density is greater than 1g/cm³The oil and fat are selected from: trimethylpentaphenyltrisiloxane, diphenylsiloxyphenyltrimethicones, trimethylsiloxyphenyldimethicones, and combinations thereof.

On the other hand, the invention also provides a preparation method of the mosquito-repellent/itching-relieving composition, which comprises the following steps:

A. preparing the microgel aqueous structural solution;

B. preparing an oil phase;

C. and D, adding the oil phase prepared in the step B into the microgel aqueous structural solution prepared in the step A, so that the oil phase is suspended in the microgel aqueous structural solution.

Detailed Description

The inventor tries to find a microgel aqueous structural solution suitable for realizing low viscosity, and finds that a high molecular polysaccharide polymer gellan gum and inorganic cations form a three-dimensional network structure through coordination interaction, so that the microgel aqueous structural solution realizing low viscosity by utilizing the action has excellent suspension stability, can stably suspend millimeter-sized essential oil beads under the condition of low viscosity, and the essential oil beads can be composed of effective active ingredients of hydroxypipedate or bisabolol.

The invention discovers a low-viscosity microgel aqueous structural solution capable of stably suspending millimeter-sized oil drops for the first time. The low viscosity microgel aqueous structural solution contains high molecular polysaccharide polymer composed of gellan gum and xanthan gum, has viscosity of less than 200 mPa.s, and density of 1 + -0.01 g/cm³。

The gellan gum and the xanthan gum adopted by the novel microgel aqueous structural solution are polysaccharides generated by microbial fermentation, wherein the xanthan gum can bring viscosity to a system and increase the rheological property of the system. However, the xanthan gum is controlled to be less than 0.2 wt% in order to achieve the low viscosity required in the present invention.

According to the invention, the low-viscosity microgel aqueous structural solution capable of stably suspending millimeter-sized oil drops is used, and the oil-soluble component hydroxypipedate or bisabolol and the composition thereof are stably suspended in the aqueous microgel system by adjusting the densities of the aqueous phase and the oil phase, so that the visible appearance is realized, the defect of using alcohol is avoided, and the mosquito-repelling and itching-relieving effects are good.

The invention also aims to provide low-viscosity alcohol-free water-type mosquito repellent or itching relieving water, which is most different from the conventional mosquito repellent and itching relieving toilet water in that the water is alcohol-free and milder, and an oil phase component containing mosquito repellent active ingredient hydroxypipedate or an oil phase component containing anti-inflammatory and itching relieving active ingredient bisabolol is stably suspended in the low-viscosity microgel aqueous structural solution.

The invention particularly provides an alcohol-free mosquito repellent/itching relieving composition, which comprises the low-viscosity microgel aqueous structural solution and an oil phase. The aqueous structuring solution comprises a high-molecular polysaccharide polymer and inorganic cations. The oil phase comprises a mosquito repellent and/or antipruritic active ingredient. For the alcohol-free mosquito repellent/antipruritic composition of the present invention, the density of the aqueous structural solution and the oil phase are both 1 + -0.01 g/cm³。

The invention provides a low-viscosity alcohol-free novel dosage form mosquito repellent or itching relieving water, which is different from the conventional mosquito repellent and itching relieving toilet water, the mosquito repellent and itching relieving water does not contain alcohol, the used effective mosquito repellent component is high-efficiency and slightly-toxic mosquito repellent hydroxypivalate, the chemical name of the hydroxypivalate is 1-piperidinecarboxylic acid-2- (2-hydroxyethyl) -1-methylpropyl ester, and the used effective anti-inflammatory and itching relieving component is bisabolol.

In some embodiments of the present invention, the polymeric polysaccharide is used in a molecular weight range of 2X 10⁵-50×10⁶And D, dalton.

In some preferred embodiments, the polymeric polysaccharide polymer used is a combination of gellan gum and xanthan gum. In other words, the present inventors have surprisingly found that the use of gellan gum in combination with xanthan gum enables the formation of an aqueous structured solution of microgel that can stably suspend millimeter-sized oil droplets.

