Mosquito-repelling composition, mosquito-repelling emulsion and preparation method of mosquito-repelling emulsion

Abstract

The invention provides a mosquito-repelling composition, a mosquito-repelling emulsion and a preparation method of the mosquito-repelling emulsion. The mosquito repellent composition comprises the following components: 15%-30% of paracardine; 1%-5% of a nonionic emulsifier; 0.1%-4% of an anionic emulsifier; 0.1%-1% of a co-emulsifier; 0.1%-1.0% of a thickening agent; the pH regulator is used for regulating the pH value of the mosquito repelling composition to 6.5 to 7; wherein% is the mass percentage of each component in the total mass of the mosquito-repellent composition. The mosquito repellent emulsion belongs to an O / W formula system, has high content of paragliptin, and has the advantages of low viscosity, good stability, refreshing skin feeling, good itching relieving effect and the like; in addition, the preparation method is simple and convenient to operate and produce.

Description

Technical Field

[0001] The invention relates to a mosquito repellent composition, a mosquito repellent emulsion and a preparation method thereof. Background Art

[0002] Mosquito bites not only cause itching and swelling on the skin, but also lead to more than 80 infectious diseases, such as malaria, dengue fever, Japanese encephalitis and filariasis, which seriously endanger human life. With the change of consumer awareness and behavior, consumers have higher requirements for the safety, effectiveness and convenience of mosquito repellent products.

[0003] At present, the market mainly uses two mechanisms of action, chemical insecticides and mosquito repellents, to prevent mosquito bites.

[0004] Chemical insecticides are mainly flumethrin and cypermethrin, which are often used in electric mosquito coils, mosquito coils and insecticide sprays. They are slightly toxic, highly efficient and have low residual properties. They are generally not recommended for children under 2 years old. Mosquito coils or electric mosquito coils made with chemical insecticides, if used for a long time, will still pose a potential threat to human health due to their high cumulative amount, so they do not meet the current consumer demands.

[0005] Mosquito repellents are mainly divided into two categories. One is the mosquito repellent that does not contain mosquito repellent ingredients, which simply uses odorous plant extracts or chemical preparations to repel mosquitoes; the other is the mosquito repellent that contains mosquito repellent ingredients, which can interfere with the ability of mosquitoes to track hosts. Specifically, mosquitoes mainly use carbon dioxide and lactic acid produced by human breathing to find hosts. When we apply products containing mosquito repellents on the surface of our skin, the mosquito repellent can form a barrier on the skin surface after evaporation, which can effectively interfere with the mosquito's chemical sensors' sensitivity to human volatiles, thereby achieving the mosquito repellent effect.

[0006] The floral water, mosquito repellent spray, mosquito repellent lotion, mosquito repellent bracelet and mosquito repellent patch prepared by the mosquito repellent mechanism are the main popular products at present. Floral water products often use essential oils to repel mosquitoes, which can effectively prevent mosquito bites, but the repellent time is short, the use is more frequent, and the smell is not popular with the public; mosquito repellent spray products often use synthetic mosquito repellents (DEET, IR3535, ) is dissolved in alcohol, polyols, solubilizers and other formulation systems, but because of the use of flammable and explosive chemical ingredients such as alcohol in the formula, there are great safety hazards, and it is not very suitable for wounds and children; emulsified mosquito repellent products are often in W / O dosage form. Such products use oil as the external phase, and the skin feel is relatively greasy, which is not very popular with consumers; mosquito repellent bracelets or mosquito repellent patches use plants to repel mosquitoes, with a relatively small range of action and average results.

[0007] The U.S. Environmental Protection Agency (EWG) has registered and certified seven effective mosquito repellent ingredients that can be used on human skin: peppermint oil, citronella oil, picaridin IR3535, DEET, oil of lemon eucalyptus, undecanoic acid.

[0008] DEET is a highly effective and long-lasting mosquito repellent, but it carries the risk of irritating the skin and eyes and long-term use should be avoided.

[0009] The full chemical name of picaridin is 2-(2-hydroxyethyl)piperidine-1-carboxylic acid sec-butyl ester, which can also be called icaridin or picaridin. It is a safe and effective mosquito repellent ingredient recommended by the World Health Organization (WHO). It has the advantages of high safety, long-lasting protection, no irritation to the skin and no toxicity. It is an active ingredient in high-end mosquito repellent products, which can effectively protect people from mosquito and tick bites, and can widely and reliably prevent a variety of insect-borne diseases, including malaria, dengue fever and Zika virus. It is currently sold in more than 50 countries. Compared with other ingredients, It is a new type of mosquito repellent ingredient discovered through extensive experimental research, which has good protection and safety for the human body. Mosquito repellents can provide up to eight hours of protection. Extensive research data and usage tests have shown that It is safe for both adults and children, so it is suitable for the whole family. It also has ideal cosmetic properties, it is non-sticky and non-greasy, will not corrode clothing, accessories, sports equipment, and is very suitable for outdoor activities. Due to its excellent properties, Can be easily formulated as needed as liquid, aerosol, pump spray, wipe, cream / ointment or stick, making it suitable for a variety of applications and facilitating custom product development. The American Academy of Pediatrics (AAP) stipulates that the frequency of use should not exceed once a day; the Canadian government stipulates that children under 6 months old cannot use mosquito repellent products containing picaridin; the Centers for Disease Control and Prevention (CDC) stipulates that children under 2 months old cannot use them.

[0010] IR3535 is a broad-spectrum and highly effective mosquito repellent with no side effects on the skin. Compared with DEET, it is safer and less irritating, but its mosquito repellent effect is weaker than DEET and Regarding IR3535, the Shenzhen Municipal Administration for Market Regulation stipulates that it should not be used by children under 2 months old.

[0011] The real mosquito repellents in lemon eucalyptus oil are citronellal and citronellol, but citronellol itself is an allergen that can easily cause allergies. Especially for infants and young children, if they are exposed to high concentrations of lemon eucalyptus oil for a long time, they may suffer varying degrees of neurological damage. The Centers for Disease Control and Prevention (CDC) stipulates that lemon eucalyptus oil cannot be used on children under 3 years old.

[0012] Citronella oil is usually a natural extract from plants and is not toxic, but it contains a large amount of aldehyde components, which may cause skin allergic reactions and may also irritate the nasal mucosa and respiratory mucosa, causing adverse effects. Therefore, it is not suitable for infants and young children.

[0013] At present, the common emulsified mosquito repellent products on the market are prepared using DEET or IR3535. In recent years, products containing DEET have been allergic to children in terms of toxicology, and the chemical structure of IR3535 is a derivative of β-alanine from a natural source. It has poor water solubility and a high degradation rate in water, which greatly reduces the mosquito repellent effect of IR3535 products. The prepared mosquito repellent product is usually in the form of mosquito repellent spray or gel. Pre-dissolved with polyols or alcohol to make it easier to dissolve in water, high content of polyols and alcohol will have high permeability problems, seriously affecting the mildness of the product, and the spray form has the risk of easy inhalation during use. Therefore, the mosquito repellent lotion of the emulsion system has good skin feel, more uniform coating, and no risk of inhalation, which is the ideal choice for current mosquito repellent products. The chemical polarity of is relatively strong, and it is difficult to be emulsified by conventional emulsifiers. In addition, there is a risk of hydrolysis and migration in the formula, which seriously affects the stability. Therefore, there are few products on the market that use high content of The prepared mosquito repellent lotion product.

