CN111789786B

CN111789786B - Mite-killing plant composition and preparation method and application thereof

Info

Publication number: CN111789786B
Application number: CN202010813985.5A
Authority: CN
Inventors: 龚德明; 容惠; 徐洁琼; 张蕴勃
Original assignee: Guangzhou Jinan Cosmetics Co ltd
Current assignee: Guangzhou Jinan Cosmetics Co ltd
Priority date: 2020-08-13
Filing date: 2020-08-13
Publication date: 2022-11-11
Anticipated expiration: 2040-08-13
Also published as: CN111789786A

Abstract

The invention provides a mite-killing plant composition and a preparation method and application thereof. The mite-killing plant composition comprises: rosewood seed extract, zanthoxylum bungeanum fruit extract, sophora flavescens root extract, stemona japonica root extract and phellodendron amurense bark extract. The mite removing plant composition can effectively remove mites, inhibit grease secretion from roots and reduce skin oil by reducing the activity of sebaceous glands, achieves the possibility of inhibiting the reproduction of mites from a food chain, has outstanding moisturizing performance, good skin feeling and good absorption effect, and has the effects of moisturizing and repairing skin barriers.

Description

Mite-killing plant composition and preparation method and application thereof

Technical Field

The invention belongs to the technical field of cosmetics, and particularly relates to a mite-killing plant composition, and a preparation method and application thereof.

Background

Mites belong to a class of small animals of the class Guangdong subclass of the phylum Arthropoda, to human parasites of the class Arthropoda Arachnida, and are also vectors for many harmful pathogens. Adult mites are highly infected, and mite-infected skin often shows mild symptoms such as oily skin, large pores with blackheads, small pimples or red papules, itchy or peeling skin, etc., and severe infectors cause mite rosacea and allergic diseases. Especially for most men, the mite infection rate of the men is higher than that of women, because the skin of the men is different from that of the women, the horny layer of the skin of the men is usually thicker, the elasticity of the corium layer is more flexible than that of the women, and sebaceous glands are more active and developed, most men are mixed with oil to oily skin and are easily disturbed by grease, so that the oil-controlling and mite-removing cosmetics for women are not suitable for most men.

Meanwhile, the existing mite-killing cosmetics are more in variety, but basically have four problems: firstly, the mite removing effect is not obvious, the speed is low, old mites are not removed completely, new mites grow out again, the circulation is repeated, and the mite removing is remote and has no period; secondly, the ingredients have complex sources and low safety, and are easy to cause subacute percutaneous toxicity when being applied to remove mites on the skin; thirdly, the understanding of the growing environment of the mites is lacked, and only the mites are removed without inhibiting the mites, so that the problem of the mites is repeated; fourth, in terms of product formulation, the design is rarely made according to the skin characteristics of men, and the using effect of most men is poor.

CN110420266A discloses a three-pepper acne-removing and mite-removing agent which mainly comprises a zanthoxylum bungeanum fruit extract, a capsicum frutescens fruit extract and a kava root extract. The three-pepper acne-removing composition disclosed by the invention has a certain mite removing effect, the mite removing effect is still to be improved, and the composition has weak capability of reducing the activity of sebaceous glands and inhibiting grease secretion, so that the aim of inhibiting the reproduction of mites cannot be achieved from a food chain.

CN110732014A discloses a traditional Chinese medicine composition for removing mites as well as a preparation method and an application thereof, and the traditional Chinese medicine composition for removing mites comprises the following traditional Chinese medicine components in parts by weight: 10-35 parts of folium artemisiae argyi, 5-35 parts of radix sophorae flavescentis, 5-30 parts of pepper, 5-30 parts of cocklebur fruit, 5-30 parts of sweet orange flower, 5-25 parts of ginger and 5-30 parts of tea seed cake. The Chinese medicinal composition can prevent the mating and reproduction of mites by emitting a special fragrance, achieves the effect of strongly killing the mites, but has weak capability of reducing the activity of sebaceous glands and inhibiting the secretion of grease. Therefore, the possibility of inhibiting the reproduction of mites from the food chain cannot be achieved, and the content of the drug for achieving high mite removal rate is high.

Therefore, the development of a composition capable of highly effective mite removal and having an oil control effect is the focus of current research in the art.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a mite-killing plant composition and a preparation method and application thereof. The mite removing plant composition can effectively remove mites, inhibit grease secretion from roots and reduce skin oil by reducing the activity of sebaceous glands, achieves the possibility of inhibiting the reproduction of mites from a food chain, has outstanding moisturizing performance, good skin feeling and good absorption effect, and has the effects of moisturizing and repairing skin barriers.

In order to achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the present invention provides an acaricidal plant composition comprising: rosewood seed extract, zanthoxylum bungeanum fruit extract, sophora flavescens root extract, stemona japonica root extract and phellodendron amurense bark extract.

In the invention, the rosewood seed extract, the pricklyash peel fruit extract, the sophora flavescens root extract, the stemona sessilifolia root extract and the phellodendron bark extract are matched with each other, so that a synergistic effect is achieved, the mite removing plant composition can interfere the permeability of the cell membrane of mites and block the absorption of the cell membrane to nutrient substances, and the mite inhibiting effect is achieved; and the possibility of inhibiting the reproduction of mites from a food chain is achieved by reducing the activity of pores, inhibiting the secretion of sebum, reducing the activity of sebaceous glands and radically inhibiting the secretion of grease.