Applicants have also attempted to use the high molecular PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether in place of xanthan gum in combination with gellan gum in hopes of forming a more stable, low viscosity microgel aqueous structured solution. However, the addition of PEG-240/HDI copolymer bis-decyltetradecylpentadien-20 ether results in a weakening of the suspensibility of the gellan gum and a phenomenon of floating oil droplets at high temperature.

The aqueous phase microgel suspension system has low viscosity of less than 200mPa & s, can effectively suspend millimeter-sized hydroxypipedate mixed oil phase and bisabolol mixed oil phase, and has good long-term stability of the mosquito repellent water and the itching relieving water; is convenient to use and can be effectively sprayed on the surface of skin.

The aqueous microgel suspension system is formed by the interaction of high molecular polysaccharide polymers and ion cross-linking coordination, wherein the high molecular polysaccharide comprises gellan gum and xanthan gum, and the ion comprises sodium ion or calcium ion. Gellan gum solution is a typical pseudoplastic fluid whose solution viscosity decreases significantly with increasing shear rate and recovers with decreasing shear rate. After the gellan gum is dissolved in water, molecules can be automatically gathered to form a double-strand helical structure, two molecular chains form double-strand parallel helices in a dextrorotation mode, acting force for stabilizing the double-helical structure is mainly intermolecular hydrogen bonds, and the double helices are further gathered to form a three-dimensional network structure.

The oil phase component of the invention uses the high-efficiency and slightly-toxic mosquito repellent hydroxypipedate (1.036 g/cm)³) And other density is less than 1g/cm³The grease is formed by mixing one or more of isooctyl palmitate, isopropyl palmitate, dioctyl carbonate, cetearyl ethyl hexanoate and the like, and can be mutually soluble and transparent in appearance.

The other oil phase component of the invention uses the anti-inflammatory and antipruritic efficacy component of bisabolol and other components with the density of more than 1g/cm³The oil and fat are mixed by one or more of trimethyl pentaphenyl trisiloxane, diphenyl siloxy phenyl poly-trimethyl siloxane, or trimethyl siloxy phenyl poly-dimethyl siloxaneThe components are mutually soluble and have transparent appearance.

The cosmetic composition of the present invention comprises 0.1 to 0.5% by weight of the high molecular polysaccharide gellan gum and xanthan gum, relative to the total weight of the composition, and when the content is less than 0.1% by weight, the suspension stability is weak; when the content is more than 0.5% by weight, gel-like form is formed, and the low viscosity property of the present invention cannot be satisfied.

The composition of the invention comprises 0.02-0.2 wt% of cationic Na⁺，K⁺，Ca²⁺Or Mg²⁺Wherein the neutralization efficiency of the divalent ions is higher. In some preferred embodiments, the ratio of the high molecular weight polysaccharide polymer to the inorganic cation is controlled to be 5: 2. In some particularly preferred embodiments, the ratio of gellan gum to inorganic cation is controlled to be 5: 2.

The composition of the invention contains 5-20 wt% of effective mosquito repellent component hydroxypipedate, 0.2-1.0 wt% of effective anti-inflammatory and antipruritic component bisabolol, and 1.0-25 wt% of oil phase component.

Detailed Description

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described herein.

The invention is further illustrated below with reference to specific examples. It is to be understood, however, that these examples are illustrative only and are not to be construed as limiting the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.

Gellan gum and xanthan gum used in the examples were polysaccharides produced by microbial fermentation, and the gellan gum of the present invention was obtained from CP Kelco corporation, usa, under the trade name

CG-LA; xanthan gum is available from danish DANISCO; the gellan gum used was a low acyl gellan gum.

Examples 1 to 8: preparation of low viscosity microgel aqueous structuring solutions

Examples 1-8 examine the selection of inorganic cations for the degree of neutralization of gellan gums in low viscosity microgel aqueous structured solution systems.