[0014] Based on the current development status, using safe, efficient and gentle The difficulty in developing mosquito repellent lotions is to prepare an O / W emulsified mosquito repellent lotion that has a refreshing skin feel, low viscosity, stability and high efficiency. Summary of the invention

[0015] In order to overcome the problems of high viscosity and instability of the oil-in-water (O / W) emulsified mosquito repellent liquid prepared in the prior art, the present invention provides a mosquito repellent composition, a mosquito repellent emulsion and a preparation method thereof; the mosquito repellent emulsion belongs to an O / W formulation system, and has a high content of picaridin The mosquito repellent emulsion has the advantages of low viscosity, good stability, refreshing skin feel, good antipruritic effect, etc.; in addition, the preparation method of the invention is simple and easy to operate and produce.

[0016] The above technical problems are solved by the following technical solutions of the present invention:

[0017] The invention provides a mosquito repellent composition, which comprises the following components: 15%-30% of picaridin; 1%-5% of a nonionic emulsifier; the nonionic emulsifier is one or more of a fatty alcohol polyether emulsifier, a polyglycerol fatty acid ester emulsifier, a sucrose fatty acid ester emulsifier, an alkyl glycoside emulsifier, a Tween emulsifier, a Span emulsifier and a fatty alcohol polyoxyethylene emulsifier; 0.1%-4% of an anionic emulsifier; the anionic emulsifier is one or more of an amino acid emulsifier, a carboxylate emulsifier, a phosphate emulsifier, a citrate emulsifier and a fatty acid salt emulsifier; 0.1%-1% of an auxiliary emulsifier; 0.1%-1.0% of a thickener; a pH regulator, used for adjusting the pH value of the mosquito repellent composition to 6.5-7; wherein % is the mass percentage of each component in the total mass of the mosquito repellent composition.

[0018] In the present invention, picaridin It is an active substance in the mosquito repellent composition that has mosquito repellent effect.

[0019] In the present invention, emulsifiers with different HLB values ​​(hydrophile-lipophile balance) are selected to adjust the hydrophile-lipophile balance between the anionic emulsifier and the nonionic emulsifier to promote the stability of picaridin in the emulsified system.

[0020] In some embodiments, the content of picaridin is 15%, 20%, 25% or 30%.

[0021] In some embodiments, the content of the nonionic emulsifier is 3%-5%.

[0022] In a specific embodiment, the content of the nonionic emulsifier is 3%, 4% or 5%.

[0023] In some embodiments, the content of the anionic emulsifier is 0.1%-2%.

[0024] In a specific embodiment, the content of the anionic emulsifier is 0.1%, 0.5%, 1%, 1.5% or 2%.

[0025] In some embodiments, the content of the co-emulsifier is 0.1%, 0.5% or 1%.

[0026] In some embodiments, the content of the thickener is 0.1%-0.5%, preferably 0.1% or 0.5%.

[0027] In some embodiments, the nonionic emulsifier is steareth-2, steareth-21, beheneth-25, sucrose polystearate, sorbitan stearate, polysorbate-60, sorbitan oleate, cocoyl glucoside, cetyl PEG / PPG-10 / 1 dimethicone, cetearyl olive oil ester, PEG-4 olive oil ester, cetearyl glucoside, sorbitan sesquioleate, lauryl PEG-9 polydimethylsiloxyethyl dimethicone, triphenin PEG-20 esters , methyl glucose sesquistearate, PEG-20 methyl glucose sesquistearate, sucrose distearate, C20-22 alcohol phosphate, tribehenin PEG-20 esters, sucrose stearate, ceteareth-25, sorbitan olivate, inulin lauryl carbamate, glycolipids, glycerin, soy bean seed extract, glyceryl stearate, PEG-100 stearate, polyglyceryl-10 laurate, polyglyceryl-4 isostearate, polyglyceryl-4 laurate and polyglyceryl-2 isostearate.

[0028] In a specific embodiment, the nonionic emulsifier includes glyceryl stearate (and) PEG-100 stearate; the mass ratio of the glyceryl stearate to the PEG-100 stearate is 1:1 or 2:1.

[0029] In a specific embodiment, the nonionic emulsifier includes inulin lauryl carbamate and (and) glycerol; the mass ratio of the inulin lauryl carbamate to the glycerol is 1:3.

[0030] In some embodiments, the anionic emulsifier is one or more of sodium stearoyl lactylate, sodium isostearyl lactylate, sodium stearoyl glutamate, potassium cetyl phosphate, sodium subtilisin, glyceryl stearate citrate, glyceryl oleate citrate, monoglyceride citrate, stearyl citrate, glyceryl citrate / lactate / linoleate / oleate, sodium laureth sulfate, sodium dodecylbenzene sulfonate, ammonium lauryl sulfate and sodium stearate.

[0031] In some embodiments, the co-emulsifier is a fatty alcohol co-emulsifier; the carbon number of the fatty alcohol co-emulsifier is greater than or equal to 12; the long carbon chain type with a carbon number of more than 12 can more effectively promote the close arrangement of the emulsifier at the oil-water interface, further stabilize the formation of the mosquito repellent emulsion, and also improve the stability of the mosquito repellent emulsion.

[0032] In a specific embodiment, the fatty alcohol emulsifier is one or more of cetyl alcohol, stearyl alcohol, cetearyl alcohol, arachidyl alcohol and behenyl alcohol.

[0033] In some embodiments, the thickener is carbomer, acrylic acid / C10-30 alkyl acrylate crosspolymer, acrylic acid esters / C10-30 alkyl acrylate crosspolymer, ammonium acryloyl dimethyl taurate / VP copolymer, sodium polyacryloyl dimethyl taurate, polyacrylate crosspolymer-6, ammonium acryloyl dimethyl taurate / behenyl alcohol polyether-25 methacrylate crosspolymer, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, sodium acrylate / acryloyl dimethyl taurate One or more of sodium methyl taurate copolymer, polyacrylamide, polyacrylate-13, acrylamide / sodium acryloyldimethyl taurate, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, carbomer, magnesium aluminum silicate, quaternium-90 bentonite, gellan gum, hydroxypropyl starch phosphate, acacia gum, tsara gum, xanthan gum, sclerotium gum, lemon peel powder, lime peel powder, crispy wave chondrus extract, hydroxypropyl methylcellulose, hydroxyethyl cellulose, cellulose gum, and microcrystalline cellulose.

[0034] In some embodiments, the pH adjuster includes one or more of citric acid, sodium citrate, sodium hydroxide, potassium hydroxide, arginine, tromethamine, and triethanolamine.

[0035] In some embodiments, the mosquito repellent composition further comprises one or more of the following components:

[0036] ①2%-10% moisturizer;

[0037] ②0.5%-5% skin feel regulator;

[0038] ③0.1%-5% soothing ingredients;

[0039] ④0.3%-0.8% preservatives;

[0040] ⑤The rest is water;

[0041] Wherein, % is the mass percentage of each component in the total mass of the mosquito repellent composition.

[0042] In a specific embodiment, the moisturizing agent is one or more of 1,3-propylene glycol, 1,2-propylene glycol, dipropylene glycol, glycerol, methyl propanediol, butylene glycol, pentylene glycol, sorbitol, polyglycerol-3, polyglycerol-4, polyglycerol-6, polyglycerol-10, polyethylene glycol-6, polyethylene glycol-7, polyethylene glycol-8, polyethylene glycol-32, glycine, and glutamic acid.

[0043] In a specific embodiment, the skin feel regulator includes inorganic powder and / or organic powder; preferably, the inorganic powder is one or more of silica, diatomaceous earth, kaolin, and perlite; the organic powder is one or more of polymethyl methacrylate, methyl methacrylate crosspolymer, vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosspolymer, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane crosspolymer, polymethylsilsesquioxane, HDI / trimethylol hexyllactone crosspolymer, lauroyl lysine, nylon-11, nylon-12, nylon-6, and polysilicone-11.

[0044] In the present invention, by adding soothing ingredients, the formula has an antipruritic effect.