Wherein the rosewood seed extract is effective in reducing sebaceous gland activity and inhibiting sebum secretion, but does not dry skin and can keep skin moist. The zanthoxylum bungeanum fruit extract contains active ingredients such as limonene, teosinte, phytosterol, benzoic acid, alkaloid and the like, and the active ingredients can easily permeate through a cell membrane structure to interfere the permeability of the cell membrane of mites, hinder the absorption of the cell membrane to amino acid, and enable the physiological activity of the mites to be disordered, so that the effect of inhibiting the mites is achieved. The sophora flavescens can balance grease secretion, dredge and astringe pores, remove toxin impurities in skin, enrich herbal nutrition, promote the growth and repair of damaged vascular nerve cells, and restore the activity of subcutaneous capillary cells. The radix Stemonae extract is derived from dried rhizome of Stemona sessilifolia (Stemona sessilifolia) of Stemonaceae, contains active ingredients such as stemonine, hodorine, stemonine and protostemonine, and has inhibitory effect on mite growth, and multiple alkaloids can effectively remove excessively secreted sebum. The cortex Phellodendri extract contains large amount of berberine hydrochloride, jateorhizine, phellodendrine, etc., and has effects in removing skin oil and fat, reducing skin luster, delaying skin keratinization, and keeping skin smooth and moist. It can be used topically for promoting absorption of subcutaneous blood, and has antiallergic effect.

Preferably, the mite removing plant composition comprises the following components in parts by weight: 5-10 parts of rosewood seed extract, 5-10 parts of zanthoxylum bungeanum fruit extract, 5-10 parts of sophora flavescens root extract, 1-5 parts of radix stemonae petiolata root extract and 1-5 parts of phellodendron bark extract.

In the present invention, the content of the rosewood seed extract is 5 to 10 parts, and may be, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.

In the invention, the content of the zanthoxylum bungeanum fruit extract is 5-10 parts, such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts and the like.

In the present invention, the content of the extract of kuh-seng root is 5-10 parts, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.

In the present invention, the content of the stemona tuberosa root extract is 1-5 parts, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, etc.

In the present invention, the content of the phellodendron amurense bark extract is 1 to 5 parts, and may be, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, etc.

Preferably, the rosewood seed extract is prepared by the following preparation method:

(1) Crushing rosewood seeds, mixing the crushed rosewood seeds with an alcohol solvent, and performing microwave extraction to obtain a rosewood seed extracting solution;

(2) Centrifuging the rosewood seed extracting solution obtained in the step (1), and concentrating by adopting a reverse osmosis membrane to obtain a crude extract of rosewood seeds;

(3) And (3) mixing the crude extract of the rosewood seeds obtained in the step (2) with maltodextrin for ultrasonic treatment, and freezing to obtain the rosewood seed extract.

Preferably, the particle size of the crushed rosewood seeds in the step (1) is 10-100 meshes, for example, 10 meshes, 20 meshes, 40 meshes, 60 meshes, 80 meshes, 100 meshes and the like.

Preferably, the alcohol solvent in step (1) is 60-80wt% ethanol water solution, for example, 60wt%, 65wt%, 70wt%, 75wt%, 80wt%, etc., and the mass ratio of the rosewood seed to the alcohol solvent is 1 (8-12), for example, 1:8, 1:9, 1.

Preferably, the microwave extraction time in step (1) is 3-7min, such as 3min, 4min, 5min, 6min, 7min, etc., the power of the microwave extraction is 0.5-1.5kW, such as 0.5kW, 0.7kW, 0.9kW, 1.1kW, 1.3kW, 1.5kW, etc., and the number of times of the microwave extraction is 2-5 times, such as 2 times, 3 times, 4 times, 5 times, etc.

Preferably, the centrifugation in step (2) is carried out by using a disk centrifuge, and the rotation speed of the centrifugation is 6000 to 8000r/min, such as 6000r/min, 6500r/min, 7000r/min, 7500r/min, 8000r/min and the like.

Preferably, the reverse osmosis membrane of step (2) is concentrated at a pressure of 5-30bar, such as 5bar, 10bar, 15bar, 20bar, 25bar, 30bar, etc.

Preferably, the mass ratio of the crude extract of the rosewood seeds in the step (3) to the maltodextrin is (3-5) to (5-7);

wherein "3 to 5" may be, for example, 3, 3.5, 4, 4.5, 5, etc.;

here, "5 to 7" may be, for example, 5, 5.5, 6, 6.5, 7, etc.

Preferably, the ultrasound in step (3) is performed for 30-90min, such as 30min, 40min, 50min, 60min, 70min, 80min, 90min, etc., and the power of the ultrasound is 100-500W, such as 100W, 200W, 300W, 400W, 500W, etc.

Preferably, the freezing temperature in step (3) is-25 to-5 ℃, such as-25 ℃, -20 ℃, -15 ℃, -10 ℃, -5 ℃ and the like, and the freezing time is 60 to 240min, such as 60min, 80min, 100min, 120min, 140min, 160min, 180min, 200min, 240min and the like.

Preferably, the zanthoxylum bungeanum maxim fruit extract is prepared by the following preparation method: crushing dry pricklyash peel, mixing with a solvent A, standing for extraction, mixing with a solvent B, standing for extraction, and filtering to obtain a filtrate; mixing the obtained filtrate with alkaline solution, stirring, mixing with saline water, standing for layering, collecting upper layer solution, and concentrating to obtain fructus Zanthoxyli extract.

Preferably, the particle size of the pulverized dry prickly ash fruit is 100 to 200 meshes, for example, 100 meshes, 120 meshes, 140 meshes, 160 meshes, 180 meshes, 200 meshes, and the like.

