Whitening nano-emulsion and preparation method thereof

Abstract

The invention discloses a whitening nano-emulsion and a preparation method thereof, and relates to the technical field of cosmetics and skin care products. The whitening nano-emulsion is prepared from the following components in percentage by weight: 2.0 to 10.0 percent of an emulsifying agent, 4.0 to 10.0 percent of an emollient, 3.0 to 8.0 percent of glycerol, 3.0 to 8.0 percent of butanediol, 0.5 to 3.0 percent of nicotinamide, 1.0 to 3.0 percent of a Soulixian extract, 0.5 to 3.0 percent of ascorbyl tetraisopalmitate, 0.3 to 3.0 percent of hydrogenated lecithin, 0.1 to 2.0 percent of hydroxyethyl piperazine ethanesulfonic acid, 0.1 to 1.0 percent of SymSitive1609, 0.03 to 0.5 percent of a mulberry root extract, 0.03 to 1.0 percent of cerium oxide and the balance of water. The toothpaste is prepared from the following components in percentage by weight: 0.05 to 0.5 percent of tocopheryl acetate, 0.03 to 0.3 percent of stearyl glycyrrhetinic acid ester, 0.01 to 0.1 percent of poly gamma-sodium glutamate, 0.03 to 0.2 percent of EDTA (Ethylene Diamine Tetraacetic Acid) disodium, 0.2 to 1.0 percent of preservative, 0.01 to 0.1 percent of aromatic and the balance of water, wherein the total The prepared whitening nano-emulsion can solve the problems of excessive addition, difficult absorption and instability of active ingredients of cosmetics, can inhibit DPPH free radical activity, hydroxyl free radical activity and tyrosinase activity through the synergistic effect of all the components, achieves the effects of resisting oxidation, whitening, removing freckles, brightening skin and the like, and does not cause damage to the skin.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics and skin care products, and in particular to a whitening nanoemulsion and a preparation method thereof. Background Art

[0003] The whitening lotions on the market are basically O / W type, which are made of basic base materials, whitening ingredients and solvents dissolved, and then added to the emulsification. The whitening agent has strong ionicity, which will cause the product stability to be weak, and there will be phenomena such as stratification, discoloration and taste change; the functional ingredients can only stay on the surface of the skin and are difficult to be absorbed by the skin. However, as they evaporate over time, many whitening ingredients cannot effectively penetrate into the stratum corneum of the skin to exert their actual effects, wasting many whitening ingredients and failing to achieve the ideal whitening effect. At the same time, the whitening functional ingredients are easily inactivated due to their own instability in the external environment.

[0004] There are many whitening products on the market, but the ingredients used are mainly those controlled by traditional regulations, such as 4-butylresorcinol, phenylhexylresorcinol, ethylresorcinol, tranexamic acid, arbutin, etc.; there are also oxidizing ingredients such as 3-o-ethylascorbic acid, ascorbic acid (vitamin C), magnesium ascorbyl phosphate, sodium ascorbyl phosphate, etc. These ingredients are not very stable, easily oxidized and discolored in the product, and have disadvantages such as a short shelf life; there are also α-hydroxy acids and their salts and esters, salicylic acid, etc. that achieve whitening effects by stripping the stratum corneum, which are prone to cause skin sensitivity, contact dermatitis and other risk warnings; developing a safe and effective product under the premise of safety and efficacy innovation has good market prospects. Summary of the invention

[0005] The present invention provides a whitening nanoemulsion and a preparation method thereof, which can solve the above problems.

[0006] In order to solve the above problems, the technical solution adopted by the present invention is as follows:

[0007] In a first aspect, the present invention provides a whitening nanoemulsion, comprising the following components in weight percentage: 2.0-10.0% of emulsifier, 4.0-10.0% of emollient, 3.0-8.0% of glycerin, 3.0-8.0% of butylene glycol, 0.5-3.0% of niacinamide, 1.0-3.0% of sea daffodil extract, 0.5-3.0% of ascorbyl tetraisopalmitate, 0.3-3.0% of hydrogenated lecithin, 0.1- 2.0%, SymSitive 1609 0.1-1.0%, mulberry root extract 0.03-0.5%, cerium oxide 0.03-1.0%, tocopherol acetate 0.05-0.5%, stearyl glycyrrhetinate 0.03-0.3%, sodium poly-gamma-glutamate 0.01-0.1%, disodium EDTA 0.03-0.2%, preservatives 0.2-1.0%, fragrance 0.01-0.1%, water to 100%.

[0008] As a further description of the above technical solution, the emulsifier consists of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE and steareth-2.

[0009] As a further description of the above technical scheme, the emollient is a combination of one or more of isodecyl neopentanoate, neopentyl glycol dicaprylate / dicaprate, isononyl isononanoate, octyldodecanol, hydrogenated polyisobutene, myristyl lactate, isopentyl laurate, cetyl ricinoleate, decyl cocoate, squalane, and myristyl stearate.

[0010] As a further description of the above technical solution, the sea daffodil extract is mixed with the following components in weight percentage: 50.0-70.0% butanediol and 20.0-30.0% water. The preparation process of the sea daffodil extract includes the following steps:

[0011] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0012] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing in a 55-60° C. water bath rotary evaporator, extracting for 60-75 minutes, and filtering with an 800-mesh filter cloth to obtain an extract I;

[0013] 3) placing the filter residue obtained in step 2) and deionized water in a mass ratio of 1:5 into a 75-80° C. water bath rotary evaporator, adjusting the pH value to 4.5-5.0 with lactic acid, extracting for 60-75 minutes, and filtering with an 800-mesh filter cloth to obtain an extract II;

[0014] 4) mixing the filter residue obtained in step 3) with butanediol at a mass ratio of 1:10, placing the mixture in a 75-80° C. water bath rotary evaporator, extracting for 60-75 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract III;

[0015] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 80-85°C, evaporate for 120-150 minutes, and obtain extract IV with a compressed density of 1.0-1.05 g / ml;

[0016] 6) The extract IV obtained in step 5) was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0017] As a further description of the above technical solution, the SymSitive 1609 includes the following components in weight percentage: 60% 1,2-pentanediol and 40% 4-tert-butyl cyclohexanol.

[0018] As a further description of the above technical solution, the mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0019] As a further description of the above technical solution, the preservative is a combination of one or more of decyl glycol, caprylyl glycol, 1,2-hexanediol, p-hydroxyacetophenone, phenoxyethanol, caprylhydroxamic acid, glyceryl caprylate, ethylhexylglycerin, methylparaben, 1,2-pentanediol, phenylpropanol, phenethyl alcohol, raspberry ketone, and glyceryl caprylate / caprate.

