Zanthoxylum bungeanum seed essential oil and its use in cosmetics

Abstract

The present invention relates to the technical field of cosmetics, and in particular to prickly ash seed essential oil and its use in cosmetics. The present invention peels dried prickly ash fruit, adds cellulase and pectinase for enzymolysis, and increases the dissolution efficiency of active ingredients in the extract; uses papain and bromelain for further enzymolysis, and increases the types and concentrations of active ingredients such as antioxidants; then adds anhydrous ethanol for further extraction, and increases the active ingredients and quality of the essential oil; uses filtration and ultrafiltration for impurity removal and enrichment of active ingredients; and then uses a composite extractant for extraction to prepare prickly ash seed essential oil. The prickly ash seed essential oil prepared by the present invention has excellent antioxidant effect and can effectively remove DPPH free radicals.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to prickly ash seed essential oil and application thereof in cosmetics. Background Art

[0002] Sichuan pepper seed essential oil is a natural oily liquid extracted from Sichuan pepper seeds. It is rich in unsaturated fatty acids and essential fatty acids, such as linoleic acid and linolenic acid, which are beneficial to human health and provide natural skin care ingredients for cosmetics. The application of Sichuan pepper seed essential oil is not limited to skin care products, but also includes shower gels, facial masks and other forms, which can provide consumers with a natural and healthy skin care experience. These products use the natural properties of Sichuan pepper seed essential oil to provide consumers with a new and healthy way to skin care. For example, the antioxidant ingredients in Sichuan pepper seed essential oil can help protect the skin from free radical damage, while its antibacterial and anti-inflammatory properties can help reduce skin inflammation and promote skin health.

[0003] ‌Mulberry root extract is used in cosmetics mainly through its antioxidant and soothing anti-allergic properties, as well as reducing the irritation of salicylic acid to the skin. ‌Mulberry root extract is rich in antioxidant ingredients, which can help neutralize free radicals and protect skin cells from oxidative stress, thereby delaying skin aging and maintaining skin health. Mulberry root extract has a soothing effect and can reduce skin sensitivity and discomfort. For sensitive skin, it can provide additional comfort and reduce skin irritation caused by the use of cosmetics.

[0004] There are many methods for extracting Zanthoxylum bungeanum essential oil, and the effects of the obtained Zanthoxylum bungeanum essential oil are uneven; therefore, providing an extraction process for Zanthoxylum bungeanum essential oil to optimize the effects of Zanthoxylum bungeanum essential oil and apply the essential oil to cosmetics with antioxidant and other effects is one of the technical problems that need to be solved at present. Summary of the invention

[0005] In view of the above technical problems, the inventors proposed the technical solution of the present invention, which includes Zanthoxylum bungeanum seed essential oil and its use in cosmetics.

[0006] The invention comprises the following steps: peeling dried Zanthoxylum bungeanum fruit, adding cellulase and pectinase for enzymolysis, thereby increasing the dissolution efficiency of active components in the extract; then using papain and bromelain for further enzymolysis, thereby increasing the types and concentrations of active components such as antioxidants; then adding anhydrous ethanol for further extraction, thereby increasing the active components and quality of essential oil; then using filtration and ultrafiltration for impurity removal and enrichment of active components; and then using a composite extractant for extraction, thereby obtaining Zanthoxylum bungeanum seed essential oil with excellent antioxidant effect.

[0007] On the one hand, the present invention provides a Zanthoxylum bungeanum seed essential oil, and the preparation of the Zanthoxylum bungeanum seed essential oil comprises the following steps:

[0008] Step 1: peel, wash and crush the dried Zanthoxylum bungeanum to obtain a crushed product;

[0009] Step 2: Add 10-30 times the mass of water, cellulase and pectinase to the crushed material, heat to 30-40°C, stir and enzymolyze for 2-5 hours, then inactivate the enzyme to obtain the first enzymolysis product;

[0010] Step 3: Inactivate the enzyme in the first enzymatic hydrolysis product, add papain and bromelain, heat to 28-38°C, stir and enzymatically hydrolyze for 3-6 hours, then inactivate the enzyme to obtain the second enzymatic hydrolysis product;

[0011] Step 4: adding anhydrous ethanol to the second enzymatic hydrolysis product, heating to 50-60° C. and stirring for 4-8 hours to obtain an extract; wherein the mass of the anhydrous ethanol is 1-3 times the mass of the water in step 2;

[0012] Step 5: filtering the extract using a filter membrane with a pore size of 0.1-10 microns, and ultrafiltering the filtrate using an ultrafiltration membrane with a molecular weight cutoff of less than 500 Da to obtain an ultrafiltrate;

[0013] Step 6: Concentrate the ultrafiltrate to 10-20% of the mass of the ultrafiltrate to obtain a concentrated material, then add an extractant composed of an aqueous phase and an oil phase solvent, extract, then pour out the aqueous phase material and concentrate under reduced pressure to obtain the Zanthoxylum bungeanum seed essential oil.