Preferably, the solvent A is any one or combination of at least two of n-hexane, petroleum ether or cyclohexane, and the mass ratio of the dry pricklyash peel to the solvent A is 1 (2-3), and can be, for example, 1:2, 1.2, 1.

Preferably, the solvent B is acetone and/or ethyl acetate, and the mass ratio of the dry pricklyash peel fruit to the solvent B is 1 (2-3), and can be, for example, 1:2, 1.

Preferably, the alkaline solution is a sodium bicarbonate solution and/or a sodium carbonate solution, the concentration of the alkaline solution is 1-5wt%, for example, it may be 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, etc.

Preferably, the mass ratio of the dry pricklyash peels to the alkaline solution is 1 (50-100), and can be, for example, 1.

Preferably, the saline is saturated saline, and the mass ratio of the dried pricklyash peel fruit to the saline is 1 (50-100), and can be, for example, 1.

Preferably, the extract of the sophora flavescens roots is prepared by the following preparation method: pulverizing radix Sophorae Flavescentis, mixing with alcohol solvent, reflux extracting, concentrating, and spray drying to obtain radix Sophorae Flavescentis extract.

Preferably, the particle size of the pulverized kushen root is 100 to 200 meshes, such as 100 meshes, 120 meshes, 140 meshes, 160 meshes, 180 meshes, 200 meshes and the like.

Preferably, the alcohol solvent is an aqueous ethanol solution with a concentration of 60-70wt%, for example, 60wt%, 65wt%, 70wt%, etc.

Preferably, the reflux extraction is performed 2-5 times, for example, 2 times, 3 times, 4 times, 5 times, etc.

Preferably, the temperature of the spray drying is 30 to 50 ℃, for example, 30 ℃, 35 ℃, 40 ℃, 45 ℃,50 ℃ and the like, and the pressure of the spray drying is 25 to 35MPa, for example, 25MPa, 27MPa, 29MPa, 31MPa, 33MPa, 35MPa and the like.

Preferably, the stemona tuberosa root extract is prepared by the following preparation method:

(a) Pulverizing radix Stemonae, mixing with water, standing, and extracting to obtain water extract;

(b) Microfiltering and ultrafiltering the water extraction product obtained in the step (a) to obtain filter residue and filtrate;

(c) And (c) carrying out alcohol precipitation on the filter residue obtained in the step (b) to obtain an extract I, concentrating and spray-drying the filtrate obtained in the step (b) to obtain an extract II, and combining the extract I and the extract II to obtain the stemona tuberosa root extract.

Preferably, the particle size of the pulverized radix stemonae tuberosi in step (a) is 100-200 meshes, for example, 100 meshes, 120 meshes, 140 meshes, 160 meshes, 180 meshes, 200 meshes, etc.

Preferably, the mass ratio of the stemona tuberosa root to the water in the step (a) is 1 (8-12), and can be 1:8, 1:9, 1.

Preferably, the microfiltration in step (b) is carried out using a ceramic membrane having a pore number of 30-40, such as 30, 32, 34, 36, 38, 40, etc., and a separation accuracy of 40-55nm, such as 40nm, 42nm, 44nm, 46nm, 48nm, 50nm, 53nm, 55nm, etc.

Preferably, the ultrafiltration in step (b) is performed using an ultrafiltration membrane, and the molecular weight of the cut-off pore size of the ultrafiltration membrane separation device is greater than 1000, and may be, for example, 1200, 1500, 2000, 3000, 4000, 5000, 8000, 10000, 20000, etc.

Preferably, the alcohol precipitation in step (c) is performed with ethanol.

Preferably, the temperature of the spray drying in step (c) is 30-50 ℃, such as 30 ℃, 35 ℃, 40 ℃, 45 ℃,50 ℃ and the like, and the pressure of the spray drying is 25-35MPa, such as 25MPa, 27MPa, 29MPa, 31MPa, 33MPa, 35MPa and the like.

Preferably, the phellodendron amurense bark extract is prepared by the following preparation method:

(A) Pulverizing cortex Phellodendri, and defatting to obtain defatted cortex Phellodendri bark powder;

(B) Mixing the degreased phellodendron amurense bark powder obtained in the step (A) with an ethanol water solution, performing ultrasonic extraction and concentrating to obtain a crude phellodendron amurense bark extract;

(C) Dissolving the coarse extract of phellodendron amurense bark obtained in the step (B), purifying and eluting by adopting a macroporous resin gel column, and concentrating to obtain the phellodendron amurense bark extract;

preferably, the particle size of the pulverized phellodendron amurense bark in the step (a) is 100-200 meshes, such as 100 meshes, 120 meshes, 140 meshes, 160 meshes, 180 meshes, 200 meshes and the like.

Preferably, the degreasing treatment in the step (a) is: pulverizing cortex Phellodendri, mixing with n-hexane, soaking, filtering, and drying to obtain defatted cortex Phellodendri powder.

Preferably, the mass ratio of the phellodendron amurense bark to the n-hexane is 1 (1-3), and can be 1:1, 1.5, 1:2, 1.5, 1:3 and the like.

Preferably, the soaking time is 2-4h, such as 2h, 2.5h, 3h, 3.5h, 4h, etc., and the soaking temperature is 25-35 deg.C, such as 25 deg.C, 27 deg.C, 29 deg.C, 31 deg.C, 33 deg.C, 35 deg.C, etc.