[0020] In a second aspect, the present invention provides a method for preparing the whitening nanoemulsion according to the first aspect, comprising the following steps:

[0021] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0022] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0023] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0024] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0025] Group D: mulberry root extract, sea daffodil extract;

[0026] Group E: preservatives and fragrances;

[0027] 2) Add the raw materials of group A into an oil pan, stir and heat to 75-80° C. at a speed of 20-25 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0028] 3) Add the raw materials of group B into a water pot, stir and heat to 83-85°C at a speed of 20-25 r / min to obtain dissolved raw materials of group B for use;

[0029] 4) The dissolved raw materials of group B are pumped into the emulsifying pot by a -0.03-0.08Mpa vacuum pump, stirred at 30-35r / min and homogenized at 30-35HZ for 2-3 minutes, and the temperature is kept constant at 83-85°C. Then, the dissolved raw materials of group A are pumped into the emulsifying pot by a -0.03-0.05Mpa vacuum pump, stirred at 30-35r / min and homogenized at 40-45HZ for 5-8 minutes;

[0030] 5) Start cooling the material in the emulsifier, stirring at a speed of 30-35 r / min, and evacuating to -0.03 Mpa;

[0031] 6) Cool the contents of the emulsifier to 50-55°C, add the raw materials of group C into the emulsifier at a stirring speed of 30-35 r / min, and evacuate to -0.03 Mpa;

[0032] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at a speed of 30-35 r / min for 8-10 minutes until a white emulsion is obtained;

[0033] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at a speed of 30-35 r / min for 1 minute, and then stir for 8-10 minutes until a white emulsion is obtained;

[0034] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0035] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 1750-2000 bar, and the frequency to 50-60 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] 1) It can solve the problems of excessive addition, poor absorption and instability of active ingredients in cosmetics. Through the synergistic effect of various components, it can inhibit the activity of DPPH free radicals, hydroxyl free radicals and tyrosinase, and achieve the effects of anti-oxidation, whitening, freckle removal and brightening skin tone;

[0038] 2) Ascorbyl tetraisopalmitate is combined with mulberry root extract to effectively inhibit the activity of intracellular tyrosinase and melanin production, and reduce UV-induced cell / DNA damage, prevent lipid peroxidation and skin aging, promote collagen synthesis and whiten and lighten spots.

[0039] 3) The combination of sea daffodil extract and niacinamide works synergistically to effectively inhibit the synthesis and release of a-MSH and melanin, reduce the level of related receptors on the surface of melanocytes, block the communication between melanocytes and keratinocytes, inhibit the release and migration of melanin, reduce dark spots caused by pigmentation, purify skin color, and lighten spots.

[0040] 4) The synergistic effect of the combination of hydroxyethylpiperazine ethane sulfonic acid and cerium oxide can effectively remove DPPH free radicals and hydroxyl free radicals, enhance the skin's ability to resist skin oxidation and aging caused by environmental factors, improve skin tone, and make the skin shiny and translucent.

[0041] 5) Niacinamide and ascorbyl tetraisopalmitate work synergistically to effectively inhibit the activity of tyrosinase, reduce melanin deposition, brighten the skin, and lighten spots.

[0042] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the embodiments of the present invention are specifically cited below and described in detail as follows. DETAILED DESCRIPTION

[0043] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0044] The technical standards of the whitening nanoemulsion product prepared by the present invention are as follows:

[0045] Appearance: White flowable emulsion;

[0046] pH: 5.0-7.5

[0047] Centrifugal test: 2000r / min, 30min, no oil-water separation;

[0048] Stability (cold resistance): kept in a (-8±2)℃ refrigerator for 24 hours, there is no significant difference after returning to room temperature;

[0049] Stability (heat resistance): After being kept in a (40±1)℃ constant temperature box for 24 hours, there is no significant difference between the test results and those before the test after returning to room temperature;

[0050] Total colony count: <10CFU / g;

[0051] Mold and yeast: <10CFU / g;

[0052] Thermotolerant coliform bacteria: shall not be detected;

[0053] Staphylococcus aureus: shall not be detected;

[0054] Pseudomonas aeruginosa: shall not be detected;

[0055] Heavy metals (lead ≤ 10 mg / kg, mercury ≤ 1 mg / kg, arsenic ≤ 2 mg / kg, cadmium ≤ 5 mg / kg).

[0056] Example 1

[0057] The following weight percentages of components are used to prepare the whitening nanoemulsion in this embodiment:

[0058] Emulsifier 3.0%, emollient 6.5%, glycerin 3.0%, butylene glycol 4.0%, niacinamide 2.0%, sea daffodil extract 1.8%, ascorbyl tetraisopalmitate 1.0%, hydrogenated lecithin 0.5%, hydroxyethylpiperazine ethane sulfonic acid 1.0%, SymSitive 1609 0.5%, mulberry root extract 0.2%, cerium oxide 0.5%, tocopheryl acetate 0.3%, stearyl glycyrrhetinate 0.03%, sodium poly-gamma-glutamate 0.03%, disodium EDTA 0.05%, preservative 1.0%, fragrance 0.05%, water to 100%.

[0059] The emulsifier is composed of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE, and steareth-2 in a mass ratio of 2.0:0.5:3.0:0.1.

[0060] The emollient is isodecyl neopentanoate, isoamyl laurate, cetyl ricinoleate, and myristyl stearate, which are mixed and used in a mass ratio of 1:1:0.5:2.

[0061] The preservative is decanediol, caprylyl glycol, and 1,2-hexanediol mixed in a mass ratio of 0.1:0.1:1.