[0014] Furthermore, the powder is crushed to a particle size of less than 0.5 mm.

[0015] Furthermore, the total mass of cellulase and pectinase is 5-10% of the mass of the pulverized material.

[0016] Furthermore, the mass ratio of cellulase to pectinase is 1-3:1.

[0017] Furthermore, the total mass of papain and bromelain is 4-12% of the mass of the pulverized material.

[0018] Furthermore, the mass ratio of papain to bromelain is 1:2-3.

[0019] Furthermore, in step 4, the mass of anhydrous ethanol is 1.2-3 times the mass of water in step 2.

[0020] Furthermore, the aqueous phase is a calcium chloride aqueous solution with a mass concentration of 1.2-2.5%.

[0021] Furthermore, the oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 2-5:1.

[0022] Furthermore, the mass ratio of the water phase to the oil phase is 1:2.5-4.

[0023] Furthermore, the mass ratio of the concentrated material to the extractant is 1:5-20.

[0024] Furthermore, the extraction temperature is 30-50°C and the extraction time is 2-10 hours.

[0025] Furthermore, in step 6, the reduced pressure concentration is carried out by distillation under reduced pressure, the temperature of the reduced pressure concentration is 50-55° C., and the reduced pressure concentration is carried out until no oil phase solvent is detected.

[0026] On the other hand, the present invention also provides a use of the above-mentioned Zanthoxylum bungeanum seed essential oil in cosmetics, wherein the mass content of the Zanthoxylum bungeanum seed essential oil in the cosmetics is 0.05-1%.

[0027] The use of Zanthoxylum bungeanum seed essential oil in the above-mentioned cosmetics makes the cosmetics have a certain antioxidant effect; at the same time, in order to further enhance the antioxidant effect of the cosmetics, you can also choose to add Morus alba root extract to the cosmetics.

[0028] Furthermore, the cosmetics also contain 0.04-0.8% of the mass of the cosmetics Morus alba root extract. The combination of Zanthoxylum bungeanum seed essential oil and Morus alba root extract in cosmetics can enrich the types and concentrations of antioxidant active factors in cosmetics and enhance the antioxidant effect of cosmetics.

[0029] Furthermore, in order to enhance the antioxidant effect of cosmetics, the mass ratio of the Zanthoxylum bungeanum seed essential oil to the Morus alba root extract is 1:0.6-1.

[0030] Furthermore, in order to enhance the antioxidant effect of the mulberry root extract, the present invention provides a method for preparing the mulberry root extract, which comprises the following steps:

[0031] Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder;

[0032] Step II: mixing the powder with 30-55 wt % ethanol aqueous solution at a mass ratio of 1:10-30, heating to 50-62° C. and stirring for 4-10 hours to obtain an extract;

[0033] Step III: filtering the extract using a filter membrane with a pore size of 2 microns, ultrafiltering the filtrate using an ultrafiltration membrane with a molecular weight cutoff lower than 800Da, and freeze-drying the filtrate to obtain the mulberry root extract.

[0034] Beneficial effects of the present invention:

[0035] The invention comprises the following steps: peeling dried Zanthoxylum bungeanum fruit, adding cellulase and pectinase for enzymolysis, thereby increasing the dissolution efficiency of active components in the extract; then using papain and bromelain for further enzymolysis, thereby increasing the types and concentrations of active components such as antioxidants; then adding anhydrous ethanol for further extraction, thereby increasing the active components and quality of essential oil; then using filtration and ultrafiltration for impurity removal and enrichment of active components; and then using a composite extractant for extraction, thereby obtaining Zanthoxylum bungeanum seed essential oil with excellent antioxidant effect.

[0036] The Zanthoxylum bungeanum seed essential oil prepared by the invention has good free radical scavenging effect and anti-aging performance.

[0037] The present invention uses two enzymatic hydrolysis processes, both of which promote the free radical scavenging effect of the Zanthoxylum bungeanum seed essential oil. In addition, papain and bromelain produce a compound effect, which mutually promotes the free radical scavenging effect of the essential oil.