Preferably, the ethanol aqueous solution of step (B) is ethanol aqueous solution with concentration of 40-80wt%, for example, 40wt%, 45wt%, 50wt%, 55wt%, 60wt%, 65wt%, 70wt%, 75wt%, 80wt%, etc.

Preferably, the time of the ultrasonic extraction in step (B) is 30-90min, such as 30min, 40min, 50min, 60min, 70min, 80min, 90min, etc., and the power of the ultrasonic extraction is 100-500W, such as 100W, 200W, 300W, 400W, 500W, etc.

Preferably, the dissolution in step (C) is carried out using an aqueous ethanol solution having a concentration of 5 to 15wt%, and may be, for example, 5wt%, 7wt%, 9wt%, 11wt%, 13wt%, 15wt%, etc.

Preferably, the filling resin of the macroporous resin gel column in the step (C) is any one or a combination of at least two of D101, D4020, HPD-100, DM130 or HPD-400;

preferably, the elution in step (C) is carried out using an aqueous ethanol solution having a concentration of 40 to 80wt%, and may be, for example, 40wt%, 45wt%, 50wt%, 55wt%, 60wt%, 65wt%, 70wt%, 75wt%, 80wt%, etc.

In a second aspect, the present invention provides a method for preparing the mite-killing plant composition according to the first aspect, wherein the method for preparing the mite-killing plant composition comprises the following steps: mixing a rosewood seed extract, a zanthoxylum bungeanum fruit extract, a sophora flavescens root extract, a sessile stemona root extract and a phellodendron bark extract to obtain the mite removing plant composition;

preferably, the mixing temperature is 20-40 deg.C, such as 20 deg.C, 25 deg.C, 30 deg.C, 35 deg.C, 40 deg.C, etc., and the mixing time is 5-20min, such as 5min, 10min, 15min, 20min, etc.

In a third aspect, the present invention provides a use of the mite-killing plant composition according to the first aspect in the preparation of cosmetics.

Preferably, the acarus-killing plant composition is added in an amount of 0.05-10% by mass of the total cosmetic, for example, 0.05%, 0.5%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10% or the like.

In a fourth aspect, the present invention provides a cosmetic product comprising the mite-killing plant composition of the first aspect.

Preferably, the cosmetic comprises any one of essence, face cleaning cream, shampoo or body wash.

Compared with the prior art, the invention has the following beneficial effects:

(1) The rosewood seed extract, the pricklyash peel fruit extract, the sophora flavescens root extract, the stemona sessilifolia root extract and the phellodendron bark extract in the mite-killing plant composition are matched with each other, have a synergistic interaction effect, and interfere the permeability of the cell membrane of mites to block the absorption of the cell membrane to nutrient substances, so that the mite-killing effect is achieved; by reducing the activity of sebaceous glands, the oil secretion is inhibited from the root, the oil production of skin is reduced, the possibility of inhibiting the reproduction of mites from a food chain is achieved, the moisture retention performance is outstanding, the skin feeling is good, the absorption effect is good, and the effects of moisturizing and repairing skin barriers are achieved;

(2) In the mite killing test of the mite killing plant composition, the insecticidal rate is more than 95 percent, and the inhibition rate to 5 alpha-reductase liquid is 70-75 percent; after 4 weeks of application of the mite removing plant composition, the reduction degree of sebum level of the back is below-30%, the reduction degree of active pore number is below-35%, and the reduction degree of sebum percentage on the surface of skin is below-40%; the plant composition for removing acarid has a moisture retention rate of more than 80%, a small change rate of percutaneous water loss, and a moisture content of skin of more than 45% after 4 hours of use, wherein the change rate of percutaneous water loss is maintained below 15%.

Detailed Description

The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.

Preparation example 1

The preparation example provides a rosewood seed extract, which is prepared by the following preparation method:

(1) Crushing rosewood seeds to a particle size of 50 meshes, mixing the rosewood seeds with 70wt% of ethanol water solution according to a mass ratio of 1;

(2) Centrifuging the rosewood seed extracting solution obtained in the step (1) at the rotating speed of 7000r/min by adopting a disc centrifuge, and concentrating by adopting a reverse osmosis membrane, wherein the concentration pressure is 10bar to obtain a crude rosewood seed extract;

(3) Mixing the crude extract of the rosewood seeds obtained in the step (2) with maltodextrin in a mass ratio of 4:6 for ultrasonic treatment, wherein the ultrasonic treatment time is 60min, the ultrasonic treatment power is 300W, and freezing at-15 ℃ to obtain the rosewood seed extract.

Preparation example 2

The preparation example provides a zanthoxylum bungeanum maxim fruit extract, which is prepared by the following preparation method: crushing dry pricklyash peel into particles with the particle size of 150 meshes, mixing the particles with petroleum ether, standing and extracting, mixing the mixture with acetone, standing and extracting, and filtering to obtain filtrate, wherein the mass ratio of the dry pricklyash peel fruit to the petroleum ether is 1:2, and the mass ratio of the dry pricklyash peel fruit to the acetone is 1:3; mixing and stirring the obtained filtrate and a 2wt% sodium bicarbonate solution, mixing the dried Chinese prickly ash fruit and the 2wt% sodium bicarbonate solution in a mass ratio of 1.

Preparation example 3

The preparation example provides a kuh-seng root extract, which is prepared by the following preparation method: crushing the sophora flavescens ait root to 150 meshes, mixing the sophora flavescens ait root with 75wt% of ethanol water solution according to the mass ratio of 1.