[0062] SymSitive 1609 includes the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

[0063] The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0064] The preparation process of the sea daffodil extract in this embodiment comprises the following steps:

[0065] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0066] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing the mixture in a 55° C. water bath rotary evaporator, extracting for 60 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract I;

[0067] 3) The filter residue obtained by preparing the extract I and deionized water were placed in a 75° C. water bath rotary evaporator at a mass ratio of 1:5, and the pH value was adjusted to 4.5 with lactic acid. After extraction for 60 minutes, the mixture was filtered with an 800-mesh filter cloth to obtain an extract II;

[0068] 4) The filter residue obtained by preparing the extract II was mixed with butanediol at a mass ratio of 1:10, and placed in a 75° C. water bath rotary evaporator. After extraction for 60 minutes, the mixture was filtered through an 800-mesh filter cloth to obtain an extract III;

[0069] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 80°C for 120 minutes, and obtain extract IV with a compressed density of 1.0 g / ml;

[0070] 6) The extract IV was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0071] The method for preparing the whitening nanoemulsion in this embodiment comprises the following steps:

[0072] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0073] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0074] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0075] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0076] Group D: mulberry root extract, sea daffodil extract;

[0077] Group E: preservatives and fragrances;

[0078] 2) Add the raw materials of group A into an oil pan, stir and heat to 75°C at a speed of 20 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0079] 3) Add the raw materials of group B into a water pot, stir and heat to 83°C at a speed of 20r / min to obtain dissolved raw materials of group B for use;

[0080] 4) The dissolved raw materials of group B are pumped into the emulsifying pot with a -0.03Mpa vacuum pump, stirred at 30r / min and homogenized at 30HZ for 2 minutes, and the temperature is kept constant at 83°C. Then, the dissolved raw materials of group A are pumped into the emulsifying pot with a -0.03Mpa vacuum pump, stirred at 30r / min and homogenized at 40HZ for 5 minutes;

[0081] 5) Start cooling the material in the emulsifier, stirring at 30 r / min, and evacuating to -0.03 Mpa;

[0082] 6) Cool the contents of the emulsifier to 50°C, add the raw materials of group C into the emulsifier at a stirring speed of 30 r / min, and evacuate to -0.03 Mpa;

[0083] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at 30 r / min for 8 minutes until a white emulsion is obtained;

[0084] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at 30 r / min for 1 minute, and then stir for 8 minutes until a white emulsion is obtained;

[0085] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0086] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 1750 bar, and the frequency to 50 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0087] Example 2

[0088] The following weight percentages of components are used to prepare the whitening nanoemulsion in this embodiment:

[0089] Emulsifier 2.0%, emollient 5.0%, glycerin 5.0%, butylene glycol 8.0%, niacinamide 0.5%, sea daffodil extract 1.5%, ascorbyl tetraisopalmitate 3.0%, hydrogenated lecithin 2.0%, hydroxyethylpiperazine ethane sulfonic acid 2.0%, SymSitive 1609 1.0%, mulberry root extract 0.35%, cerium oxide 0.3%, tocopheryl acetate 0.05%, stearyl glycyrrhetinate 0.05%, sodium poly-gamma-glutamate 0.01%, disodium EDTA 0.03%, preservative 0.80%, fragrance 0.01%, water to 100%.

[0090] The emulsifier is composed of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE, and steareth-2 in a mass ratio of 1.0:3.0:2.0:0.5.

[0091] The emollient is neopentyl glycol dicaprylate / dicaprate, isononyl isononanoate, and isoamyl laurate, which are mixed in a mass ratio of 1:2:1.

[0092] The preservatives are 1,2-hexanediol, p-hydroxyacetophenone and methylparaben, which are mixed in a mass ratio of 1:0.5:0.2.

[0093] SymSitive 1609 includes the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

[0094] The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0095] The preparation process of the sea daffodil extract in this embodiment comprises the following steps:

[0096] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0097] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing the mixture in a 58° C. water bath rotary evaporator, extracting for 68 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract I;

[0098] 3) The filter residue obtained by preparing the extract I and deionized water were placed in a 78° C. water bath rotary evaporator at a mass ratio of 1:5, and the pH value was adjusted to 4.7 with lactic acid. After extraction for 68 minutes, the mixture was filtered with an 800-mesh filter cloth to obtain an extract II;

[0099] 4) The filter residue obtained by preparing the extract II was mixed with butanediol at a mass ratio of 1:10, and placed in a 77° C. water bath rotary evaporator. After extraction for 67 minutes, the mixture was filtered through an 800-mesh filter cloth to obtain an extract III;

[0100] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 83°C, evaporate for 130 minutes, and obtain extract IV with a compressed density of 1.02 g / ml;

[0101] 6) The extract IV was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0102] The method for preparing the whitening nanoemulsion in this embodiment comprises the following steps:

[0103] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0104] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0105] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0106] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0107] Group D: mulberry root extract, sea daffodil extract;

[0108] Group E: preservatives and fragrances;

[0109] 2) Add the raw materials of group A into an oil pan, stir and heat to 77°C at a speed of 23 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0110] 3) Add the raw materials of group B into a water pot, stir and heat to 84°C at a speed of 23r / min to obtain dissolved raw materials of group B for use;

[0111] 4) The dissolved raw materials of group B were pumped into the emulsifying pot with a -0.05Mpa vacuum pump, stirred at 33r / min and homogenized at 33HZ for 2.5 minutes, and the temperature was kept constant at 84°C. Then, the dissolved raw materials of group A were pumped into the emulsifying pot with a -0.04Mpa vacuum pump, stirred at 34r / min and homogenized at 43HZ for 6 minutes;

[0112] 5) Start cooling the material in the emulsifier, stirring at 34r / min, and evacuating to -0.03Mpa;

[0113] 6) Cool the contents of the emulsifier to 53°C, add the raw materials of group C into the emulsifier at a stirring speed of 33 r / min, and evacuate to -0.03 Mpa;

[0114] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at 33 r / min for 9 minutes until a white emulsion is obtained;

[0115] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at 34 r / min for 1 minute, and then stir for 9 minutes until a white emulsion is obtained;

[0116] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0117] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 1900 bar, and the frequency to 55 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0118] Example 3

[0119] The following weight percentages of components are used to prepare the whitening nanoemulsion in this embodiment:

[0120] Emulsifier 10.0%, emollient 10.0%, glycerin 3.0%, butylene glycol 3.0%, niacinamide 1.0%, sea daffodil extract 2.0%, ascorbyl tetraisopalmitate 1.5%, hydrogenated lecithin 0.3%, hydroxyethylpiperazine ethane sulfonic acid 0.5%, SymSitive 1609 0.1%, mulberry root extract 0.03%, cerium oxide 0.1%, tocopheryl acetate 0.5%, stearyl glycyrrhetinate 0.3%, sodium poly-gamma-glutamate 0.02%, disodium EDTA 0.1%, preservative 0.5%, fragrance 0.08%, water to 100%.

[0121] The emulsifier is composed of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE, and steareth-2 in a mass ratio of 3.0:3.0:1.0:0.1.