[0045] In a specific embodiment, the soothing ingredient is one or more of Rosa centifolia flower extract, Rhizoma Cyperi flower extract, Bellis perennis flower extract, dipotassium glycyrrhizinate, Portulaca oleracea extract, Centella asiatica extract, Peucedanum peucedanum extract, Arugula leaf extract, Hops extract and dihydrooatmoyl anthranilic acid.

[0046] In the present invention, the antiseptic property of the formula can be effectively improved by adding a preservative.

[0047] In a specific embodiment, the preservative is one or more of phenoxyethanol, phenylpropanol, caprylhydroxamic acid, p-hydroxyacetophenone, DMDM ​​hydantoin, imidazolidinyl urea, polyaminopropyl biguanide, chlorphenesin, 4-hydroxybenzoic acid and its salts and esters, potassium sorbate, sodium benzoate, 1,2-pentanediol, 1,2-hexanediol, phenylethyl alcohol, phenylpropanol and caprylyl glycol.

[0048] The present invention provides a method for preparing a mosquito repellent emulsion, which uses the mosquito repellent composition as described above and comprises the following steps:

[0049] S1, mixing the first dispersion and the second dispersion at 70-90° C. to obtain a mixture;

[0050] In step S1, the preparation method of the first dispersion includes: first stirring picaridin, nonionic emulsifier, anionic emulsifier and co-emulsifier, and then performing a first homogenization process; the speed of the first homogenization is 3000-10000 rpm, and the time of the first homogenization is 2-20 min;

[0051] In step S1, the preparation method of the second dispersion includes: performing a second stirring on the moisturizer, the thickener and the water, and then performing a second homogenization process; the speed of the second homogenization process is 3000-10000 rpm, and the time of the second homogenization process is 2-10 min;

[0052] S2, mixing the mixture with a third material to obtain the mosquito repellent emulsion;

[0053] In step S2, the third material is one or more of a skin feel regulator, a soothing ingredient and a preservative;

[0054] In step S2, during the mixing process, a pH adjuster is used to adjust the pH value to 6.5-7.

[0055] In some embodiments, in step S1, the temperature of the first stirring is 70-90°C.

[0056] In some embodiments, in step S1, the rotation speed of the first stirring is 50-200 rpm.

[0057] In some embodiments, in step S1, the first stirring time is 30-60 min.

[0058] In some embodiments, in step S1, the temperature of the second stirring is 70-90°C.

[0059] In some embodiments, in step S1, the rotation speed of the second stirring is 100-600 rpm.

[0060] In some embodiments, in step S1, the second stirring time is 30-60 min.

[0061] In some embodiments, in step S2, the mixing temperature is 50°C.

[0062] In some embodiments, in step S2, the mixing speed is 100-600 rpm.

[0063] In some embodiments, in step S2, the mixing time is 10-60 min.

[0064] In one embodiment, the raw materials of the mosquito repellent emulsion include the mosquito repellent composition as described above, and the steps of the preparation method of the mosquito repellent emulsion are as follows:

[0065] 1) heating and stirring picaridin, nonionic emulsifier, anionic emulsifier and co-emulsifier at 70-90° C. to dissolve them, and then homogenizing to obtain a first dispersion; the stirring speed is 50-200 rpm, the stirring time is 30-60 min; the homogenizing speed is 3000-10000 rpm, and the homogenizing time is 2-20 min;

[0066] 2) heating and stirring the moisturizer, thickener and water at 70-90° C. to dissolve them, and then homogenizing to obtain a second dispersion; the stirring temperature is 70-90° C., the stirring speed is 100-600 rpm, and the stirring time is 30-60 min; the homogenizing speed is 3000-10000 rpm, and the homogenizing time is 2-10 min;

[0067] 3) slowly adding the first dispersion prepared in step 1) into the second dispersion prepared in step 2);

[0068] 4) placing the composition of step 3) under a stirrer, stirring and mixing at 100-600 rpm for 10-60 min, and when the temperature drops to 50° C., adding a third material; the third material is one or more of a skin feel regulator, a soothing ingredient and a preservative; and adjusting the pH value of the system to 6.5-7.

[0069] In step 3), "slowly adding" means adding the liquid in a linear manner or dropwise using a dropper.

[0070] The present invention also provides a mosquito repellent emulsion, which is prepared by the mosquito repellent emulsion preparation method as described above.

[0071] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0072] The reagents and raw materials used in the present invention are commercially available.

[0073] The positive and progressive effects of the present invention are:

[0074] (1) The mosquito repellent emulsion of the present invention has a high content of picaridin, is homogeneous, has a low viscosity, has good pH stability at different temperatures, and has a good mosquito repellent effect and skin feel; specifically, it has high stability under 45°C, 25°C, -15°C and cyclic conditions; and the mosquito repellent emulsion also has a good antipruritic effect.

[0075] (2) The preparation method of the mosquito repellent emulsion of the present invention is simple and easy to operate and produce. BRIEF DESCRIPTION OF THE DRAWINGS

[0076] Figure 1 This is a schematic diagram of the results of the high and low temperature stability summary of Examples 1-10.

[0077] Figure 2 This is a schematic diagram of the results of the high and low temperature stability summary of Examples 11-17.

[0078] Figure 3Schematic diagram of the results summarizing the high and low temperature stability of Examples 18-26 and Comparative Example 6.

[0079] Figure 4 This is a schematic diagram of the results of the high and low temperature stability summary of Examples 27-30.

[0080] Figure 5 This is the antipruritic effect of the mosquito repellent emulsions of Examples 22 and 27-30.

[0081] Figure 6 This is a schematic diagram of the results summarizing the high and low temperature stability of Examples 31-33.

[0082] Figure 7 This is a schematic diagram of the results of the high and low temperature stability summary of Comparative Example 7.

[0083] Figure 8 This is a schematic diagram of the results summarizing the high and low temperature stability of Examples 34-35.

[0084] Fig. 9 The viscosity test results of different embodiments and comparative examples are shown in FIG.

[0085] Fig.10 The pH values ​​of different embodiments and comparative examples at 45°C and 25°C.

[0086] Fig.11 The mosquito repellent effects of different embodiments and comparative examples are shown.

[0087] Fig.12 This is a comparison chart of the skin feel test of Example 22 and Comparative Example 6. DETAILED DESCRIPTION

[0088] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods in the following examples without specifying specific conditions are carried out according to conventional methods and conditions, or selected according to the product specifications.

[0089] Example 1

[0090] The present embodiment discloses a mosquito repellent composition, which contains 20% picaridin, 4% polyglycerol-4 isostearate as a nonionic emulsifier, 0.2% potassium cetyl phosphate and 0.3% sodium stearoyl glutamate as anionic emulsifiers, 1% cetearyl alcohol as a co-emulsifier, 5% glycerin as a moisturizer, 0.3% ammonium acryloyldimethyltaurate / VP copolymer as a thickener, 0.6% phenoxyethanol as a preservative, citric acid and sodium citrate as pH regulators, and is used to adjust the pH of the mosquito repellent composition to 6.5-7, and the remaining components are water; % is the mass percentage of each component in the total mass of the mosquito repellent composition.

[0091] This embodiment also provides a method for preparing a mosquito repellent emulsion, which comprises:

[0092] 1) According to the above ratio, picaridin, polyglyceryl-4 isostearate, glyceryl stearate citrate and cetearyl alcohol are heated and stirred at 85° C. to dissolve them, and then homogenized to obtain a first dispersion; the stirring speed is 100 rpm, the stirring time is 30 min; the homogenization speed is 6000 rpm, and the homogenization time is 5 min;

[0093] 2) According to the above ratio, glycerol, ammonium acryloyldimethyltaurate / VP copolymer and water are heated and stirred at 85° C. to dissolve them, and then homogenized to obtain a second dispersion; the stirring temperature is 85° C., the stirring speed is 300 rpm, and the stirring time is 40 min; the homogenization speed is 6000 rpm, and the homogenization time is 10 min;

[0094] 3) slowly adding the first dispersion prepared in step 1) dropwise into the second dispersion prepared in step 2) through a dropper to obtain a composition;

[0095] 4) placing the composition of step 3) under a stirrer, stirring at 100-600 rpm for 30 min, and when the temperature drops to 50° C., adding 0.6% preservative (phenoxyethanol), using citric acid and sodium citrate as pH adjusters, adjusting the pH value of the system to 6.5-7, and obtaining a mosquito repellent lotion.