Preparation example 4

The preparation example provides a stemona tuberosa root extract, which is prepared by the following preparation method:

(a) Crushing the stemona tuberosa roots to a particle size of 150 meshes, mixing the stemona tuberosa roots with water according to a mass ratio of 1;

(b) Microfiltration is carried out on the water extraction product obtained in the step (a), the microfiltration is carried out by adopting a ceramic membrane, the number of pores of the ceramic membrane is 35, the separation precision of the ceramic membrane is 80nm, then ultrafiltration is carried out, and the molecular weight of the interception pore diameter of ultrafiltration membrane separation equipment is larger than 1000, so that filter residue and filtrate are obtained;

(c) Mixing the filter residue obtained in the step (b) with ethanol for alcohol precipitation to obtain an extract I, concentrating the filtrate obtained in the step (b), performing spray drying at 40 ℃ and under 30MPa to obtain an extract II, and combining the extract I and the extract II to obtain the stemona tuberosa root extract.

Preparation example 5

The preparation example provides a phellodendron amurense bark extract, which is prepared by the following preparation method:

(A) Pulverizing cortex Phellodendri bark to 150 mesh, mixing with n-hexane at a mass ratio of 1:2, soaking at 30 deg.C for 3h, filtering, and drying to obtain defatted cortex Phellodendri bark powder;

(B) Mixing the degreased phellodendron amurense bark powder obtained in the step (A) with 60wt% ethanol water solution according to the mass ratio of 1;

(C) Dissolving the coarse extract of the phellodendron amurense bark obtained in the step (B) by using 10wt% ethanol water solution, purifying by using a D4020 macroporous resin gel column, eluting by using 60wt% ethanol water solution, and concentrating to obtain the phellodendron amurense bark extract.

Examples 1 to 6

Examples 1-6 provide different mite-killing botanical compositions, respectively, and the extracts of the examples were prepared according to preparation examples 1-5, and the formulations of the examples in parts by weight are shown in table 1 below:

TABLE 1

The preparation method of the mite-killing plant composition in the embodiment comprises the following steps: mixing and stirring the rosewood seed extract, the zanthoxylum bungeanum fruit extract, the sophora flavescens root extract, the stemona tuberosa root extract and the phellodendron amurense bark extract at 25 ℃ for 10min according to the formula amount to obtain the mite removing plant composition.

Comparative examples 1 to 10

Comparative examples 1-10 each provide a different mite-combating botanical composition, each of the formulations in parts by weight are shown in table 2 below:

TABLE 2

The preparation method of the mite removing plant composition in the comparative example comprises the following steps: mixing and stirring the rosewood seed extract, the zanthoxylum bungeanum fruit extract, the sophora flavescens root extract, the stemona japonica root extract and the phellodendron amurense bark extract at the temperature of 25 ℃ for 10min according to the formula amount to obtain the mite removing plant composition.

Test example 1

Safety performance testing

The mite-killing plant compositions provided in examples 1-6 and the mite-killing plant compositions provided in comparative examples 1-5 were subjected to safety performance tests as follows:

(1) Haemolysis test of erythrocytes

Preparation of the erythrocyte suspension: selecting healthy rabbit, taking 9mL of blood from heart, adding 1mL of 2% potassium oxalate solution, centrifuging, discarding supernatant, diluting the precipitate to 20mL with 20mmol/L PBS solution, and storing at 4 ℃ for later use. Select samples were diluted with PBS solution to different concentrations, with 5 concentration gradients set for each sample. Adding 200 μ L of the above erythrocyte suspension (final concentration of the sample is controlled to be 5, 10, 20, 50, 100mg/mL respectively) into 10mL of diluent of the sample to be tested, taking distilled water as total blood-dissolving control, taking PBS solution as negative control, mixing gently, incubating at 37 deg.C for 30min, centrifuging at 2000r/min for 10min, collecting supernatant, and testing its absorbance at 560nm with spectrophotometer (A) ₅₆₀ ) Calculating the hemolysis rate according to the following formula;

a standard curve of hemolysis rate vs. sample concentration was plotted, and the sample concentration at which hemolysis occurred in 50% erythrocytes (HD) was calculated ₅₀ )。

(2) Protein denaturation experiments:

will sampleDiluting the product with PBS solution to 10g/L, collecting 10mL dilution of sample to be tested, adding 200 μ L of the above erythrocyte suspension, using distilled water as blank control, 1mg/mL Sodium Dodecyl Sulfate (SDS) solution as positive control, mixing, incubating at 37 deg.C for 30min, centrifuging at 2000r/min for 10min, collecting supernatant, and testing absorbance A at 540nm and 575nm with spectrophotometer ₅₄₀ And A ₅₇₅ Calculating a protein Denaturation Index (DI) according to the following formula;

wherein R is ₁ = blank control group a ₅₇₅ Blank control group A ₅₄₀ ，R ₂ = Experimental group A ₅₇₅ Experimental group A ₅₄₀ ，R ₃ = positive control group a ₅₇₅ Positive control group A ₅₄₀ 。

Evaluating the irritation of the sample to be tested according to the L/D value, wherein the L/D value is HD ₅₀ DI, erythrocyte hemolysis assay irritation grading criteria are shown in Table 3 below:

TABLE 3

L/D	Grading
		>100	Has no irritation
10<L/D≤100	Micro-stimulation property
		1<L/D≤10	Mild irritation
0.1<L/D≤1	Moderate irritation

The results of the above-described hemolysis test and protein denaturation test are shown in Table 4 below:

TABLE 4

As can be seen from the test results in Table 4, the mite-removing plant compositions provided in examples 1 to 6 of the present invention are mild and non-irritating, and have a sample concentration HD at which 50% of erythrocytes are hemolyzed ₅₀ HD more than 26000mg/L than that of the mite-killing plant composition provided by the comparative examples 1-5 ₅₀ (ii) a Meanwhile, the protein denaturation index DI is below 1.5 percent and is obviously smaller than the mite removing plant composition provided by the comparative examples 1-5, which shows that the addition of the mite removing plant composition can obviously reduce toxic and side effects and irritation and is safer and more reliable.