[0038] The process of adding anhydrous ethanol to extract the ethanol aqueous solution can promote the extraction of antioxidant active ingredients; and when the amount of anhydrous ethanol added is 1.2-3 times the mass of water in step 2, the obtained essential oil extract has a better free radical scavenging effect.

[0039] The present invention further prepares essential oil by extracting with a composite extractant (an aqueous phase composed of an aqueous solution of calcium chloride and an oil phase composed of isohexane and ethyl acetate) after adding anhydrous ethanol for extraction, which can make the essential oil have a better free radical scavenging effect. The extraction effect of the extractant oil phase solvent composed of isohexane and ethyl acetate is better than that of single isohexane or ethyl acetate, and the combination of the two can improve the free radical scavenging efficiency of the essential oil. In particular, when isohexane and ethyl acetate form the oil phase solvent in a mass ratio of 2-5:1, the Zanthoxylum bungeanum seed essential oil obtained by the extraction process has a better effect.

[0040] The present invention adopts ultrafiltration with an ultrafiltration membrane having a molecular weight cut-off lower than 500Da, which can further enhance the free radical scavenging effect of the essential oil.

[0041] The mulberry root extract obtained by extraction with ethanol aqueous solution has a good free radical scavenging effect.

[0042] The invention adopts Zanthoxylum bungeanum seed essential oil and Morus alba root extract to have good DPPH free radical scavenging efficiency, and the two synergistically increase the DPPH free radical scavenging effect. The combination of the two in a dosage ratio of 1:0.6-1 has a better free radical scavenging effect.

[0043] Hypoallergenic and non-irritating cosmetics can be prepared by using the Zanthoxylum bungeanum seed essential oil and Morus alba root extract prepared by the invention. DETAILED DESCRIPTION

[0044] The present invention will be described below in conjunction with specific embodiments, and various effects of the present invention will be more clearly presented. It should be understood by those skilled in the art that these specific embodiments are used to illustrate the present invention, rather than to limit the present invention.

[0045] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

[0046] Cellulase: Cellulase R-10, 1,4-β-D-glucan glucoside hydrolase, 10u / mg, product number S10043-25g; Pectinase: Pectinase Y-23, 300000u / g, product number S10008-5g; Papain: 10u / mg, product number S27241-500g; Bromelain: 300u / mg, product number S10009-500g; all purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0047] 1. Preparation and testing of Zanthoxylum bungeanum seed essential oil

[0048] Zanthoxylum bungeanum seed essential oil 1:

[0049] The preparation method is as follows:

[0050] Step 1: peel the dried Zanthoxylum bungeanum fruit, wash it, and crush it to a particle size of less than 0.5 mm to obtain a crushed product;

[0051] Step 2: Add 20 times the mass of water, cellulase and pectinase to the crushed material, heat to 35°C, stir at 60rpm and perform enzymolysis for 4.2 hours, then inactivate the enzyme to obtain the first enzymolysis product;

[0052] Among them, the total mass of cellulase and pectinase is 6.9% of the mass of the crushed material; the mass ratio of cellulase to pectinase is 2:1;

[0053] Step 3: inactivate the enzyme in the first enzymatic hydrolysis product, add papain and bromelain, heat to 37°C, stir at 70 rpm and perform enzymolysis for 5 hours, then inactivate the enzyme to obtain the second enzymatic hydrolysis product;

[0054] Among them, the total mass of papain and bromelain is 10% of the mass of the crushed material; the mass ratio of papain to bromelain is 1:3;

[0055] Step 4: adding anhydrous ethanol to the second enzymatic hydrolysis product, heating to 56° C. and stirring for 5 hours to obtain an extract; wherein the mass of anhydrous ethanol is 2.5 times the mass of water in step 2;

[0056] Step 5: filtering the extract using a filter membrane with a pore size of 2 microns, and ultrafiltering the filtrate using an ultrafiltration membrane with a molecular weight cutoff of 400 Da to obtain an ultrafiltrate;

[0057] Step 6: Concentrate the ultrafiltrate to 12.7% of the mass of the ultrafiltrate to obtain a concentrated material, then add an extractant composed of an aqueous phase and an oil phase solvent, extract, then pour out the aqueous phase material and concentrate under reduced pressure to obtain the Zanthoxylum bungeanum seed essential oil;

[0058] Wherein, the aqueous phase is a calcium chloride aqueous solution with a mass concentration of 2.07%;

[0059] The oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 5:1;

[0060] The mass ratio of water phase to oil phase is 1:3.2;

[0061] The mass ratio of concentrated material to extractant is 1:15;

[0062] The extraction temperature was 42°C and the time was 4.7 hours;

[0063] The vacuum concentration was carried out by vacuum distillation at a temperature of 52° C., and the vacuum concentration was carried out until no oil phase solvent could be detected.