[0096] The mosquito repellent compositions in Examples 1-17 and Comparative Examples 1-4 adopt a basic formula 1, and the basic formula is shown in Table 1, which summarizes the basic formula 1:

[0097] Table 1

[0098]

[0099] Among them, the mosquito repellent compositions of Examples 1-17 and Comparative Examples 1-4 all contain 20% picaridin, 1% cetearyl alcohol, 5% glycerin, 0.3% ammonium acryloyldimethyltaurate / VP copolymer, water, and 0.6% preservative; wherein citric acid and sodium citrate are added in appropriate amounts to adjust the pH value of the mosquito repellent composition to 6.5-7; wherein the types and amounts of nonionic emulsifiers and anionic emulsifiers are variables.

[0100] The nonionic emulsifier is selected from one or more of polyglyceryl-4 isostearate, glyceryl stearate (and) PEG-100 stearate, steareth-21, inulin lauryl carbamate (and) glycerin, and glycolipids; wherein "glyceryl stearate (and) PEG-100 stearate" refers to a mixture of glyceryl stearate and PEG-100 stearate; the mass ratio of glyceryl stearate (and) PEG-100 stearate is 1:1; the mass ratio of inulin lauryl carbamate (and) glycerin is 1:3.

[0101] The anionic emulsifier is one or more of potassium cetyl phosphate, glyceryl stearate citrate, and sodium stearoyl glutamate.

[0102] Examples 2-10 and Comparative Examples 1-2

[0103] Based on the basic formula 1 in Table 1, the formulas of the mosquito repellent compositions of Examples 2-10 and Comparative Examples 1-2 are different from that of Example 1, in which the nonionic emulsifier and the anionic emulsifier are adjusted. The preparation methods of these Examples and Comparative Examples are basically the same as that of Example 1, only involving the replacement of raw materials; Table 2 is the specific formula of Examples 2-10 and Comparative Examples 1-2.

[0104] Table 2

[0105]

[0106] The “blank” in the table means the content is “0”.

[0107] Effect Example 1

[0108] This effect example tests the physical and chemical properties and stability of the mosquito repellent lotions of Examples 1-10 and Comparative Examples 1-2. The stability test method includes a centrifugal stability test and a high and low temperature stability test, and the stability of the samples prepared in the examples and comparative examples is examined with reference to GB / T 29665--2013 "Skin Care Lotion" and QB / T 1857--2013 "Skin Care Cream".

[0109] 1) Centrifugal stability test (25°C)

[0110] The mosquito repellent emulsions of Examples 1-10 and Comparative Examples 1-2 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the emulsified state and centrifugal stability test results. Table 3 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 1-10 and Comparative Examples 1-2:

[0111] Table 3

[0112] Emulsified state Centrifugal stability Example 1 Uniform No abnormality Example 2 Uniform A small amount of oil on the upper layer Example 3 Uniform No abnormality Example 4 Uniform No abnormality Example 5 Uniform No abnormality Example 6 Uniform No abnormality Example 7 Uniform No abnormality Example 8 Uniform No abnormality Example 9 Uniform A small amount of oil on the upper layer Example 10 Uniform No abnormality Comparative Example 1 Oil from upper layer \ Comparative Example 2 Not emulsified \

[0113] As shown in Table 1, compared with Comparative Examples 1 and 2, Examples 1-10 can emulsify Picaridin. Therefore, a more uniform mosquito repellent lotion can be prepared by using non-ionic emulsifiers (such as glyceryl stearate (and) PEG-100 stearate, inulin lauryl carbamate (and) glycerin, etc.) in combination with anionic emulsifiers (such as potassium cetyl phosphate, sodium stearoyl glutamate, glyceryl stearate citrate), and the effect of the emulsion on mosquito repellent is shown. Excellent emulsifying properties.

[0114] 2) High and low temperature stability test

[0115] Under the temperature conditions of 45°C, 25°C, and -15°C, the time for the mosquito repellent emulsions of Examples 1-10 to maintain system stability was tested respectively. System stability means that the mosquito repellent emulsion remains uniform, and the mosquito repellent emulsion has no obvious stratification, oiling, water separation, or coarsening phenomenon;

[0116] The mosquito repellent emulsions of Examples 1-10 were tested for the number of cycles in which the system remained stable after several cycles; wherein a single cycle was: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0117] Figure 1 The figure is a schematic diagram of the results of the high and low temperature stability of Examples 1-10. Figure 1 It can be seen that the mosquito repellent emulsions of Examples 1-10 are stable at high or low temperatures. Among them, the mosquito repellent emulsions of Examples 5 and 6 have the best stability, which can be maintained for 3 months at 45°C, 25°C, and -15°C, and the number of cycles can reach 5 cycles.

[0118] Examples 11-17 and Comparative Examples 3-4

[0119] Based on the basic formula 1 in Table 1, the formulas of the mosquito repellent compositions of Examples 11-17 and Comparative Examples 3-4 are different from that of Example 1, in which the nonionic emulsifier and the anionic emulsifier are adjusted. The preparation methods of these Examples and Comparative Examples are basically the same as that of Example 1, only involving the replacement of raw materials; the specific formulas of Examples 11-17 and Comparative Examples 3-4 are shown in Table 4.

[0120] Table 4

[0121]

[0122] The “blank” in the table means the content is “0”.

[0123] Effect Example 2

[0124] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of Examples 11-17 and Comparative Examples 3-4. The stability test method is the same as that of Effect Example 1.

[0125] 1) Centrifugal stability test (25°C)

[0126] The mosquito repellent emulsions of Examples 11-17 and Comparative Examples 3-4 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the emulsified state and centrifugal stability. Table 5 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 11-17 and Comparative Examples 3-4.

[0127] Table 5

[0128] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 11 Uniform No abnormality Example 12 Uniform No abnormality Embodiment 13 Uniform No abnormality Embodiment 14 Uniform No abnormality Embodiment 15 Uniform No abnormality Example 16 Uniform No abnormality Embodiment 17 Uniform No abnormality <![CDATA[Comparative Example 3]]> The paste is thick <![CDATA[Comparative Example 4]]> Not emulsified

[0129] As shown in Table 5, compared with Comparative Example 4, the compounding systems of Examples 11-17 show The composite anionic emulsifier and composite nonionic emulsifier have excellent emulsification performance and will not affect the physical and chemical properties of the mosquito repellent emulsion. However, due to the relatively high content of anionic emulsifier in the formula of Comparative Example 3, the solubility in the formula system is relatively poor, resulting in the precipitation of crystals of the emulsifier, the rough appearance of the system, and the poor spreadability. Therefore, in order to make the system emulsification stability better, the nonionic emulsifier is added in the range of 1-5%, and the anionic emulsifier is added in the range of 0.1-4%.

[0130] 2) High and low temperature stability test

[0131] Under the temperature conditions of 45°C, 25°C, and -15°C, the time for the mosquito repellent emulsions of Examples 11-17 to maintain the stability of the system was tested respectively;

[0132] The mosquito repellent emulsions of Examples 11-17 were tested for the number of cycles in which the system remained stable after several cycles; wherein a single cycle was: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0133] Figure 2 The figure is a schematic diagram of the results of the high and low temperature stability of Examples 11-17. Figure 2 It can be seen that the mosquito repellent lotions of Examples 11-17 have better stability at high or low temperatures than Examples 1-4 and 7-10. The mosquito repellent lotions of Examples 11-17 can be kept for 3 months at 45°C, 25°C, and -15°C, and the number of cycles can reach 5 cycles.