TABLE 1

Weighing the components according to the addition amounts of the raw materials shown in the table 1, mixing, dissolving, stirring and dispersing completely at 80 ℃, stirring and cooling to room temperature to prepare the low-viscosity microgel aqueous structural solution for later use. The viscosities of examples 1-8 were less than 200 mPas, as measured by a Brookfield RVDV-C viscometer, Brookfield fly (Brookfield), and the densities of the aqueous systems were 1.0000. + -. 0.01g/cm as measured by a densitometer³Can form the microgel aqueous structural solution with low viscosity.

Examples 9 to 12: preparation of low viscosity microgel aqueous structuring solutions

Examples 9-12 examine the effect of the addition of gellan gum on low viscosity aqueous structural solutions of microgels.

TABLE 2

Weighing the components according to the addition amounts of the raw materials shown in the table 2, mixing, dissolving, stirring and dispersing completely at 80 ℃, stirring and cooling to room temperature to prepare the low-viscosity microgel aqueous structural solution for later use. Viscosity measurements were made using a Brookfield RVDV-C viscometer from Boehringer fly (Brookfield) company, examples 9-12 all had viscosities less than 200 mPas, and the density of the aqueous system was 1.0000. + -. 0.01g/cm as measured using a densitometer³Can form the microgel aqueous structural solution with low viscosity.

Examples 13 to 16: preparation of the Mixed oil phase

Examples 13-16 various mixed oil phases of the present invention were prepared.

TABLE 3

In accordance with the amounts of the raw materials shown in Table 3, in examples 13 to 16, hydroxypipedate, isopropyl palmitate, isooctyl palmitate, dioctyl carbonate, and cetearyl ethyl hexanoate were mixed in the above ratios, and then stirred and dispersed uniformly to prepare a transparent oil mixture with good intersolubility, and the density was adjusted to 1.0000. + -. 0.01g/cm³. Comparative examples 1-2 Each of hydroxypivalate, octyl methicone and cyclopentadimethicone was mixed in a ratio, uniformly dispersed by stirring, allowed to stand and then mixed at a low temperature, and thus a transparent oil mixture phase could not be obtained.

Examples 17 to 20: preparation of the Mixed oil phase

Examples 17-20 various mixed oil phases of the present invention were prepared.

TABLE 4

Mixing bisabolol with trimethylpentaphenyltrisiloxane, diphenylsiloxyphenyl trimethicone and trimethylsiloxyphenyl polydimethylsiloxane respectively according to the raw material addition amounts shown in Table 3, stirring and dispersing uniformly to prepare transparent mixed oil phase, and adjusting the density to be 1.0000 +/-0.01 g/cm³。

Examples 21 to 24: preparation of mosquito repellent composition comprising the low viscosity microgel aqueous structural solution of the present invention

Mosquito repellent compositions comprising the low viscosity microgel aqueous structuring solutions of the present invention were prepared according to the formulations shown in table 5.

TABLE 5

Weighing gellan gum, xanthan gum, calcium chloride, PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether, methyl paraben and deionized water according to the addition amounts shown in Table 5, dissolving, stirring and dispersing completely at 80 ℃, stirring and cooling to room temperature, and adding phenoxyethanol to prepare the low-viscosity microgel aqueous structure solution for later use.

Mixing hydroxypipedate with isopropyl palmitate, isooctyl palmitate, dioctyl carbonate and cetearyl ethyl hexanoate at room temperature, stirring and dispersing uniformly to obtain transparent mixed oil phase.

And adding the transparent mixed oil phase into the low-viscosity microgel aqueous structural solution to disperse the transparent mixed oil phase into oil drops of 0.5-2 mm in the low-viscosity microgel aqueous structural solution, thereby preparing the mosquito repellent composition containing the low-viscosity microgel aqueous structural solution.

Examples 25 to 28: preparation of an anti-itch composition comprising the low viscosity aqueous structured solution of microgel of the present invention

An anti-itching composition comprising the low viscosity microgel aqueous structured solution of the present invention was prepared according to the formulation shown in table 6.

TABLE 6

Gellan gum, xanthan gum, calcium chloride, PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether, methylparaben and deionized water were weighed according to the amounts shown in table 6, dissolved, stirred and dispersed completely at 80 ℃, stirred and cooled to room temperature, phenoxyethanol was added to prepare a low-viscosity microgel aqueous structural solution for later use.