Test example 2

Mite killing rate test

(1) Test samples: the mite-killing plant composition provided in examples 1-6 and the mite-killing plant composition provided in comparative examples 1-5;

(2) Acquisition of human demodex: adopting a transparent adhesive tape sticking method to obtain the demodex, and specifically comprising the following steps: order the examinee to wash the face before sleeping, and then apply the scotch tape with length of 6cm and width of 1.5cm to the forehead, cheek, nose, chin, etc., and then take off the scotch tape the next morning, examine the scotch tape, and seal the scotch tape in the glass slide.

(3) Grouping tests: 0.1mg/cm is dripped into each glass slide ² The samples were tested to ensure that each composition was in sufficient contact with the worm. Placing at relative humidity of 70-80% and temperature of 2Taking out the demodex after 1h in an environment of 6-28 ℃, and observing the survival condition of the demodex under a microscope. After continuously observing under a microscope at 400X for 3min, the dead insect is judged to be dead by the unmoved insect body.

The specific test results are shown in table 5 below:

TABLE 5

Test sample	Mite killing rate/%)
		Example 1	99.9
Example 2	99.7
		Example 3	99.5
Example 4	97.5
		Example 5	98.2
Example 6	95.8
		Comparative example 1	70.5
Comparative example 2	72.8
		Comparative example 3	75.3
Comparative example 4	74.2
		Comparative example 5	73.2

As can be seen from the test results in Table 5, the insecticidal ratio in the mite removing test of the mite removing plant compositions provided in examples 1 to 6 was 95% or more. The result shows that the rosewood seed extract, the pricklyash peel fruit extract, the sophora flavescens root extract, the stemona sessilifolia root extract and the phellodendron bark extract in the mite-killing plant composition are matched with each other, so that a synergistic effect is achieved, the mite-killing plant composition can interfere the permeability of the cell membrane of mites and block the absorption of the cell membrane to nutrient substances, and the mite-killing effect is achieved.

Test example 3

In vitro oil control test

(2) The testing steps are as follows: 11 identical 5 alpha-reducing enzyme solutions are prepared by using liver homogenates of 5 male SD rats, one of the composition samples is added into each group, and the inhibition rate of each test sample on the 5 alpha-reducing enzyme solution is detected through a series of reaction systems, wherein the higher the inhibition rate is, the better the oil control effect is.

The specific test results are shown in table 6 below:

TABLE 6

Test sample	5 alpha-reductase solutionInhibition rate of
		Example 1	75.0
Example 2	74.7
		Example 3	73.9
Example 4	71.2
		Example 5	71.8
Example 6	70.5
		Comparative example 1	55.5
Comparative example 2	50.8
		Comparative example 3	57.3
Comparative example 4	58.2
		Comparative example 5	60.2

As shown in the test results in table 6, the mite removing plant compositions provided in examples 1 to 6 have an inhibition rate of 5 α -reductase solution of 70 to 75%, which indicates that the combination of the rosewood seed extract, the zanthoxylum bungeanum fruit extract, the sophora flavescens root extract, the stemona japonica root extract and the phellodendron bark extract in the mite removing plant composition of the present invention has synergistic effect, can inhibit sebum secretion, reduce sebaceous gland activity, inhibit oil secretion from root source, and inhibit the possibility of mite reproduction from food chain.

Test example 4

Oil control Performance test

(1) Test samples: the mite-removing plant compositions provided in examples 1-6 and the mite-removing plant compositions provided in comparative examples 1-5;

(2) Sebum Level (CSL) test method: 110 volunteers, male 25-50 years old, were selected and randomly divided into 11 groups of 10 persons each, and each group was applied with appropriate amount of each test sample on the face, once a day, morning and evening. Testing the sebum level (CSL) of the 4 th week by using a sebum test analyzer, taking the average value of the test result of a user, taking the sebum level 30min after the test area is cleaned as an initial value, and recording the sebum level reduction degree;

(3) Number of Active Pores (NAP) and percent skin Surface Sebum (SSP) test: 110 volunteers, male 25-50 years old, were selected and randomly divided into 11 groups of 10 persons, each group was applied with appropriate amount of each test sample on the face, and used once a day, morning and evening. The Number of Active Pores (NAP) and the percentage of skin Surface Sebum (SSP) were measured at week 4 using an active skin surface analysis system, and the average of the user's test results was taken, and the reduction in the number of active pores and the reduction in the percentage of skin Surface Sebum (SSP) were recorded using the Number of Active Pores (NAP) and the percentage of skin Surface Sebum (SSP) at 30min after cleaning of the test area as initial values.

The specific test results are shown in table 7 below:

TABLE 7

As can be seen from the test results in Table 7, the decrease of sebum level in the back after 4 weeks of application of the mite-removing plant composition is below-30%, the decrease of number of active pores is below-35%, and the decrease of sebum percentage on the surface of skin is below-40%. The plant mite-killing composition has the advantages that all components are matched with each other to realize synergistic interaction, the activity of pores can be reduced, sebum secretion is inhibited, water-oil balance of skin is adjusted, the activity of sebaceous glands is reduced, and the possibility of inhibiting the reproduction of mites from a food chain is achieved.