[0134] Examples 18-26 and Comparative Examples 5-6

[0135] The mosquito repellent compositions in Examples 18-26 and Comparative Examples 5-6 adopt basic formula 2, and the basic formula is shown in Table 6, which summarizes the basic formula 2:

[0136] Table 6

[0137]

[0138] Among them, the mosquito repellent compositions of Examples 18-26 and Comparative Examples 5-6 all contain 20% of picaridin, 2% of glyceryl stearate (and) PEG-100 stearate (non-ionic emulsifier), the mass ratio of glyceryl stearate to PEG-100 stearate is 1:1; 0.5% of inulin lauryl carbamate (and) glycerol (non-ionic emulsifier), the mass ratio of inulin lauryl carbamate to glycerol is 1:3, 1% steareth-21 (non-ionic emulsifier), 1% sodium stearoyl glutamate (anionic emulsifier), 0.5% potassium cetyl phosphate (anionic emulsifier), 5% glycerin (humectant), water, 0.6% phenoxyethanol (preservative); citric acid and sodium citrate are added in appropriate amounts to adjust the pH value of the mosquito repellent composition to 6.5-7; wherein, the type and amount of the co-emulsifier and thickener are variables.

[0139] The auxiliary emulsifier is a fatty alcohol, which is cetearyl alcohol or behenyl alcohol.

[0140] The thickener is one of ammonium acryloyldimethyltaurate / VP copolymer, lemon peel powder (and) sclerotium gum (and) lemon peel powder, Chondrus crispus extract, and carbomer. When the thickener is a mixture of lemon peel powder (and) sclerotium gum (and) lemon peel powder, the mass ratio of lemon peel powder (and) sclerotium gum (and) lemon peel powder is 2:1:1.

[0141] Based on the basic formula 2 in Table 6, the formulas of the mosquito repellent compositions of Examples 18-26 and Comparative Examples 5-6 were adjusted, but their preparation methods were basically the same as that of Example 1, only involving the replacement of raw materials. Table 7 shows the specific formulas of Examples 18-26 and Comparative Examples 5-6:

[0142] Table 7

[0143]

[0144] The “blank” in the table means the content is “0”.

[0145] Effect Example 3

[0146] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of Examples 18-26 and Comparative Examples 5-6. The stability test method is the same as that of Effect Example 1.

[0147] 1) Centrifugal stability test (25°C)

[0148] The mosquito repellent emulsions of Examples 18-26 and Comparative Examples 5-6 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the emulsified state and centrifugal stability test results. Table 8 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 18-26 and Comparative Examples 5-6.

[0149] Table 8

[0150] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 18 Slightly higher viscosity, uniform No abnormality Embodiment 19 Uniform No abnormality Embodiment 20 Slightly higher viscosity, uniform No abnormality Embodiment 21 Uniform No abnormality Embodiment 22 Uniform No abnormality Embodiment 23 Uniform No abnormality Embodiment 24 Uniform No abnormality Embodiment 25 Uniform No abnormality Embodiment 26 Uniform No abnormality Comparative Example 5 Not emulsified / Comparative Example 6 High viscosity, uniform No abnormality

[0151] As shown in Table 8, Examples 18-26 can emulsify Picaridin. Since there is no auxiliary emulsifier in Comparative Example 5, a uniform effect cannot be achieved; although the mosquito repellent emulsion in Comparative Example 6 can achieve a uniform effect, it has a very high viscosity after emulsification because no thickener is added.

[0152] 2) High and low temperature stability test

[0153] Under the temperature conditions of 45°C, 25°C, and -15°C, the time for which the mosquito repellent emulsions of Examples 18-26 and Comparative Example 6 can still maintain the stability of the system is tested respectively, that is, the mosquito repellent emulsion remains uniform;

[0154] The mosquito repellent emulsions of Examples 18-26 and Comparative Example 6 were tested respectively to see how many cycles the system could still maintain stability after several cycles; wherein a single cycle was: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0155] Figure 3 The results of high and low temperature stability of Examples 18-26 and Comparative Example 6 are summarized in the figure. Figure 3 It can be seen that the mosquito repellent emulsions of Examples 18-26 are stable at high or low temperatures, and can be maintained for 3 months at 45°C, 25°C, and -15°C, and the number of cycles can reach 5 cycles. However, the mosquito repellent emulsion of Comparative Example 6 has poor high and low temperature stability, and can be maintained for 2 months at 45°C and 1 month at -15°C, and the number of cycles is only 2 cycles.

[0156] According to the effect embodiment, when the total amount of the co-emulsifier added to the mosquito repellent emulsion is 0.1-1% and the amount of the thickener added is 0.1-1.0%, a stable emulsion can be formed.

[0157] Examples 27-30

[0158] Examples 27-30 disclose mosquito repellent lotions, which study whether the introduction of soothing ingredients will affect the physicochemical properties and high and low temperature stability of the mosquito repellent lotions. The raw material formula is shown in Table 9, which is the formula of the mosquito repellent lotions of Examples 27-30.

[0159] Table 9

[0160]

[0161] The “blank” in the table means the content is “0”.

[0162] Among them, the mosquito repellent compositions of Examples 27-30 all contain 20% picaridin, 1% cetearyl alcohol (co-emulsifier), 2% glyceryl stearate (and) PEG-100 stearate (non-ionic emulsifier), the mass ratio of glyceryl stearate to PEG-100 stearate is 1:1; 0.5% inulin lauryl carbamate (and) glycerol (non-ionic emulsifier), the mass ratio of inulin lauryl carbamate to glycerol is 1:3; 1% steareth-21 (non-ionic emulsifier), 1% sodium stearoyl glutamate (anionic emulsifier), 0.5% potassium cetyl phosphate (anionic emulsifier), 5% glycerol, 0.3% ammonium acryloyldimethyltaurate / VP copolymer (thickener), water, 0.6% phenoxyethanol (preservative); citric acid and sodium citrate are added in appropriate amounts to adjust the pH value of the mosquito repellent composition to 6.5-7.

[0163] The soothing ingredient is one of Rosa centifolia flower extract (and) Herba Sophorae Flavescentis flower extract, Portulaca oleracea extract, Hops extract, and Centella asiatica extract; wherein the mass ratio of Rosa centifolia flower extract to Herba Sophorae Flavescentis flower extract is 1:1.

[0164] The preparation methods of these mosquito repellent emulsions are substantially the same as those of Example 1, except for the replacement of raw materials.

[0165] Effect Example 4

[0166] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of Examples 27-30. The test method of the stability is the same as that of Effect Example 1.

[0167] 1) Centrifugal stability test (25°C)

[0168] The mosquito repellent emulsions of Examples 27-30 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the emulsified state and centrifugal stability. Table 10 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 27-30.

[0169] Table 10

[0170] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 27 Uniform No abnormality Embodiment 28 Uniform No abnormality Embodiment 29 Uniform No abnormality Embodiment 30 Uniform No abnormality

[0171] It can be seen from Table 10 that the addition of soothing ingredients will not affect the physical and chemical properties of the mosquito repellent lotion of the present application.

[0172] 2) High and low temperature stability test

[0173] Under the temperature conditions of 45°C, 25°C, and -15°C, the time for which the mosquito repellent emulsions of Examples 27-30 can still maintain the stability of the system is tested respectively, that is, the mosquito repellent emulsions remain uniform;

[0174] The mosquito repellent emulsions of Examples 27-30 were tested for the number of cycles at which the system could remain stable after several cycles; wherein a single cycle was: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0175] Figure 4 The figure is a schematic diagram of the results of the high and low temperature stability of Examples 27-30. Figure 4 It can be seen that the mosquito repellent lotions of Examples 27-30 are stable under high or low temperature conditions, and can be maintained for 3 months at 45°C, 25°C, and -15°C, and the number of cycles can reach 5 cycles; the addition of soothing ingredients will not affect the high and low temperature stability of the mosquito repellent lotion of the present application.