Mixing bisabolol, trimethylpentaphenyl trisiloxane, diphenyl siloxy phenyl trimethicone, pigment and colorant according to a proportion at room temperature, stirring and dispersing uniformly to prepare transparent mixed oil phase.

And adding the transparent mixed oil phase into the low-viscosity microgel aqueous structural solution to disperse the transparent mixed oil phase into oil drops of 0.5-2 mm in the low-viscosity microgel aqueous structural solution to prepare the itching relieving composition containing the low-viscosity microgel aqueous structural solution.

Test example 1: stability survey

Stability examination of mosquito repellent compositions comprising the low viscosity aqueous structural microgel solutions of the present invention in examples 21-24 and anti-itch compositions comprising the low viscosity aqueous structural microgel solutions of the present invention in examples 25-28

TABLE 7

4℃

25℃

40℃

48℃

-15℃

Circulation of

Illumination of light

Time of day

3 months old

1 is provided withMoon cake

3 months old

Example 21

Good taste

Example 22

Good taste

Example 23

Good taste

Example 24

Good taste

Comparative example 3

Good taste

Layering

Good taste

Layering

Example 25

Good taste

Example 26

Good taste

Example 27

Good taste

Example 28

Good taste

Comparative example 4

Good taste

Layering

Good taste

Layering

As can be seen from Table 7, examples 21 to 28 were good in stability under high temperature (40 ℃ C. and 48 ℃ C.), low temperature (4 ℃ C. and-15 ℃ C.), room temperature (25 ℃ C.), light and circulation conditions, and no floating or sinking of oil droplets occurred in the system; wherein, under the centrifugal experiment condition (the rotating speed is 1000, the time is 30 minutes), the phenomenon that oil drops float or sink does not occur, and the stability is good. Experiments prove that the low-viscosity aqueous structural solution has good suspension stability, can well suspend millimeter-sized oil drops under the condition of well controlling the density of the two phases of water and oil, and obtains the stable mosquito-repellent/itching-relieving composition containing the low-viscosity microgel aqueous structural solution

Comparative examples 3 and 4 exhibited delamination at both high temperature cycling and light exposure.

Test example 2: mosquito repellent efficacy test

The test method comprises the following steps: GB/T13917.9-2009

Test samples: examples 21-24 mosquito repellent compositions

Test subjects: sensitive Aedes albopictus (Aedes albopictus), eclosion of 3-5 days of uninjured female adults; the source is as follows: sensitive strain which is fed for a long time in Shanghai plant physiological and ecological research institute laboratories of Chinese academy of sciences.

Temperature: 26 plus or minus 1 ℃ and relative humidity of 65 plus or minus 10 percent

Mosquito cage: 400mmX length, 300mmX width and 300mm height

Attack force experiment: 300 test insects are put into the mosquito cage, the back of the hand of a tester exposes 40mmX 40mm skin, and the rest part is tightly shielded. The hands are put into the mosquito cage for 2 minutes, closely observed, the mosquitoes are found to stop falling, the arms are shaken to drive the mosquitoes away before the mouth organ of the mosquitoes penetrates into the skin, and the record is that 1 test insect stops falling. More than 30 test persons who stop before and test insects are qualified in attack power, and the person and the cage mosquitoes can be subjected to repelling experiments.

Repelling experiment: selecting 5-7 testers with qualified offensive power (half of man and woman, no wine, tea or coffee is drunk before and during the test, and no essence-containing product is used), drawing skin areas of 50mmX 50mm on the backs of the hands of the testers, uniformly coating the mosquito repellent to be tested on one hand according to the dosage of 1.5 mu L/cm2, exposing 40mmX 40mm skin in the skin, and tightly shielding the rest parts, wherein the other hand is blank control. And (3) coating the mosquito repellent for 2 hours, putting hands into a mosquito cage with qualified attack power for 2 minutes, and observing whether mosquitoes come and stop falling and sucking blood. And then testing once every 1 hour, and judging that the mosquito fails to be used as the repellent as long as one mosquito sucks blood in front. The effective protection time (hours) for the repellent was recorded. The contrast test is firstly carried out by the contrast hand each time, the test insects with qualified attack force can be continuously tested, and the test insects with unqualified attack force need to be replaced by the qualified test insects for testing.