Test example 5

Test for moisture retention

The mite-killing plant compositions provided in examples 1-6 and the mite-killing plant compositions provided in comparative examples 1-5 were subjected to a moisturizing performance test by the following method:

(1) In vitro weighing method for testing moisture retention performance

0.2g of each composition is weighed and evenly coated on a 5 cm-by-5 cm glass plate stuck with the microporous breathable adhesive tape respectively, the glass plate is placed in a dryer with constant temperature and constant humidity, the mass of the glass plate after being placed for 4 hours is weighed respectively, and the moisture retention rate is calculated. The moisture retention rate calculation formula is as follows:

moisture retention rate/% = (M) ₂ -M ₀ )/(M ₁ -M ₀ )×100％。

Wherein M is ₀ Is the mass/g, M, of the glass sheet ₁ For the mass/g, M of the glass plate after sample application ₂ The glass plate mass/g after being left in the desiccator for several hours.

(2) Rate of change of transepidermal water loss

110 volunteers, men 25-50 years of age, were selected and randomly divided into 11 groups of 10 persons, and the mite removing plant composition provided in examples 1-6 and the mite removing plant composition provided in comparative examples 1-5 were used, respectively. The test apparatus is Tewameter TM300 from CK corporation, germany, and the external environment is tested: room temperature 25 ℃ and humidity 60%. Before the composition was applied and after 4 consecutive days, the rate of change of transepidermal water loss was measured for each subject three times, and after taking the average value, the average value for each group was calculated and one decimal point was retained.

(3) Water retention rate

110 volunteers, men aged 25-50 years, were selected and randomly divided into 11 groups of 10 persons, and the mite removing plant compositions provided in examples 1-6 and comparative examples 1-5 were used, respectively. The instrument is a Courage + Khazaka electronic model Germany: derma Unit SSC, test temperature 25 ℃, humidity 60%. The skin moisture content of each subject was tested before and 4h after use, three times for each data, and after taking the average, the average of each group was calculated, and one decimal place was retained.

Specific test results are shown in table 8.

TABLE 8

The data in the table show that the mite removing plant composition provided by the invention has a good moisturizing effect, the moisturizing rate is more than 80%, the change rate of percutaneous water loss is small and is kept below 15%, and the moisture content of skin after the mite removing plant composition is used for 4 hours is more than 45%.

The applicant states that the present invention is illustrated by the above examples of mite-killing plant compositions and methods of making and using the same, but the present invention is not limited to the above examples, i.e., it is not meant to imply that the present invention must be practiced by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims

1. The mite removing plant composition is characterized by comprising the following components in parts by weight: 5-10 parts of rosewood seed extract, 5-10 parts of zanthoxylum bungeanum fruit extract, 5-10 parts of sophora flavescens root extract, 1-5 parts of stemona tuberosa root extract and 1-5 parts of phellodendron amurense bark extract;

the rosewood seed extract is prepared by the following preparation method:

(3) Mixing the crude extract of the rosewood seeds obtained in the step (2) with maltodextrin for ultrasonic treatment, and freezing to obtain the rosewood seed extract;

the zanthoxylum bungeanum maxim extract is prepared by the following preparation method: crushing dry pepper fruits, mixing the crushed dry pepper fruits with a solvent A, standing for extraction, mixing the mixture with a solvent B, standing for extraction, and filtering to obtain filtrate; mixing the obtained filtrate with alkaline solution, stirring, mixing with saline water, standing for layering, collecting upper layer solution, and concentrating to obtain fructus Zanthoxyli extract;

the kuh-seng root extract is prepared by the following preparation method: pulverizing radix Sophorae Flavescentis, mixing with alcohol solvent, reflux extracting, concentrating, and spray drying to obtain radix Sophorae Flavescentis extract;

the stemona tuberosa root extract is prepared by the following preparation method:

(c) Precipitating the filter residue obtained in the step (b) with ethanol to obtain an extract I, concentrating and spray-drying the filtrate obtained in the step (b) to obtain an extract II, and combining the extract I and the extract II to obtain the stemona tuberosa root extract;

the phellodendron amurense bark extract is prepared by the following preparation method:

(C) Dissolving the coarse extract of the phellodendron amurense bark obtained in the step (B), purifying and eluting by adopting a macroporous resin gel column, and concentrating to obtain the phellodendron amurense bark extract.

2. The acarus killing plant composition of claim 1, wherein the size of the pulverized rosewood seed of step (1) is 10-100 mesh.

3. The mite removing plant composition of claim 1, wherein the alcohol solvent in the step (1) is an ethanol water solution with the concentration of 60-80wt%, and the mass ratio of the rosewood seeds to the alcohol solvent is 1 (8-12).

4. The acarus killing plant composition of claim 1, wherein the microwave extraction time of step (1) is 3-7min, the power of the microwave extraction is 0.5-1.5kW, and the number of times of the microwave extraction is 2-5.

5. The acaricidal plant composition according to claim 1, wherein the centrifugation in step (2) is carried out using a disk centrifuge at a rotation rate of from 6000 to 8000r/min.

6. The acarus killing plant composition of claim 1, wherein the reverse osmosis membrane of step (2) is concentrated at a pressure of 5 to 30bar.

7. The mite-killing plant composition of claim 1, wherein the mass ratio of the crude extract of red wood seeds to maltodextrin in step (3) is (3-5) to (5-7).