[0176] 3) Antipruritic effect test

[0177] Test population for antipruritic effect: Those with positive lactic acid stinging reaction were selected as test volunteers; the number of test persons was 12.

[0178] The antipruritic effect test method includes the following steps:

[0179] s1. At room temperature, apply 50 μL of 10% lactic acid solution to the inner side of the arm. After 5 minutes, ask the subject about his / her subjective symptoms. If itching symptoms occur, follow-up experiments will be conducted.

[0180] s2. Select 5 areas on the inner side of the arm and apply 50 μL of lactic acid solution (10% aqueous solution) to each of them. After waiting for 5 minutes, apply 0.1 g of the mosquito repellent emulsion of Examples 22 and 27-30 to the 5 itchy areas respectively. Wait for 3 hours and ask the volunteers about their test experience.

[0181] s3. Scoring criteria: Ask the testers whether they have itching and record the number of people.

[0182] The antipruritic effect test method was used to test the antipruritic effect of the mosquito repellent emulsions of Examples 22 and 27-30, respectively. Figure 5 Table 11 is a comparison of the antipruritic effects of the mosquito repellent emulsions of Examples 22 and 27-30. Compared with Example 22, Examples 27-30 have better antipruritic effects.

[0183] Table 11

[0184] Number of people with itching No itching Antipruritic effect (%) Embodiment 22 1 11 8.33％ Embodiment 27 10 2 83.33％ Embodiment 28 9 3 75.00％ Embodiment 29 11 1 91.67％ Embodiment 30 10 2 83.33％

[0185] Examples 31-33

[0186] Examples 31-33 disclose mosquito repellent lotions, which investigate the The influence of different addition amounts on the emulsification system, and its raw material formula are shown in Table 12, which is the formula of the mosquito repellent emulsions of Examples 28 and 31-33 (Example 28 in the table is used for comparison).

[0187] Table 12

[0188]

[0189] Among them, the mosquito repellent compositions of Examples 31-33 all contain 1% cetearyl alcohol (co-emulsifier), 2% glyceryl stearate (and) PEG-100 stearate (non-ionic emulsifier), with a mass ratio of 1:1, 0.5% inulin lauryl carbamate (and) glycerol (non-ionic emulsifier), with a mass ratio of 1:3, 1% steareth-21 (non-ionic emulsifier), 1% sodium stearoyl glutamate (anionic emulsifier), 0.5% potassium cetyl phosphate (anionic emulsifier), 5% glycerol, 0.3% ammonium acryloyldimethyltaurate / VP copolymer (thickener), water, 0.6% phenoxyethanol (preservative), and 0.5% purslane extract (soothing ingredient); citric acid and sodium citrate are added in appropriate amounts to adjust the pH value of the mosquito repellent composition to 6.5-7.

[0190] The dosage of picaridin is 15%, 25% and 30% respectively.

[0191] The preparation methods of these mosquito repellent emulsions are substantially the same as those of Example 1, except for the replacement of raw materials.

[0192] Effect Example 5

[0193] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of Examples 31-33. The test method of the stability is the same as that of Effect Example 1.

[0194] 1) Centrifugal stability test (25°C)

[0195] The mosquito repellent emulsions of Examples 27-30 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the emulsified state and centrifugal stability. Table 13 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 28, 31-33.

[0196] Table 13

[0197] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 28 Uniform No abnormality Embodiment 31 Uniform No abnormality Embodiment 32 Uniform No abnormality Embodiment 33 Uniform No abnormality

[0198] As shown in Table 13, the formula of the mosquito repellent emulsion has a good emulsification effect on different amounts of picaridin, and the centrifugal stability of different amounts of picaridin is good. When the addition amount is 15-30%, a uniform emulsified system can be prepared.

[0199] 2) High and low temperature stability test

[0200] Under the temperature conditions of 45°C, 25°C, and -15°C, the time for which the mosquito repellent emulsions of Examples 31-33 can still maintain the stability of the system is tested respectively, that is, the mosquito repellent emulsions remain uniform;

[0201] The mosquito repellent emulsions of Examples 31-33 were tested respectively for the number of cycles at which the system could remain stable after several cycles; wherein a single cycle was: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0202] Figure 6 The figure is a schematic diagram of the results of the high and low temperature stability of Examples 31-33. Figure 6 It can be seen that the mosquito repellent emulsions of Examples 31-33 are stable under high or low temperature conditions, and can be maintained for 3 months at 45°C, 25°C, and -15°C, and the number of cycles can reach 5 cycles.

[0203] Picaridin It has high chemical polarity. When the amount of addition is high, it will greatly affect the emulsification effect, destroy the distribution of the emulsifier at the oil-water interface, and cause the system to break. Due to the combination of the anionic emulsifier and the nonionic emulsifier in the present application, the outer layer of the spherical micelles formed by the two in the system will have a diffuse double layer, which effectively prevents the aggregation of emulsion droplets, further reduces the surface tension between the emulsion droplets, and improves the stability of the emulsification system.

[0204] Comparative Example 7

[0205] This comparative example is a mosquito repellent spray, and its formula is a transparent aqueous system, which is used to compare the mosquito repellent effect, skin feel and stability with the examples. Table 14 is the mosquito repellent liquid formula of comparative example 7.

[0206] Table 14

[0207]

[0208] Effect Example 6

[0209] This effect example tests the physical and chemical properties and stability of the mosquito repellent liquid of comparative example 7. The test method of the stability is the same as that of effect example 1.

[0210] 1) Centrifugal stability test (25°C)

[0211] The mosquito repellent spray of comparative example 7 was centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the prepared state and centrifugal stability. Table 15 shows the physical and chemical properties of the mosquito repellent of comparative example 7.

[0212] Table 15

[0213] Physical and chemical properties Preparation status Centrifugal stability Comparative Example 7 Uniform No abnormality

[0214] Since this comparative example is a transparent aqueous system, it is homogeneous.

[0215] 2) High and low temperature stability test

[0216] The mosquito repellent liquid of Comparative Example 7 was tested at 45°C, 25°C, and -15°C;

[0217] The mosquito repellent liquid of comparative example 7 can still maintain the number of cycles of system stability after several cycles; among them, a single cycle is: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0218] Figure 7 The result diagram of the high and low temperature stability of comparative example 7 is summarized. The aqueous phase system has good high and low temperature stability.

[0219] Comparative Examples 8-9

[0220] Comparative Examples 8-9 are mosquito repellent lotions; Comparative Example 8 removes the anionic emulsifier in the system of Example 28; Compared with Example 28, Comparative Example 9 does not add citric acid or sodium citrate, but adds 0.2% disodium hydrogen phosphate as a pH buffer to compare the pH migration phenomenon. Table 16 is the mosquito repellent lotion formula of Comparative Examples 8-9.

[0221] Table 16

[0222]

[0223] The “blank” in the table means the content is “0”.

[0224] It can be seen from the above table that the formula of the mosquito repellent lotion in Comparative Example 8 is similar to that in Example 28, except that: the mosquito repellent lotion in Comparative Example 8 does not contain the anionic emulsifier (sodium stearoyl glutamate and potassium cetyl phosphate) in Example 28, and Comparative Example 9 uses disodium hydrogen phosphate instead of citric acid and sodium citrate for adjusting pH as a buffer; the other components in the formula are the same as those in Comparative Example 8.

[0225] The preparation methods of these mosquito repellent emulsions are substantially the same as those of Example 1, except for the replacement of raw materials.