Test results

Test sample	Effective repelling time (hours)
		Example 21 mosquito repellent composition	6.33
Example 22 mosquito repellent composition	6.14
		Example 23 mosquito repellent composition	6.28
Example 24 mosquito repellent composition	6.17

The effective repelling time of the mosquito repelling compositions in the embodiments 21 to 24 is longer than 6 hours, and the effective repelling time is grade A according to the evaluation standard of the traditional Chinese medicine effect index in GB/T13917.9-2009 indoor pesticide effect test method for pesticide registration hygiene, and the effective repelling time is not shorter than 6 hours, so that the mosquito repelling compositions prepared in the embodiments 21 to 24 can be judged to reach grade A, and the effective mosquito repelling effect can be achieved. Test example 3: test for relieving itching

Test materials:

animals: guinea pig 110 (10 per group) body weight: 300g left and right Shanghai dried turtle Shell Biotech Co Ltd

Histamine phosphate: china institute for testing and testing food and medicine

Positive control: dexamethasone (30g:22.5mg) Sanjiu medicine industry

Sample preparation: EXAMPLES 25 to 28 antipruritic compositions

The test conditions are as follows: laboratory temperature: relative humidity at 20-25 ℃: 60 to 70 percent

The test method comprises the following steps:

guinea pigs were randomly divided into 8 groups of 10 animals each. The test sample is divided into three groups, namely a blank control group, a positive control group and a sample. One day prior to the experiment, the right hind instep of each group of guinea pigs was painted with a sample. On the day of the experiment, the shaved area of the right hind paw of the animal was scratched with a coarse sandpaper in the range of about 1 cm square, and the sample was applied once again to the shaved area, and the blank control group was given an equal amount of distilled water. After 10 minutes, 0.01% histamine phosphate 0.05 ml/tube was initially applied to the wound surface, followed by 0.01%, 0.02%, 0.03%, 0.04%. multidentation at 3 minute intervals, each time 0.05 ml/tube. Until the guinea pig licks the right hind paw, the sum of histamine phosphate administered when the guinea pig licks the right hind paw was last taken as the scratchiness threshold. The scratchiness threshold of each group was recorded and compared.

And (3) test results:

examples 25-28 Effect of anti-itching compositions on histamine phosphate-induced itching response

*: p values were all compared between test and blank control

Compared with the blank control, the antipruritic compositions in the examples 25 to 28 have the effect of improving the threshold of itching of the guinea pig (P <0.01) and have obvious antipruritic effect.

While typical embodiments have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.

Claims

1. An alcohol-free mosquito repellent/antipruritic composition comprising:

(i) a high molecular polysaccharide polymer, wherein the high molecular polysaccharide polymer is a combination of gellan gum and xanthan gum, and the total amount of the gellan gum and the xanthan gum is 0.1-0.5 wt% based on the total weight of the composition;

(ii) inorganic cations in an amount of 0.02 to 0.2 weight percent, based on the total weight of the composition;

(b) an oil phase containing mosquito repellent active ingredient hydroxypivalate and having a low densityAt 1g/cm³Wherein the density is less than 1g/cm³The oil and fat are selected from: isooctyl palmitate, isopropyl palmitate, dioctyl carbonate, cetearyl ethylhexanoate, and combinations thereof; or the oil phase contains bisabolol with antipruritic effect and density of more than 1g/cm³Wherein the density is more than 1g/cm³The oil and fat are selected from: trimethylpentaphenyltrisiloxane, diphenylsiloxyphenyltrimethicones, trimethylsiloxyphenyldimethicones, and combinations thereof.

2. The composition of claim 1, wherein the inorganic cation is selected from the group consisting of: k⁺，Ca²⁺Or Mg²⁺。

3. A process for preparing a mosquito repellent/antipruritic composition according to claim 1, said process comprising the steps of:

A. preparing the microgel aqueous structural solution;

B. preparing an oil phase;