[0064] Zanthoxylum bungeanum seed essential oil 2:

[0065] The preparation method is as follows:

[0066] Step 1: peel the dried Zanthoxylum bungeanum fruit, wash it, and crush it to a particle size of less than 0.5 mm to obtain a crushed product;

[0067] Step 2: Add 17 times the mass of water, cellulase and pectinase to the crushed material, heat to 30°C, stir at 65rpm and perform enzymolysis for 5 hours, then inactivate the enzyme to obtain the first enzymolysis product;

[0068] Among them, the total mass of cellulase and pectinase is 8.4% of the mass of the crushed material; the mass ratio of cellulase to pectinase is 1:1;

[0069] Step 3: inactivate the enzyme in the first enzymatic hydrolysis product, add papain and bromelain, heat to 38°C, stir at 60rpm and perform enzymatic hydrolysis for 4.5 hours, then inactivate the enzyme to obtain the second enzymatic hydrolysis product;

[0070] Among them, the total mass of papain and bromelain is 8% of the mass of the crushed material; the mass ratio of papain to bromelain is 1:2;

[0071] Step 4: adding anhydrous ethanol to the second enzymatic hydrolysis product, heating to 52° C. and stirring for 4 hours to obtain an extract; wherein the mass of anhydrous ethanol is twice that of water in step 2;

[0072] Step 5: Filter the extract using a filter membrane with a pore size of 2 microns, and ultrafilter the filtrate using an ultrafiltration membrane with a molecular weight cutoff of 350 Da to obtain an ultrafiltrate;

[0073] Step 6: Concentrate the ultrafiltrate to 14.38% of the mass of the ultrafiltrate to obtain a concentrated material, then add an extractant composed of an aqueous phase and an oil phase solvent, extract, then pour out the aqueous phase material and concentrate under reduced pressure to obtain the Zanthoxylum bungeanum seed essential oil;

[0074] Wherein, the aqueous phase is a calcium chloride aqueous solution with a mass concentration of 1.48%;

[0075] The oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 2:1;

[0076] The mass ratio of water phase to oil phase is 1:4;

[0077] The mass ratio of concentrated material to extractant is 1:10;

[0078] The extraction temperature was 47°C and the time was 6.2 hours;

[0079] The vacuum concentration was carried out by vacuum distillation at a temperature of 54° C., and the vacuum concentration was carried out until no oil phase solvent could be detected.

[0080] Zanthoxylum bungeanum essential oil 3: Compared with Zanthoxylum bungeanum essential oil 1, the difference is: Step 2: add 20 times the mass of water to the crushed material, heat to 35°C, stir at 60rpm for 4.2 hours; the rest is the same as Zanthoxylum bungeanum essential oil 1.

[0081] Zanthoxylum bungeanum essential oil 4: Compared with Zanthoxylum bungeanum essential oil 1, step 3 is omitted; the rest is the same as that of Zanthoxylum bungeanum essential oil 1.

[0082] Zanthoxylum bungeanum essential oil 5: Compared with Zanthoxylum bungeanum essential oil 1, the enzyme used in step 3 is only papain, and its mass is 10% of the mass of the crushed substance; the rest are the same as those of Zanthoxylum bungeanum essential oil 1.

[0083] Zanthoxylum bungeanum essential oil 6: Compared with Zanthoxylum bungeanum essential oil 1, the enzyme used in step 3 is only bromelain, and its mass is 10% of the mass of the crushed substance; the rest are the same as those of Zanthoxylum bungeanum essential oil 1.

[0084] Zanthoxylum bungeanum essential oil 7: Compared with Zanthoxylum bungeanum essential oil 1, step 4 is omitted; the rest is the same as Zanthoxylum bungeanum essential oil 1.

[0085] Zanthoxylum bungeanum seed essential oil 8: Compared with Zanthoxylum bungeanum seed essential oil 1, in step 4, the mass of anhydrous ethanol is 5 times that of water in step 2; the rest is the same as that of Zanthoxylum bungeanum seed essential oil 1.

[0086] Zanthoxylum bungeanum seed essential oil 9: Compared with Zanthoxylum bungeanum seed essential oil 1, the extraction process in step 6 is omitted; the rest is the same as that of Zanthoxylum bungeanum seed essential oil 1.