[0226] Effect Example 7

[0227] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of comparative examples 8-9. The stability test method is the same as that of effect example 1.

[0228] 1) Centrifugal stability test (25°C)

[0229] The mosquito repellent emulsion of comparative example 8-9 was centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the emulsified state and centrifugal stability. Table 17 shows the physical and chemical properties of the mosquito repellent emulsion of comparative example 8-9.

[0230] Table 17

[0231] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 28 Uniform No abnormality Comparative Example 8 Oil \ Comparative Example 9 Not emulsified \

[0232] As can be seen from the above table, Comparative Example 8 removes the anionic emulsifier in the system of Example 28, and disodium hydrogen phosphate is used as a buffer in the formula of Comparative Example 9. The addition of this buffer will introduce a certain amount of ions, which seriously affects the stability of the formula and makes the mosquito repellent emulsion unable to achieve a uniform effect.

[0233] Examples 34-35 and Comparative Example 10

[0234] Examples 34-35 and Comparative Example 10 disclose a method for preparing a mosquito repellent emulsion, and the formula thereof is the same as that of Example 28; the process conditions are different from those of Example 28, and Table 18 is a comparison of the process conditions of Examples 34-35 and Comparative Example 10.

[0235] Table 18

[0236]

[0237]

[0238] Effect Example 8

[0239] This effect example tests the physical and chemical properties and stability of the mosquito repellent emulsions of Examples 34-35 and Comparative Example 10. The stability test method is the same as that of Effect Example 1.

[0240] 1) Centrifugal stability test (25°C)

[0241] The mosquito repellent emulsions of Examples 34-35 and Comparative Example 10 were centrifuged at a centrifugal speed of 2000 rpm and a centrifugal time of 30 min to obtain the test results of the emulsified state and centrifugal stability. Table 19 shows the physical and chemical properties of the mosquito repellent emulsions of Examples 34-35 and Comparative Example 10.

[0242] Table 19

[0243] Physical and chemical properties Emulsified state Centrifugal stability Embodiment 34 Uniform No abnormality Embodiment 35 Uniform No abnormality Comparative Example 10 Unemulsified, stratified \

[0244] It can be seen from the table that after adjusting the process steps, the mosquito repellent emulsion of Comparative Example 9 is not uniform.

[0245] 2) High and low temperature stability test

[0246] The mosquito repellent liquids of Examples 34-35 were tested at 45°C, 25°C, and -15°C;

[0247] The mosquito repellent liquid of test examples 34-35 can still maintain the number of cycles of system stability after several cycles; wherein, a single cycle is: 3 days at 45°C, 1 day at 25°C, and 3 days at -15°C.

[0248] Figure 8 The schematic diagram is a summary of the high and low temperature stability results of Examples 34-35. The preparation process of Examples 34-35 can prepare a mosquito repellent emulsion that is stable at high and low temperatures.

[0249] Effect Example 9

[0250] This effect example tests the viscosity of the mosquito repellent emulsions of Examples 11, 13-15, 18-20, 22, 28, 31-33 and Comparative Example 6. At 25° C., the viscosity of the mosquito repellent emulsions of the above examples and comparative examples was tested using an IKA viscometer.

[0251] Fig. 9 The viscosity test results of different embodiments and comparative examples are shown in FIG. Fig. 9 As shown, the viscosity of the mosquito repellent emulsion in Comparative Example 6 is significantly higher than that in Examples 11, 13-15, 18-20, 22, 28, and 31-33.

[0252] Effect Example 10

[0253] This effect example tests the pH values ​​of mosquito repellent lotions of Examples 5-6, 12, 18, 22, 28, 31-33 and Comparative Examples 1-2, 7-9 at different temperatures. The pH value test method is to place them at a high temperature of 45°C and a medium and low temperature of 25°C for 3 months respectively.

[0254] Fig.10 are the pH values ​​of different embodiments and comparative examples at 45°C and 25°C. Fig.10 As shown, the aqueous formulations of Comparative Example 7, Comparative Examples 1 and 8 (containing only nonionic emulsifiers and no anionic emulsifiers), and Comparative Example 2 (containing only anionic emulsifiers and no nonionic emulsifiers) have a significant increase in pH under high temperature conditions. This is because picaridin is prone to hydrolysis at high temperatures, resulting in a high pH value. In Comparative Example 9, a buffer was added, and there was no pH migration problem. However, the addition of the buffer disodium hydrogen phosphate would bring in a large amount of ions, seriously affecting the stability of the emulsified system.

[0255] Under high temperature conditions, the pH value of the formula in the example does not change significantly, which is mainly due to the compounding of non-ionic emulsifier and anionic emulsifier in the formula. The prepared emulsion droplets have excellent stability, which effectively hinders the contact between the oil phase component picaridin and the aqueous phase, avoids the hydrolysis of picaridin, further enhances the mosquito repellent effect of the product, and greatly improves the utilization rate of picaridin.

[0256] Effect Example 11

[0257] This effect example tests the mosquito repellent effects of the mosquito repellent emulsions of Examples 5-6, 12, 18, 22, 28, 31-33 and Comparative Examples 6-7.

[0258] The mosquito repellent effect test was carried out in accordance with GB / T 13917.9-2009 "Indoor efficacy test and evaluation of public health insecticides for pesticide registration Part 9: Repellents". Fig.11 The mosquito repellent effects of different embodiments and comparative examples are shown.

[0259] Depend on Fig.11 It can be seen that the mosquito repellent effect of Examples 5-6, 12, 18, 22, 28, 31-33 is significantly better than that of Comparative Examples 6 and 7, that is, the effective protection time of Examples 5-6, 12, 18, 22, 28, 31-33 is longer than that of Comparative Examples 6 and 7. Therefore, compared with the spray formulation and the high-viscosity emulsion, the low-viscosity emulsion formulation shows a better mosquito repellent effect, mainly because the low-viscosity emulsion formulation has a higher effective usage rate and forms a more uniform protective film after application, which is helpful Maximize mosquito repellent effect.

[0260] Effect Example 12

[0261] This effect example tests the skin feel comparison of the mosquito repellent lotion of Example 28 and the spray of Comparative Example 7.

[0262] Skin feel test population: Skin feel test volunteers, 6 people;

[0263] The skin feel test method includes the following steps: double-blind random comparison test, 6 volunteers compare and score each group. Product evaluation is performed on the back of the hand (a circle with a diameter of about 5 cm is the evaluation area), and the sample volume on the left and right sides is 50 μL each.

[0264] The volunteer scoring criteria are shown in Table 20 below:

[0265] Table 20

[0266]

[0267] Table 21 is a comparison of the skin feel effects of the mosquito repellent lotion of Example 28 and the spray of Comparative Example 7.

[0268] Table 21

[0269]

[0270] Fig.12 The figure is a comparison chart of the skin feel test of Example 22 and Comparative Example 6. Fig.12 As can be seen from Table 21, the low-viscosity mosquito repellent lotion prepared by this invention shows better absorbency and less sticky feeling during use compared with conventional mosquito repellent sprays; in the post-use stage, this type of mosquito repellent lotion has a lower residual feeling and effectively reduces the sticky feeling.

Claims

1. A mosquito repellent composition, characterized in that: It includes the following components: 15%-30% picaridin; 1%-5% nonionic emulsifier; the nonionic emulsifier is one or more of fatty alcohol polyether emulsifier, polyglycerol fatty acid ester emulsifier, sucrose fatty acid ester emulsifier, alkyl glycoside emulsifier, Tween emulsifier, Span emulsifier and fatty alcohol polyoxyethylene emulsifier; 0.1%-4% anionic emulsifier; the anionic emulsifier is one or more of amino acid emulsifier, carboxylate emulsifier, phosphate emulsifier, citrate emulsifier and fatty acid salt emulsifier; 0.1%-1.0% of co-emulsifier; 0.1%-1.0% thickener; A pH regulator, used to adjust the pH value of the mosquito repellent composition to 6.5-7; Wherein, % is the mass percentage of each component in the total mass of the mosquito repellent composition.