[0122] The emollients are isodecyl neopentanoate, octyldodecanol, myristyl lactate, cetyl ricinoleate, and squalane, which are mixed and used in a mass ratio of 1:1:0.5:1.

[0123] The preservatives are decanediol, glyceryl caprylate, and raspberry ketone mixed in a mass ratio of 0.5:1:1.

[0124] SymSitive 1609 includes the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

[0125] The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0126] The preparation process of the sea daffodil extract in this embodiment comprises the following steps:

[0127] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0128] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing the mixture in a 60° C. water bath rotary evaporator, extracting for 75 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract I;

[0129] 3) The filter residue obtained by preparing the extract I and deionized water were placed in a water bath rotary evaporator at 80° C. in a mass ratio of 1:5, and the pH value was adjusted to 5.0 with lactic acid. After extraction for 75 minutes, the mixture was filtered with an 800-mesh filter cloth to obtain an extract II;

[0130] 4) The filter residue obtained by preparing the extract II was mixed with butanediol at a mass ratio of 1:10, and placed in a rotary evaporator in a water bath at 80° C., extracted for 75 minutes, and filtered with an 800-mesh filter cloth to obtain an extract III;

[0131] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 85°C, evaporate for 150 minutes, and obtain extract IV with a compressed density of 1.05 g / ml;

[0132] 6) The extract IV was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0133] The method for preparing the whitening nanoemulsion in this embodiment comprises the following steps:

[0134] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0135] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0136] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0137] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0138] Group D: mulberry root extract, sea daffodil extract;

[0139] Group E: preservatives and fragrances;

[0140] 2) Add the raw materials of group A into an oil pan, stir and heat to 80°C at a speed of 25 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0141] 3) Add the raw materials of group B into a water pot, stir and heat to 85°C at a speed of 25r / min to obtain dissolved raw materials of group B for use;

[0142] 4) The dissolved raw materials of group B are pumped into the emulsifying pot with a -0.08Mpa vacuum pump, stirred at 35r / min and homogenized at 35HZ for 3 minutes, and the temperature is kept constant at 85°C. Then, the dissolved raw materials of group A are pumped into the emulsifying pot with a -0.05Mpa vacuum pump, stirred at 35r / min and homogenized at 45HZ for 8 minutes;

[0143] 5) Start cooling the material in the emulsifier, stirring at 35 r / min, and evacuating to -0.03 Mpa;

[0144] 6) Cool the contents of the emulsifier to 55°C, add the raw materials of group C into the emulsifier at a stirring speed of 35 r / min, and evacuate to -0.03 Mpa;

[0145] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at 35 r / min for 10 minutes until a white emulsion is obtained;

[0146] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at 35 r / min for 1 minute, and then stir for 10 minutes until a white emulsion is obtained;

[0147] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0148] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 2000 bar, and the frequency to 60 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0149] Example 4

[0150] The following weight percentages of components are used to prepare the whitening nanoemulsion in this embodiment:

[0151] Emulsifier 5.0%, emollient 8.0%, glycerin 8.0%, butylene glycol 3.0%, niacinamide 3.0%, sea daffodil extract 1.0%, ascorbyl tetraisopalmitate 0.5%, hydrogenated lecithin 0.8%, hydroxyethylpiperazine ethane sulfonic acid 0.8%, SymSitive 1609 0.35%, mulberry root extract 0.45%, cerium oxide 0.03%, tocopheryl acetate 0.25%, stearyl glycyrrhetinate 0.15%, sodium poly-gamma-glutamate 0.08%, disodium EDTA 0.2%, preservative 0.2%, fragrance 0.1%, water to 100%.

[0152] The emulsifier is composed of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE, and steareth-2 in a mass ratio of 2.0:1.0:1.0:0.5.

[0153] The emollient is isononyl isononanoate, hydrogenated polyisobutene, cetyl ricinoleate, and decyl cocoate, which are mixed and used in a mass ratio of 2:1:1:1.

[0154] The preservatives are methylparaben and phenethyl alcohol mixed in a mass ratio of 1:1.

[0155] SymSitive 1609 includes the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

[0156] The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0157] The preparation process of the sea daffodil extract in this embodiment comprises the following steps:

[0158] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0159] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing the mixture in a 58° C. water bath rotary evaporator, extracting for 69 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract I;

[0160] 3) The filter residue obtained by preparing the extract I and deionized water were placed in a 79° C. water bath rotary evaporator at a mass ratio of 1:5, and the pH value was adjusted to 4.7 with lactic acid. After extraction for 70 minutes, the mixture was filtered with an 800-mesh filter cloth to obtain an extract II;

[0161] 4) The filter residue obtained by preparing the extract II was mixed with butanediol at a mass ratio of 1:10, and placed in a 79° C. water bath rotary evaporator. After extraction for 68 minutes, the mixture was filtered through an 800-mesh filter cloth to obtain an extract III;

[0162] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 84°C, evaporate for 140 minutes, and obtain extract IV with a compressed density of 1.04 g / ml;

[0163] 6) The extract IV was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0164] The method for preparing the whitening nanoemulsion in this embodiment comprises the following steps:

[0165] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0166] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0167] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0168] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0169] Group D: mulberry root extract, sea daffodil extract;

[0170] Group E: preservatives and fragrances;

[0171] 2) Add the raw materials of group A into the oil pan, stir and heat to 76°C at a speed of 24 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0172] 3) Add the raw materials of group B into a water pot, stir and heat to 84°C at a speed of 24r / min to obtain dissolved raw materials of group B for use;

[0173] 4) The dissolved raw materials of group B were pumped into the emulsifying pot with a -0.07Mpa vacuum pump, stirred at 34r / min and homogenized at 34HZ for 2.6 minutes, and the temperature was kept constant at 84°C. Then, the dissolved raw materials of group A were pumped into the emulsifying pot with a -0.04Mpa vacuum pump, stirred at 33r / min and homogenized at 43HZ for 7 minutes;

[0174] 5) Start cooling the material in the emulsifier, stirring at 34r / min, and evacuating to -0.03Mpa;

[0175] 6) Cool the contents of the emulsifier to 54°C, add the raw materials of group C into the emulsifier at a stirring speed of 34 r / min, and evacuate to -0.03 Mpa;

[0176] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at 34 rpm for 9 minutes until a white emulsion is obtained;

[0177] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at 30 r / min for 1 minute, and then stir for 10 minutes until a white emulsion is obtained;

[0178] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0179] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 1800 bar, and the frequency to 56 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0180] Example 5

[0181] The following weight percentages of components are used to prepare the whitening nanoemulsion in this embodiment:

[0182] Emulsifier 3.5%, emollient 4.0%, glycerin 6.0%, butylene glycol 5.0%, niacinamide 2.5%, sea daffodil extract 3.0%, ascorbyl tetraisopalmitate 0.8%, hydrogenated lecithin 3.0%, hydroxyethylpiperazine ethane sulfonic acid 0.1%, SymSitive 1609 0.75%, mulberry root extract 0.5%, cerium oxide 1.0%, tocopheryl acetate 0.2%, stearyl glycyrrhetinate 0.1%, sodium poly-gamma-glutamate 0.1%, disodium EDTA 0.15%, preservative 0.8%, fragrance 0.07%, water to 100%.