[0087] Zanthoxylum bungeanum seed essential oil 10: Compared with Zanthoxylum bungeanum seed essential oil 1, in step 6, the oil phase solvent is only isohexane; the rest are the same as those of Zanthoxylum bungeanum seed essential oil 1.

[0088] Zanthoxylum bungeanum seed essential oil 11: Compared with Zanthoxylum bungeanum seed essential oil 1, in step 6, the oil phase solvent is only ethyl acetate; the rest are the same as those of Zanthoxylum bungeanum seed essential oil 1.

[0089] Zanthoxylum bungeanum seed essential oil 12: Compared with Zanthoxylum bungeanum seed essential oil 1, in step 6, the oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 0.5:1; the rest is the same as that of Zanthoxylum bungeanum seed essential oil 1.

[0090] Zanthoxylum bungeanum seed essential oil 13: Compared with Zanthoxylum bungeanum seed essential oil 1, in step 6, the oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 8:1; the rest is the same as that of Zanthoxylum bungeanum seed essential oil 1.

[0091] Zanthoxylum bungeanum essential oil 14: Compared with Zanthoxylum bungeanum essential oil 1, step 5 is omitted; the rest is the same as that of Zanthoxylum bungeanum essential oil 1.

[0092] The above-mentioned Zanthoxylum bungeanum seed essential oils 1-13 were diluted to a mass concentration of 0.25% using 50% mass concentration of ethanol aqueous solution, and then used as test samples to test the effect of scavenging DPPH free radicals.

[0093] The specific test method is: take 20μL of the test sample and 2mL of 120μmol / L DPPH free radical solution and mix them to obtain the test solution. Take the same volume of 50% ethanol aqueous solution instead of the test sample and mix it with 2mL of 120μmol / L DPPH free radical solution to obtain the control solution. Keep them away from light for half an hour, then measure the absorbance value A of the DPPH free radical mixed solution at 520nm and calculate the DPPH free radical scavenging efficiency K value of the test sample. Among them, the calculation formula of K value is 100%×(absorbance value A of control solution-absorbance value A of the test solution) / absorbance value A of control solution. The results are shown in Table 1.

[0094] Table 1: K value of scavenging DPPH free radical efficiency of Zanthoxylum bungeanum seed essential oil

[0095] Testing / 0.25% K value / % Zanthoxylum bungeanum seed essential oil1 63.23 Zanthoxylum bungeanum seed essential oil2 62.02 Zanthoxylum bungeanum seed essential oil3 58.67 Zanthoxylum bungeanum seed essential oil4 53.24 Zanthoxylum bungeanum seed essential oil5 58.56 Zanthoxylum bungeanum seed essential oil6 60.14 Zanthoxylum bungeanum seed essential oil7 42.73 Zanthoxylum bungeanum seed essential oil8 59.04 Zanthoxylum bungeanum seed essential oil9 38.95 Zanthoxylum bungeanum seed essential oil 10 56.23 Zanthoxylum bungeanum seed essential oil11 57.81 Zanthoxylum bungeanum seed essential oil 12 59.12 Zanthoxylum bungeanum seed essential oil 13 60.37 Zanthoxylum bungeanum seed essential oil 14 51.01

[0096] The test results in Table 1 show that the essential oil of Zanthoxylum bungeanum seed prepared by the present invention has a good free radical scavenging effect and anti-aging performance.

[0097] It can be seen from the test results of Zanthoxylum bungeanum seed essential oil 1, 3-4 that the present invention uses two enzymatic hydrolysis processes, both of which promote the free radical scavenging effect of Zanthoxylum bungeanum seed essential oil. Moreover, papain and bromelain produce a compounding effect, which mutually promotes the free radical scavenging effect of essential oils. The above content can be obtained in combination with the test results of Zanthoxylum bungeanum seed essential oil 1, 5-6; the reason for the analysis may be that papain and bromelain further enzymolysis improves the types and concentrations of active ingredients such as antioxidants in the extract, and the efficacy between the active ingredients produces a mutually complementary and promoting effect, which improves the free radical scavenging effect of the essential oil.

[0098] The present invention adopts a process of adding anhydrous ethanol to perform ethanol-water solution extraction in step 4, which can promote the extraction of antioxidant active ingredients, and the content can be obtained by comparing the test results of Zanthoxylum bungeanum seed essential oil 1 and 7; and the amount of anhydrous ethanol added in step 4 (1.2-3 times the mass of water in step 2) affects the concentration of the extraction solvent ethanol-water solution, thereby affecting the free radical scavenging effect of the essential oil extract, and the content can be obtained by comparing the test results of Zanthoxylum bungeanum seed essential oil 1, 7-8.