8. The acarus killing plant composition of claim 1, wherein the time of the ultrasound in step (3) is 30-90min, and the power of the ultrasound is 100-500W.

9. The acarus killing plant composition of claim 1, wherein the temperature of the freezing in step (3) is-25 to-5 ℃, and the time of the freezing is 60 to 240min.

10. The acarus killing plant composition of claim 1, wherein the particle size of the pulverized dry prickly ash fruit is 100-200 mesh.

11. The acarus killing plant composition as claimed in claim 1, wherein the solvent A is any one or combination of at least two of n-hexane, petroleum ether or cyclohexane, and the mass ratio of the dry pricklyash peel to the solvent A is 1 (2-3).

12. The acarus killing plant composition as claimed in claim 1, wherein the solvent B is acetone and/or ethyl acetate, and the mass ratio of the dry pricklyash peel fruit to the solvent B is 1 (2-3).

13. The acaricidal plant composition according to claim 1, wherein said alkaline solution is a sodium bicarbonate solution and/or a sodium carbonate solution, said alkaline solution having a concentration of 1-5% by weight.

14. The acarus killing plant composition as claimed in claim 1, wherein the mass ratio of the dry prickly ash fruit to the alkaline solution is 1 (50-100).

15. The acarus killing plant composition as claimed in claim 1, wherein the saline water is saturated saline water, and the mass ratio of the dried pricklyash peel fruit to the saline water is 1 (50-100).

16. The acarus killing plant composition of claim 1, wherein the pulverized root of Sophora flavescens ait has a particle size of 100-200 mesh.

17. The mite-killing plant composition of claim 1, wherein the alcohol solvent is an ethanol water solution with the concentration of 60-70wt%, and the mass ratio of the sophora flavescens roots to the alcohol solvent is 1 (8-12).

18. The acaricidal plant composition of claim 1 wherein the number of reflux extractions is from 2 to 5.

19. The acarus killing plant composition of claim 1, wherein the extract of the roots of sophora flavescens ait is prepared by the spray drying temperature of 30-50 ℃ and the spray drying pressure of 25-35MPa.

20. The acaricidal plant composition of claim 1, wherein the particle size of the comminuted tuberostemona tuberosa root of step (a) is 100-200 mesh.

21. The acarus killing plant composition of claim 1, wherein the mass ratio of the tuberostemona tuberosa root to the water in the step (a) is 1 (8-12).

22. The acarus killing plant composition of claim 1, wherein the microfiltration in step (b) is performed using a ceramic membrane, the number of pores of the ceramic membrane is 30-40, and the separation precision of the ceramic membrane is 40-55nm.

23. The acarus killing plant composition of claim 1 wherein the ultrafiltration of step (b) is performed using an ultrafiltration membrane, said ultrafiltration membrane separation device having a molecular weight cutoff greater than 1000.

24. The acarus killing plant composition of claim 1, wherein the alcohol precipitation in step (c) is ethanol.

25. An acarus killing plant composition according to claim 1, wherein the temperature of the spray drying in step (c) is 30-50 ℃ and the pressure of the spray drying is 25-35MPa.

26. The acarus-killing plant composition of claim 1, wherein the pulverized cork tree bark of step (a) has a particle size of 100-200 mesh.

27. The acarus killing plant composition of claim 1, wherein the defatting treatment of step (a) is: pulverizing cortex Phellodendri, mixing with n-hexane, soaking, filtering, and drying to obtain defatted cortex Phellodendri powder.

28. The acarus-killing plant composition of claim 1, wherein the mass ratio of phellodendron amurense bark to n-hexane is 1 (1-3).

29. The mite-killing plant composition of claim 27, wherein said soaking time is from 2 to 4 hours and said soaking temperature is from 25 to 35 ℃.

30. The acarus killing plant composition of claim 1, wherein the aqueous ethanol solution of step (B) is 40-80wt% aqueous ethanol solution.

31. The acarus killing plant composition according to claim 1, wherein the time of the ultrasonic extraction in the step (B) is 30-90min, and the power of the ultrasonic extraction is 100-500W.

32. The acaricidal plant composition according to claim 1, wherein said dissolving in step (C) is carried out using an aqueous ethanol solution having a concentration of 5-15% by weight.

33. The acarus killing plant composition of claim 1, wherein the filling resin of the macroporous resin gel column in the step (C) is any one or a combination of at least two of D101, D4020, HPD-100, DM130 or HPD-400.

34. The acarus killing plant composition of claim 1, wherein the elution in step (C) is performed with an aqueous solution of ethanol having a concentration of 40 to 80 wt%.

35. The method of making an acarus killing plant composition of any one of claims 1-34, wherein the acarus killing plant composition is made by: mixing the extract of the red wood seeds, the extract of the pricklyash peel, the extract of the root of the lightyellow sophora root, the extract of the root of sessile stemona root and the extract of the bark of phellodendron amurense to obtain the acarus-killing plant composition.

36. The method of preparing an acarus killing botanical composition of claim 35 wherein the temperature of mixing is 20-40 ℃ and the time of mixing is 5-20min.

37. Use of the mite-killing plant composition of any one of claims 1-34 in the preparation of a cosmetic.

38. The use of claim 37, wherein said acarus-killing botanical composition is added in an amount of 0.05-10% of the total mass of said cosmetic.

39. A cosmetic product comprising the acarus killing botanical composition of any of claims 1-34.

40. The cosmetic as claimed in claim 39, wherein the cosmetic comprises any one of essence, face wash, shampoo or body wash.