[0183] The emulsifier is composed of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE, and steareth-2 in a mass ratio of 3.0:0.1:3.0:0.1.

[0184] The emollient is isodecyl neopentanoate, isoamyl laurate, decyl cocoate, and myristyl stearate, which are mixed in a mass ratio of 1:1:1:2.

[0185] The preservative is 1,2-hexanediol and raspberry ketone mixed in a mass ratio of 1:1.

[0186] SymSitive 1609 includes the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

[0187] The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:1.

[0188] The preparation process of the sea daffodil extract in this embodiment comprises the following steps:

[0189] 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use;

[0190] 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing the mixture in a 60° C. water bath rotary evaporator, extracting for 75 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract I;

[0191] 3) The filter residue obtained by preparing the extract I and deionized water were placed in a water bath rotary evaporator at 80° C. in a mass ratio of 1:5, and the pH value was adjusted to 5.0 with lactic acid. After extraction for 75 minutes, the mixture was filtered with an 800-mesh filter cloth to obtain an extract II;

[0192] 4) The filter residue obtained by preparing the extract II was mixed with butanediol at a mass ratio of 1:10, and placed in a 75° C. water bath rotary evaporator. After extraction for 75 minutes, the mixture was filtered through an 800-mesh filter cloth to obtain an extract III;

[0193] 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 80°C for 150 minutes, and the compressed density is 1.0 g / ml, thereby obtaining extract IV;

[0194] 6) The extract IV was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

[0195] The method for preparing the whitening nanoemulsion in this embodiment comprises the following steps:

[0196] 1) Weigh each component and feed it separately. The specific sub-items are as follows:

[0197] Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate;

[0198] Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA;

[0199] Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609;

[0200] Group D: mulberry root extract, sea daffodil extract;

[0201] Group E: preservatives and fragrances;

[0202] 2) Add the raw materials of group A into an oil pan, stir and heat to 75°C at a speed of 25 r / min for later use, and obtain the dissolved raw materials of group A for later use;

[0203] 3) Add the raw materials of group B into a water pot, stir and heat to 83°C at a speed of 25r / min to obtain dissolved raw materials of group B for use;

[0204] 4) The dissolved raw materials of group B are pumped into the emulsifying pot with a -0.08Mpa vacuum pump, stirred at 30r / min and homogenized at 35HZ for 2 minutes, and the temperature is kept constant at 83°C. Then, the dissolved raw materials of group A are pumped into the emulsifying pot with a -0.05Mpa vacuum pump, stirred at 35r / min and homogenized at 40HZ for 8 minutes;

[0205] 5) Start cooling the material in the emulsifier, stirring at 30 r / min, and evacuating to -0.03 Mpa;

[0206] 6) Cool the contents of the emulsifier to 50°C, add the raw materials of group C into the emulsifier at a stirring speed of 35 r / min, and evacuate to -0.03 Mpa;

[0207] 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at 35 r / min for 8 minutes until a white emulsion is obtained;

[0208] 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at 35 r / min for 1 minute, and then stir for 10 minutes until a white emulsion is obtained;

[0209] 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use;

[0210] 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 2000 bar, and the frequency to 60 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

[0211] Comparative Example 1

[0212] Compared with Example 1, nicotinamide was replaced by ascorbyl tetraisopalmitate, and the contents of other components and the process remained unchanged.

[0213] Comparative Example 2

[0214] Compared with Example 1, cerium oxide is replaced by nicotinamide, and the contents of other components and the process remain unchanged.

[0215] Comparative Example 3

[0216] Compared with Example 1, nicotinamide was used to replace the mulberry root extract, and the contents of other components and the process remained unchanged.

[0217] Comparative Example 4

[0218] Compared with Example 1, the sea daffodil extract was replaced by deionized water, and the contents of other components and the process remained unchanged.

[0219] Comparative Example 5

[0220] Compared with Example 1, hydroxyethylpiperazineethanesulfonic acid was replaced by deionized water, and the component contents remained unchanged.

[0221] In order to demonstrate the advantages of the technical solution provided by the present invention, the experimental results of the technical solution provided by the present invention are given below:

[0222] 1.1. In vitro test - antioxidant effect test

[0223] 1.1.1. This test is divided into two parts. The first part detects the ability of the sample to scavenge free radicals (DPPH); the second part detects the ability of the sample to scavenge hydroxyl radicals, and comprehensively evaluates the antioxidant capacity of test examples 1-5 and comparative examples 1-5.

[0224] 1.1.2 Principle: 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) is a stable long-lived free radical. Its ethanol solution is dark purple and has strong absorption near 517nm. When there is a free radical scavenger, the light absorption of DPPH ethanol solution is weakened due to pairing with its single electron. The degree of fading of DPPH ethanol solution is linearly related to the number of electrons it accepts, which can be used to evaluate the ability of the test sample to scavenge free radicals, that is, the size of the antioxidant activity.

[0225] When pH=2-9, o-phenanthroline and Fe 2+ A stable orange complex is generated. 2+ It is a redox agent whose color change reflects the change of redox state in the solution. 2+ The system generates free radicals (·OH) and o-phenanthroline-Fe through the Fenton reaction. 2+ Fe in aqueous solution 2+ Oxidized by OH to Fe 3+ , resulting in o-phenanthroline-Fe 2+ The maximum absorption peak at 536 nm disappears, and the yield of ·OH in the system is obtained according to the absorbance change. Therefore, the ability of the sample to scavenge hydroxyl radicals can be reflected by measuring the absorbance value at 536 nm.

[0226] 1.1.3. DPPH free radical scavenging rate test

[0227] 1.1.3.1 Reagent preparation

[0228] Preparation of the test solution: dilute the whitening nanoemulsion with deionized water to a mass percentage concentration of 1.0%.