[0099] After adding anhydrous ethanol for leaching, the present invention further adopts a composite extractant (a water phase composed of a calcium chloride aqueous solution and an oil phase composed of isohexane and ethyl acetate) for extraction to prepare essential oil, which can make the essential oil have a better free radical scavenging effect. And the extraction effect of the extractant oil phase solvent composed of isohexane and ethyl acetate is better than that of single isohexane or ethyl acetate, and the combination of the two can improve the free radical scavenging efficiency of the essential oil. In particular, when isohexane and ethyl acetate form the oil phase solvent in a mass ratio of 2-5:1, the prickly ash seed essential oil obtained by the extraction process has a better effect. The above can be obtained in combination with the comparison of prickly ash seed essential oils 1, 9-13.

[0100] By comparing the Zanthoxylum bungeanum seed essential oils 1 and 14, it can be seen that the ultrafiltration of the present invention using an ultrafiltration membrane with a molecular weight cutoff lower than 500 Da can further enhance the free radical scavenging effect of the essential oils.

[0101] 2. Preparation and testing of Mulberry root extract

[0102] Chicken mulberry root extract 1:

[0103] The preparation method is as follows:

[0104] Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder;

[0105] Step II: mixing the powder with 47.5 wt % ethanol aqueous solution at a mass ratio of 1:22, heating to 58° C., stirring at 80 rpm for 8.4 hours to obtain an extract;

[0106] Step III: Filter the extract using a filter membrane with a pore size of 2 microns, ultrafilter the filtrate using an ultrafilter membrane with a molecular weight cutoff of 500Da, and freeze-dry the filtrate at -40°C to a water content of 4.38%, thereby obtaining the mulberry root extract.

[0107] Chicken Mulberry Root Extract 2:

[0108] The preparation method is as follows:

[0109] Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder;

[0110] Step II: mixing the powder with a 30 wt % ethanol aqueous solution at a mass ratio of 1:30, heating to 50° C., stirring at 80 rpm for 10 hours to obtain an extract;

[0111] Step III: The extract is filtered using a filter membrane with a pore size of 2 microns, the filtrate is ultrafiltered using an ultrafiltration membrane with a molecular weight cutoff of 600Da, and the filtrate is freeze-dried at -40°C to a water content of 4.19%, thereby obtaining the mulberry root extract.

[0112] Chicken mulberry root extract 3:

[0113] The preparation method is as follows:

[0114] Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder;

[0115] Step II: mixing the powder with a 55 wt % ethanol aqueous solution at a mass ratio of 1:10, heating to 62° C., stirring at 80 rpm for 4 hours to obtain an extract;

[0116] Step III: The extract is filtered using a filter membrane with a pore size of 2 microns, the filtrate is ultrafiltered using an ultrafiltration membrane with a molecular weight cutoff of 800Da, and the filtrate is freeze-dried at -40°C to a water content of 4.02% to obtain the mulberry root extract.

[0117] Chicken mulberry root extract 4:

[0118] The preparation method is as follows:

[0119] Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder;

[0120] Step II: Mix the powder and water in a mass ratio of 1:22, heat to 58° C., and stir at 80 rpm for 8.4 hours to obtain an extract;

[0121] Step III: Filter the extract using a filter membrane with a pore size of 2 microns, ultrafilter the filtrate using an ultrafilter membrane with a molecular weight cutoff of 500Da, and freeze-dry the filtrate at -40°C to a water content of 4.31%, thereby obtaining the mulberry root extract.

[0122] The extracts 1-4 of the above-mentioned Morus alba root were diluted to a mass concentration of 0.25% using an ethanol aqueous solution with a mass concentration of 50%, and then used as test samples to test the scavenging effect of DPPH free radicals. The specific experimental steps of the test refer to the method described above. The test results are shown in Table 2.

[0123] Table 2: K value of scavenging DPPH free radical efficiency of Morus alba root extract

[0124] Testing / 0.25% K value / % Chicken mulberry root extract 1 65.74 Chicken Mulberry Root Extract2 63.49 Chicken mulberry root extract 3 62.13 Chicken mulberry root extract 4 30.42

[0125] The test results in Table 2 show that the mulberry root extract obtained by extraction with ethanol aqueous solution in the present invention has a good free radical scavenging effect.