2. The mosquito repellent composition according to claim 1, characterized in that The mosquito repellent composition meets one or more of the following conditions: ① The content of picaridin is 15%, 20%, 25% or 30%; ② The content of the nonionic emulsifier is 3%-5%, preferably 3%, 4% or 5%; ③ The content of the anionic emulsifier is 0.1%-2%, preferably 0.1%, 0.5%, 1%, 1.5% or 2%; ④ The content of the auxiliary emulsifier is 0.1%, 0.5% or 1%; ⑤ The content of the thickener is 0.1%-0.5%, preferably 0.1% or 0.5%.

3. The mosquito repellent composition according to claim 1, characterized in that: The nonionic emulsifier is steareth-2, steareth-21, beheneth-25, sucrose polystearate, sorbitan stearate, polysorbate-60, sorbitan oleate, cocoyl glucoside, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, cetearyl olive oil ester, PEG-4 olive oil ester, cetearyl glucoside, sorbitan sesquioleate, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, triphenin PEG-20 esters, methyl glucoside. One or more of saccharide sesquistearate, PEG-20 methyl glucose sesquistearate, sucrose distearate, C20-22 alcohol phosphate, tribehenin PEG-20 esters, sucrose stearate, ceteareth-25, sorbitan olivate, inulin lauryl carbamate, glycolipids, glycerin, glycine soja seed extract, glyceryl stearate, PEG-100 stearate, polyglyceryl-10 laurate, polyglyceryl-4 isostearate, polyglyceryl-4 laurate and polyglyceryl-2 isostearate.

4. The mosquito repellent composition according to claim 1, characterized in that: The anionic emulsifier is one or more of sodium stearoyl lactylate, sodium isostearyl lactylate, sodium stearoyl glutamate, potassium cetyl phosphate, sodium subtilisin, glyceryl stearate citrate, glyceryl oleate citrate, monoglyceride citrate, stearyl citrate, glyceryl citrate / lactate / linoleate / oleate, sodium laureth sulfate, sodium dodecylbenzene sulfonate, ammonium lauryl sulfate and sodium stearate.

5. The mosquito repellent composition according to claim 1, characterized in that: The auxiliary emulsifier is a fatty alcohol auxiliary emulsifier, and the carbon number of the fatty alcohol auxiliary emulsifier is greater than or equal to 12; preferably, the fatty alcohol auxiliary emulsifier is one or more of cetyl alcohol, stearyl alcohol, cetearyl alcohol, arachidyl alcohol and behenyl alcohol; And / or, the thickener is carbomer, acrylic acid / C10-30 alkyl acrylate crosspolymer, acrylate / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyl taurate / VP copolymer, sodium polyacryloyldimethyl taurate, polyacrylate crosspolymer-6, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate crosspolymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, sodium acrylate / acryloyldimethyl taurate One or more of sodium sulfonate copolymer, polyacrylamide, polyacrylate-13, acrylamide / sodium acryloyldimethyl taurate, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, carbomer, magnesium aluminum silicate, quaternium-90 bentonite, gellan gum, hydroxypropyl starch phosphate, acacia gum, tsara gum, xanthan gum, sclerotium gum, lemon peel powder, lime peel powder, Chondrus crispus extract, hydroxypropyl methylcellulose, hydroxyethyl cellulose, cellulose gum, and microcrystalline cellulose; And / or, the pH adjuster includes one or more of citric acid, sodium citrate, sodium hydroxide, potassium hydroxide, arginine, tromethamine, and triethanolamine.

6. The mosquito repellent composition according to claim 1, characterized in that: The mosquito repellent composition further comprises one or more of the following components: ①2%-10% moisturizer; ②0.5%-5% skin feel regulator; ③0.1%-5% soothing ingredients; ④0.3%-0.8% preservatives; ⑤The rest is water; Wherein, % is the mass percentage of each component in the total mass of the mosquito repellent composition.

7. The mosquito repellent composition according to claim 6, characterized in that The mosquito repellent composition meets one or more of the following conditions: ① The moisturizing agent is one or more of 1,3-propylene glycol, 1,2-propylene glycol, dipropylene glycol, glycerol, methyl propanediol, butylene glycol, pentylene glycol, sorbitol, polyglycerol-3, polyglycerol-4, polyglycerol-6, polyglycerol-10, polyethylene glycol-6, polyethylene glycol-7, polyethylene glycol-8, polyethylene glycol-32, glycine, and glutamic acid; ② The skin feel regulator includes inorganic powder and / or organic powder; preferably, the inorganic powder is one or more of silica, diatomaceous earth, kaolin, and perlite; the organic powder is one or more of polymethyl methacrylate, methyl methacrylate crosspolymer, vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosspolymer, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane crosspolymer, polymethylsilsesquioxane, HDI / trimethylol hexyl lactone crosspolymer, lauroyl lysine, nylon-11, nylon-12, nylon-6, and polysilicone-11; ③ The soothing ingredients are one or more of Rosa centifolia flower extract, Bellis perennis flower extract, dipotassium glycyrrhizinate, Portulaca oleracea extract, Centella asiatica extract, Peucedanum peucedanum extract, Arugula leaf extract, Hops extract and dihydrooatmoyl anthranilic acid; ④ The preservative is one or more of phenoxyethanol, phenylpropanol, caprylhydroxamic acid, p-hydroxyacetophenone, DMDM ​​hydantoin, imidazolidinyl urea, polyaminopropyl biguanide, chlorphenesin, 4-hydroxybenzoic acid and its salts and esters, potassium sorbate, sodium benzoate, 1,2-pentanediol, 1,2-hexanediol, phenylethyl alcohol, phenylpropanol and caprylyl glycol.

8. A method for preparing a mosquito repellent emulsion, characterized in that: The method adopts the mosquito repellent composition according to any one of claims 1 to 7, and comprises the following steps: S1, mixing the first dispersion and the second dispersion at 70-90° C. to obtain a mixture; In step S1, the preparation method of the first dispersion includes: first stirring picaridin, nonionic emulsifier, anionic emulsifier and co-emulsifier, and then performing a first homogenization process; the speed of the first homogenization is 3000-10000 rpm, and the time of the first homogenization is 2-20 min; In step S1, the preparation method of the second dispersion includes: performing a second stirring on the moisturizer, the thickener and the water, and then performing a second homogenization process; the speed of the second homogenization process is 3000-10000 rpm, and the time of the second homogenization process is 2-10 min; S2, mixing the mixture with a third material to obtain the mosquito repellent emulsion; In step S2, the third material is one or more of a skin feel regulator, a soothing ingredient and a preservative; In step S2, during the mixing process, a pH adjuster is used to adjust the pH value to 6.5-7.

9. The method for preparing the mosquito repellent emulsion according to claim 8, characterized in that: The preparation method of the mosquito repellent emulsion meets one or more of the following conditions: ① In step S1, the first stirring temperature is 70-90°C, ② In step S1, the first stirring speed is 50-200 rpm, ③ In step S1, the first stirring time is 30-60 min; ④ In step S1, the second stirring temperature is 70-90°C; ⑤ In step S1, the second stirring speed is 100-600 rpm; ⑥ In step S1, the second stirring time is 30-60 min; ⑦ In step S2, the mixing temperature is 50°C; ⑧ In step S2, the mixing speed is 100-600 rpm; ⑨ In step S2, the mixing time is 10-60 minutes.

10. A mosquito repellent lotion, characterized in that: The mosquito repellent emulsion is prepared by the preparation method of the mosquito repellent emulsion as claimed in claim 8 or 9.

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