[0229] DPPH solution: dilute to 10 mg / L by adding anhydrous ethanol. Store at 0-5℃ away from light, use immediately after preparation, and it is valid within 24 hours.

[0230] 1.1.3.2 Experimental methods

[0231] Take 1.0 mL of the test solution and mix it with 2.0 mL of 10 mg / L DPPH solution to a total volume of 3 mL. The resulting solution is the sample group, and the measured absorbance is recorded as A1;

[0232] Take 1.0 mL of anhydrous ethanol and 2.0 mL of 10 mg / L DPPH solution and mix them to a total volume of 3 mL. The resulting solution is the blank control group, and the measured absorbance is recorded as A2;

[0233] Take 2.0mL of anhydrous ethanol and 1.0mL of the test solution and mix them evenly to a total volume of 3mL. The resulting solution is the negative control group, and the measured absorbance is recorded as A3.

[0234] After reacting for 30 min, take 1.0 ml and measure the absorbance of A1, A2 and A3 at 517 nm.

[0235] 1.1.3.3 Calculation formula:

[0236] The calculation formula of Clearance Rate (CR) is:

[0237]

[0238] Where:

[0239] A1—sample absorbance, i.e., the absorbance of the solution after the test solution reacts with DPPH;

[0240] A2—absorbance of blank control group, i.e. absorbance of the solution after the test solution reacts with anhydrous ethanol;

[0241] A3—absorbance of negative control group, i.e. absorbance of solution after reaction of anhydrous ethanol and DPPH;

[0242] 1.1.3.4 Test results

[0243] The test data results are shown in Table 1.

[0244] Table 1 Data results

[0245] Sample name Clearance rate (%, Mean ± SD) Example 1 60.80±2.35 Example 2 63.85±2.40 Example 3 58.15±2.30 Example 4 61.35±2.35 Example 5 64.55±2.40 Comparative Example 1 27.55±0.85 Comparative Example 2 31.25±0.85 Comparative Example 3 26.55±0.80 Comparative Example 4 32.25±0.85 Comparative Example 5 33.55±0.85

[0246] 1.1.3.5 Conclusion:

[0247] According to the test results in Table 1, Examples 1-5 have significant DPPH free radical scavenging ability, and the DPPH free radical scavenging rate is about 58.15%, while the ratio 1-5 is lower than 33.55%, indicating that Examples 1-5 have outstanding antioxidant activity, which can effectively improve the dull skin caused by oxidative damage and achieve the effect of whitening and brightening the skin.

[0248] 1.1.4 Hydroxyl free radical scavenging rate test

[0249] 1.1.4.1. Reagent configuration

[0250] Preparation of the test solution: dilute the whitening nanoemulsion with deionized water to a mass percentage concentration of 1.0%.

[0251] Prepare the following reagents: 0.01% H2O2 solution, 0.05 mol / L PBS phosphate buffer, 0.1% FeSO4·7H2O solution, and 0.1% o-phenanthroline solution.

[0252] 1.1.4.2、Test steps:

[0253] Take 0.5 ml of 0.1% o-phenanthroline solution in a test tube, add 1 ml PBS and 0.5 ml of the test solution in sequence, mix thoroughly, add 0.5 ml of 0.1% FeSO4·7H2O solution, mix again, add 0.5 ml of 0.01% H2O2 solution, incubate in a constant temperature water bath at 37°C for 50 minutes, and measure the absorbance at 536 nm; record it as T.

[0254] Take 0.5 ml of 0.1% o-phenanthroline solution in a test tube, add 1 ml PBS and 1.0 ml deionized water in sequence, mix thoroughly, add 0.5 ml 0.1% FeSO4·7H2O solution, incubate in a constant temperature water bath at 37°C for 50 minutes, and measure the absorbance at 536 nm; record it as C.

[0255] Take 0.5 ml of 0.1% o-phenanthroline solution in a test tube, add 1 ml PBS and 0.5 ml deionized water in sequence, mix thoroughly, add 0.5 ml 0.1% FeSO4·7H2O solution, mix again, add 0.5 ml 0.01% H2O2 solution, incubate in a constant temperature water bath at 37°C for 50 minutes, and measure the absorbance at 536 nm; record it as C0.

[0256] 1.1.4.3 Calculation formula

[0257]

[0258] 1.1.4.4 Test results

[0259] The test data results are shown in Table 2.

[0260] Table 2

[0261] Sample name Clearance rate (%, Mean ± SD) Example 1 65.50±1.50 Example 2 67.50±1.55 Example 3 63.15±1.37 Example 4 67.75±1.55 Example 5 70.35±1.65 Comparative Example 1 32.25±0.50 Comparative Example 2 33.65±0.58 Comparative Example 3 30.15±0.42 Comparative Example 4 33.35±0.49 Comparative Example 5 35.45±0.65

[0262] 1.1.5 Conclusion

[0263] According to the test results in Table 2, the scavenging rates of Examples 1-5 for hydroxyl radicals are about 63.15%, while those of Comparative Examples 1-5 are lower than 35.45%, indicating that Examples 1-5 have significant scavenging rates for hydroxyl radicals, can prevent and show outstanding antioxidant activity in environmental factors, can effectively improve skin damage and pigmentation caused by environmental factors, and achieve whitening effects.

[0264] 1.2. In vitro test - tyrosinase inhibition test

[0265] 1.2.1 Principle: Tyrosinase is the main rate-limiting enzyme in melanin synthesis, and its activity is closely related to the production of melanin. Therefore, the strength of tyrosinase inhibition is the main indicator for evaluating whitening cosmetics; tyrosinase and its substrate L-tyrosine can undergo catalytic reactions. When samples with tyrosinase activity inhibition are added to the experimental system, the catalytic reaction can be inhibited. The inhibition rate of the sample on tyrosinase activity is evaluated by measuring the absorbance at 475nm before and after adding the sample.

[0266] 1.2.2 Reagent preparation

[0267] Preparation of the test solution: dilute the whitening nano-microemulsion with PBS diluent to a mass percentage concentration of 1.0%.

[0268] L-Tyrosine (Chinese medicine) solution: diluted to 0.05% with PBS buffer.

[0269] Tyrosinase (sigma) solution: dilute with PBS buffer to 500 U / mL, aliquot, and store at -20°C to avoid secondary freezing and thawing.