[0126] 3. The effect of combining Zanthoxylum bungeanum seed essential oil and Morus alba root extract

[0127] According to the above content, the DPPH free radical scavenging efficiency of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 is the best. Therefore, the Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 prepared above are matched to study the free radical scavenging effects of the two.

[0128] The mixture of Zanthoxylum bungeanum seed essential oil and Morus alba root extract in different mass ratios was diluted to a mass concentration of 0.25% with a 50% ethanol aqueous solution, and then used as a test sample to test the DPPH free radical scavenging effect. The specific test experimental steps refer to the method described above. The test results are shown in Table 3.

[0129] Table 3: K value of scavenging efficiency of DPPH free radicals of Morus alba root extract

[0130] Testing / 0.25% K value / % A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:0.2 66.78 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:0.4 67.53 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:0.6 70.04 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:0.7 71.39 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:0.9 73.57 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:1 72.16 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:1.5 68.12 A mixture of Zanthoxylum bungeanum seed essential oil 1 and Morus alba root extract 1 in a mass ratio of 1:2 67.25 Zanthoxylum bungeanum seed essential oil1 63.23 Chicken mulberry root extract 1 65.74

[0131] According to the test results in Table 3, the present invention uses Zanthoxylum bungeanum seed essential oil and Morus alba root extract to combine, which has a better scavenging efficiency of DPPH free radicals, and the two synergistically increase the scavenging effect of DPPH free radicals. The combination of the two in a dosage ratio of 1:0.6-1 has a better scavenging effect of free radicals.

[0132] IV. Application

[0133] The above-mentioned Zanthoxylum bungeanum seed essential oil and Morus alba root extract were prepared into cosmetic products for effect testing.

[0134] The specific cosmetic ingredients are:

[0135] Cosmetic 1: measured in parts by mass: 5.2 parts of glycerin, 3.4 parts of 1,2-propylene glycol, 1 part of sodium hyaluronate, 0.8 parts of β-glucan, 2.2 parts of grape seed oil, 1.8 parts of camellia oil, 2.4 parts of avocado oil, 2.4 parts of polyglyceryl-2 caprylate, 3.1 parts of PPG-2-laureth-5, 1.5 parts of Tween-60, 0.4 parts of purslane extract, 0.5 parts of chamomile extract, 0.8 parts of Zanthoxylum bungeanum seed essential oil 1, 0.7 parts of Morus alba root extract 1, 0.6 parts of carbomer-941, 0.2 parts of phenoxyethanol, 0.4 parts of citric acid and the remainder of water, a total of 100 parts by mass.

[0136] Cosmetic 2: measured in parts by mass: 4.8 parts of glycerin, 3.2 parts of 1,2-propylene glycol, 0.6 parts of sodium hyaluronate, 0.7 parts of β-glucan, 3 parts of grape seed oil, 1.5 parts of camellia oil, 2.2 parts of avocado oil, 2.8 parts of polyglyceryl-2 caprylate, 2.1 parts of PPG-2-laureth-5, 1.7 parts of Tween-60, 0.7 parts of purslane extract, 0.2 parts of chamomile extract, 0.9 parts of Zanthoxylum bungeanum seed essential oil 1, 0.6 parts of Morus alba root extract 1, 0.55 parts of carbomer-941, 0.21 parts of phenoxyethanol, 0.4 parts of citric acid and the remainder of water, a total of 100 parts by mass.

[0137] The preparation method of the above-mentioned cosmetics is: add water into a container, heat it to 70°C, add glycerin, 1,2-propylene glycol, grape seed oil, camellia oil, avocado oil, polyglycerol-2 caprylate, PPG-2-laureth-5 and Tween-60, and stir at 60rpm for 0.6 hours; cool to 35°C, add the remaining raw materials, continue to stir at the speed for 0.4 hours to obtain the cosmetics.

[0138] The cosmetic 1-2 was diluted with deionized water to a concentration of 6 wt % as a test substance, and then a skin patch test was performed.

[0139] The experimental method is: volunteers with sensitive skin aged between 30 and 45 were selected and randomly divided into 2 groups, 10 people in each group. 2 , a patch test device with a depth of about 1mm. The test substance is placed in the small chamber of the patch tester, and the amount of the test substance is 0.02mL; then the patch tester with the test substance added is taped to the back of the subject. After 24 hours, the patch tester is removed. One hour after the patch tester is removed and the indentation disappears, observe the skin reaction according to the standards recorded in Table 4 (i.e., the skin reaction grading standard for skin occlusion patch test), and record the observation results. The specific results are shown in Table 5.