[0270] 1.2.3 Experimental methods

[0271] Take 0.1 ml of the sample to be tested and mix with 1.0 ml of L-tyrosine solution, 1.0 ml of tyrosinase solution, and 0.9 ml of phosphate buffered saline (PBS) to a total volume of 3 ml, place at 25°C, incubate for 30 min, take 1.0 ml and measure the absorbance at 475 nm as A1;

[0272] Take 0.1 ml of the sample to be tested, mix it with 1.0 ml of L-tyrosine solution and 1.9 ml of phosphate buffered saline (PBS) to a total volume of 3 ml, place it at 25°C, incubate it for 30 min, take 1.0 ml and measure the absorbance at 475 nm as A2;

[0273] Take 1.0 mL of L-tyrosine solution, 1.0 mL of tyrosinase solution, and 1.0 mL of phosphate buffered saline (PBS), mix them to a total volume of 3 mL, place at 25°C, incubate for 30 min, take 1.0 mL and measure the absorbance at 475 nm as A3;

[0274] The reaction system was prepared according to Table 3, and the absorbance was measured at a wavelength of 475 nm. The inhibition of the test substance on tyrosinase activity was calculated based on the absorbance.

[0275] Table 3 Reaction system (ml)

[0276]

[0277]

[0278] 1.2.4 Calculation formula

[0279] The calculation formula of inhibition rate (IR) is:

[0280]

[0281] Where:

[0282] A1—sample absorbance, i.e., the absorbance of the solution after the test solution and tyrosinase solution;

[0283] A2—absorbance of blank control group, i.e. absorbance of the solution after the test solution reacts with L-tyrosine solution;

[0284] A3—Absorbance of negative control group, i.e. absorbance of the solution after the reaction of L-tyrosine solution and tyrosinase solution.

[0285] 1.2.5 Test results

[0286] The test data results are shown in Table 4

[0287] Table 4 Data results

[0288] Sample name Inhibition rate (%, Mean ± SD) Example 1 75.35±3.25 Example 2 77.85±3.30 Example 3 74.36±3.20 Example 4 76.40±3.25 Example 5 77.80±3.35 Comparative Example 1 54.35±2.65 Comparative Example 2 42.23±1.95 Comparative Example 3 33.40±1.55 Comparative Example 4 31.35±1.50 Comparative Example 5 35.25±1.55

[0289] 1.2.6 Conclusion:

[0290] The test results show that Examples 1-5 have a significant inhibitory effect on tyrosinase activity, with an inhibition rate of about 76.4%. After the ingredients in Comparative Examples 1-5 are replaced, the inhibition of tyrosinase activity is significantly reduced, indicating that the whitening nanoemulsions of Examples 1-5 of the present invention have a significant inhibitory effect on tyrosinase activity, that is, the whitening nanoemulsions of the present invention have a good whitening effect.

[0291] 1.3. Human body test - skin color test, skin gloss test

[0292] 1.3.1 Principle: The change of skin color is measured with reference to the colorimetric system (Lab colorimetric system) specified by the International Commission on Illumination (CIE). The Lab colorimetric system is used to represent the change of skin color. Among them: L* is brightness, a* is red-green color, and b* is blue-yellow color. The comprehensive evaluation of the three can reflect the change of skin color; the ITA° value is the skin individual type angle, which is a numerical value related to L* and b* that characterizes the brightness of the skin. The larger the ITA° value, the brighter the skin, and vice versa, the darker the skin. The glossiness of the skin is reflected by the direct reflection and scattering of light irradiated to the skin surface at an angle of 60°. Two sensors are used to receive the light directly reflected by the skin and the light scattered by the skin respectively. DSC (diffuse scattering correction value) is used to deduct the diffuse light to minimize the influence of skin color. The test results are expressed in glossiness values. The higher the glossiness value measured, the better the skin gloss.

[0293] 1.3.2 Test requirements

[0294] Volunteers: 50 (42 females, 8 males, aged 45-55 years old), healthy, no dropouts during the test.

[0295] Test site: flexed forearm

[0296] Testing period: 4 weeks

[0297] 1.3.3 Test Instruments

[0298] Skin color tester (Colorimeter CL400, CK, Germany)

[0299] Gloss analyzer (Glossymeter GL200, CK, Germany)

[0300] 1.3.4 Testing process

[0301] Divide 50 volunteers into 10 groups, with 5 people in each group.

[0302] A test area was demarcated on the flexor side of the forearm, and the whitening nanoemulsions of Examples 1-5 and Comparative Examples 1-5 were used according to the corresponding groups, respectively, and applied once in the morning and evening every day according to the normal product usage amount. Data on skin color changes and skin gloss changes were collected before use of the product and 1 week, 2 weeks, and 4 weeks after use.

[0303] 1.3.5 Calculation formula

[0304] Initial value: refers to the basic value when no product is used.

[0305] Mean Where x = individual parameter measurement value, n = number of valid data

[0306] Difference from initial value = xT使用后 -x T使用前

[0307] 1.3.6 Test Results

[0308] 1.3.6.1. The skin color test results before use, and after 1 week, 2 weeks, and 4 weeks of use are shown in Table 5.

[0309] Table 5 Average values ​​and statistical results of skin whitening ITA° before use, 1 week, 2 weeks, and 4 weeks after use, n=50

[0310]

[0311]

[0312] 1.3.6.2. The skin gloss test results before use, and after 1 week, 2 weeks, and 4 weeks of use are shown in Table 6.

[0313] Table 6 Average values ​​and statistical results of skin glossiness before use, after 1 week, 2 weeks and 4 weeks of use, n=50

[0314]

[0315]

[0316] 1.3.6.3 Conclusion

[0317] From the results in Table 5, it can be seen that compared with before use, the skin whitening ITA° value of the test area of ​​the sample group of Examples 1-5 gradually increases over time, and the difference between it and the initial value is greater than that of Comparative Examples 1-5 at each test time point. After 4 weeks of use, the skin color and brightness are significantly improved, indicating that the whitening nanoemulsions of Examples 1-5 of the present invention have significant whitening effects.

[0318] 1.3.6.4 Conclusion

[0319] From the results in Table 6, it can be seen that compared with before use, the skin glossiness of the test area of ​​the sample group of Examples 1-5 gradually increased, and the difference between the initial value and the sample group was greater than that of Comparative Examples 1-5 at each test time point, indicating that Examples 1-5 of the present invention have outstanding effects on increasing skin gloss.

[0320] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A whitening nanoemulsion, characterized in that: The invention comprises the following components in weight percentage: emulsifier 2.0-10.0%, emollient 4.0-10.0%, glycerin 3.0-8.0%, butylene glycol 3.0-8.0%, niacinamide 0.5-3.0%, sea daffodil extract 1.0-3.0%, ascorbyl tetraisopalmitate 0.5-3.0%, hydrogenated lecithin 0.3-3.0%, hydroxyethylpiperazine ethane sulfonic acid 0.1-2.0%, SymSi tive1609 0.1-1.0%, mulberry root extract 0.03-0.5%, cerium oxide 0.03-1.0%, tocopherol acetate 0.05-0.5%, stearyl glycyrrhetinate 0.03-0.3%, sodium poly-gamma-glutamate 0.01-0.1%, disodium EDTA 0.03-0.2%, preservatives 0.2-1.0%, fragrance 0.01-0.1%, water to 100%.

2. The whitening nanoemulsion according to claim 1, characterized in that The emulsifier consists of ceteareth-20, polyglyceryl-4 stearate, glyceryl stearate SE and steareth-2.

3. The whitening nanoemulsion according to claim 1, characterized in that The emollient is one or more of isodecyl neopentanoate, neopentyl glycol dicaprylate / dicaprate, isononyl isononanoate, octyldodecanol, hydrogenated polyisobutene, myristyl lactate, isopentyl laurate, cetyl ricinoleate, decyl cocoate, squalane, and myristyl stearate.

4. The whitening nanoemulsion according to claim 1, characterized in that The sea daffodil extract is mixed with the following components in weight percentage: 50.0-70.0% of butanediol and 20.0-30.0% of water. The preparation process of the sea daffodil extract includes the following steps: 1) Clean the whole plant of daffodil and grind it into a paste with a crusher for later use; 2) adding the muddy sea daffodils to 95% ethanol at a mass ratio of 1:10, placing in a 55-60° C. water bath rotary evaporator, extracting for 60-75 minutes, and filtering with an 800-mesh filter cloth to obtain an extract I; 3) placing the filter residue obtained in step 2) and deionized water in a mass ratio of 1:5 into a 75-80° C. water bath rotary evaporator, adjusting the pH value to 4.5-5.0 with lactic acid, extracting for 60-75 minutes, and filtering with an 800-mesh filter cloth to obtain an extract II; 4) mixing the filter residue obtained in step 3) with butanediol at a mass ratio of 1:10, placing the mixture in a 75-80° C. water bath rotary evaporator, extracting for 60-75 minutes, and filtering the mixture with an 800-mesh filter cloth to obtain an extract III; 5) Combine extracts I, II and III, add the remaining butanediol, put into a rotary evaporator at 80-85°C, evaporate for 120-150 minutes, and obtain extract IV with a compressed density of 1.0-1.05 g / ml; 6) The extract IV obtained in step 5) was placed in a high-pressure microfluidizer at a pressure of 20,000 psi, circulated and homogenized for 3 times, and filtered through a 0.45 um PES filter sand core filtration device to obtain the sea daffodil extract.

5. The whitening nanoemulsion according to claim 1, characterized in that The SymSitive 1609 comprises the following components in weight percentage: 60% of 1,2-pentanediol and 40% of 4-tert-butyl cyclohexanol.

6. The whitening nanoemulsion according to claim 1, characterized in that The mulberry root extract is mixed with hydroxypropyl cyclodextrin, and the hydroxypropyl cyclodextrin and the mulberry root extract are mixed in a mass ratio of 1:

1.

7. The whitening nanoemulsion according to claim 1, characterized in that: The preservative is one or more of decanediol, caprylyl glycol, 1,2-hexanediol, p-hydroxyacetophenone, phenoxyethanol, caprylhydroxamic acid, glyceryl caprylate, ethylhexylglycerin, methylparaben, 1,2-pentanediol, phenylpropanol, phenethyl alcohol, raspberry ketone, glyceryl caprylate / caprate and used in combination.

8. The method for preparing the whitening nanoemulsion according to any one of claims 1 to 7, characterized in that: The steps include: 1) Weigh each component and feed it separately. The specific sub-items are as follows: Group A: emulsifiers, emollients, ascorbyl tetraisopalmitate, cerium oxide, stearyl glycyrrhetinate, tocopheryl acetate; Group B: water, glycerin, butylene glycol, hydrogenated lecithin, sodium poly-gamma-glutamate, disodium EDTA; Group C: niacinamide, hydroxyethylpiperazineethane sulfonic acid, SymSitive1609; Group D: mulberry root extract, sea daffodil extract; Group E: preservatives and fragrances; 2) Add the raw materials of group A into an oil pan, stir and heat to 75-80° C. at a speed of 20-25 r / min for later use, and obtain the dissolved raw materials of group A for later use; 3) Add the raw materials of group B into a water pot, stir and heat to 83-85°C at a speed of 20-25 r / min to obtain dissolved raw materials of group B for use; 4) The dissolved raw materials of group B are pumped into the emulsifying pot by a -0.03-0.08Mpa vacuum pump, stirred at 30-35r / min and homogenized at 30-35HZ for 2-3 minutes, and the temperature is kept constant at 83-85°C. Then, the dissolved raw materials of group A are pumped into the emulsifying pot by a -0.03-0.05Mpa vacuum pump, stirred at 30-35r / min and homogenized at 40-45HZ for 5-8 minutes; 5) Start cooling the material in the emulsifier, stirring at a speed of 30-35 r / min, and evacuating to -0.03 Mpa; 6) Cool the contents of the emulsifier to 50-55°C, add the raw materials of group C into the emulsifier at a stirring speed of 30-35 r / min, and evacuate to -0.03 Mpa; 7) Cool the contents of the emulsifier to below 45°C, add the raw materials of group D into the emulsifier in order, and stir at a speed of 30-35 r / min for 8-10 minutes until a white emulsion is obtained; 8) Add the raw materials of group E into the emulsifying pot, stir and homogenize at a speed of 30-35 r / min for 1 minute, and then stir for 8-10 minutes until a white emulsion is obtained; 9) After the physical and chemical indicators of the emulsion in the emulsification pot are tested to be qualified, filter and discharge the material for standby use; 10) Turn on the low-temperature cooling circulation pump of the high-pressure homogenizer, adjust the temperature to 4°C for circulation, adjust the working pressure to 1750-2000 bar, and the frequency to 50-60 Hz. Then add the emulsion obtained in step 9) into the high-pressure homogenizer and circulate and homogenize 3 times to obtain a whitening nanoemulsion.

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