[0140] Table 4: Skin occlusion patch test skin reaction grading criteria

[0141]

[0142] Table 5: Patch test results

[0143] Test / dilute to 5wt% Level 0 people Level 1 Number of people Level 2 Number of People Level 3 Number of People Level 4 Number of People Cosmetics 1 10 0 0 0 0 Cosmetics 2 10 0 0 0 0

[0144] It can be seen from the test results in Table 5 that hypoallergenic and non-irritating cosmetics can be prepared using the Zanthoxylum bungeanum seed essential oil and Morus alba root extract prepared by the present invention.

[0145] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A Zanthoxylum bungeanum seed essential oil, characterized in that: The preparation of the Zanthoxylum bungeanum seed essential oil comprises the following steps: Step 1: peel, wash and crush the dried Zanthoxylum bungeanum to obtain a crushed product; Step 2: Add 10-30 times the mass of water, cellulase and pectinase to the crushed material, heat to 30-40°C, stir and enzymolyze for 2-5 hours, then inactivate the enzyme to obtain the first enzymolysis product; Step 3: Inactivate the enzyme in the first enzymatic hydrolysis product, add papain and bromelain, heat to 28-38°C, stir and enzymatically hydrolyze for 3-6 hours, then inactivate the enzyme to obtain the second enzymatic hydrolysis product; Step 4: adding anhydrous ethanol to the second enzymatic hydrolysis product, heating to 50-60° C. and stirring for 4-8 hours to obtain an extract; wherein the mass of the anhydrous ethanol is 1-3 times the mass of the water in step 2; Step 5: filtering the extract using a filter membrane with a pore size of 0.1-10 microns, and ultrafiltering the filtrate using an ultrafiltration membrane with a molecular weight cutoff of less than 500 Da to obtain an ultrafiltrate; Step 6: Concentrate the ultrafiltrate to 10-20% of the mass of the ultrafiltrate to obtain a concentrated material, then add an extractant composed of an aqueous phase and an oil phase solvent, extract, then pour out the aqueous phase material and concentrate under reduced pressure to obtain the Zanthoxylum bungeanum seed essential oil; Among them, the total mass of cellulase and pectinase is 5-10% of the mass of the crushed material; The total mass of papain and bromelain is 4-12% of the mass of the crushed material; The aqueous phase is a calcium chloride aqueous solution with a mass concentration of 1.2-2.5%; The oil phase solvent is composed of isohexane and ethyl acetate in a mass ratio of 2-5:1; The mass ratio of water phase to oil phase is 1:2.5-4; The mass ratio of papain to bromelain is 1:2-3; The mass ratio of cellulase to pectinase is 1-3:1; In step 6, the mass ratio of concentrated material to extractant is 1:5-20.

2. The Zanthoxylum bungeanum seed essential oil according to claim 1, characterized in that In step 4, the mass of anhydrous ethanol is 1.2-3 times of the mass of water in step 2.

3. The Zanthoxylum bungeanum seed essential oil according to claim 1, characterized in that In step 6, the extraction temperature is 30-50° C. and the extraction time is 2-10 hours.

4. The Zanthoxylum bungeanum seed essential oil according to claim 1, characterized in that In step 6, the temperature for vacuum concentration is 50-55° C., and the vacuum concentration is performed until no oil phase solvent is detected.

5. A use of the Zanthoxylum bungeanum seed essential oil according to any one of claims 1 to 4 in cosmetics, characterized in that: The mass content of the Zanthoxylum bungeanum seed essential oil in cosmetics is 0.05-1%.

6. The use according to claim 5, characterized in that: The cosmetic further contains 0.04-0.8% of the mass of the cosmetic by weight of Morus altissima root extract, and the mass ratio of the Zanthoxylum bungeanum seed essential oil to the Morus altissima root extract is 1:0.6-1; The preparation method of the mulberry root extract comprises the following steps: Step I: crush the dried mulberry root and sieve through 80 mesh to obtain powder; Step II: mixing the powder with 30-55 wt % ethanol aqueous solution at a mass ratio of 1:10-30, heating to 50-62° C. and stirring for 4-10 hours to obtain an extract; Step III: filtering the extract using a filter membrane with a pore size of 2 microns, ultrafiltering the filtrate using an ultrafiltration membrane with a molecular weight cutoff lower than 800Da, and freeze-drying the filtrate to obtain the mulberry root extract.

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