CN113398055B - Silkworm excrement extract, preparation method thereof and application thereof in cosmetics - Google Patents

Silkworm excrement extract, preparation method thereof and application thereof in cosmetics Download PDF

Info

Publication number
CN113398055B
CN113398055B CN202110802651.2A CN202110802651A CN113398055B CN 113398055 B CN113398055 B CN 113398055B CN 202110802651 A CN202110802651 A CN 202110802651A CN 113398055 B CN113398055 B CN 113398055B
Authority
CN
China
Prior art keywords
silkworm excrement
application
extract
pure water
silkworm
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110802651.2A
Other languages
Chinese (zh)
Other versions
CN113398055A (en
Inventor
刘玉梅
周安
吴成亮
高先亭
张冬生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei Kadier Biotechnology Co ltd
Original Assignee
Hefei Kadier Biotechnology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hefei Kadier Biotechnology Co ltd filed Critical Hefei Kadier Biotechnology Co ltd
Priority to CN202110802651.2A priority Critical patent/CN113398055B/en
Publication of CN113398055A publication Critical patent/CN113398055A/en
Application granted granted Critical
Publication of CN113398055B publication Critical patent/CN113398055B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/63Arthropods
    • A61K35/64Insects, e.g. bees, wasps or fleas
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/18Antioxidants, e.g. antiradicals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P37/00Drugs for immunological or allergic disorders
    • A61P37/08Antiallergic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/005Preparations for sensitive skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Insects & Arthropods (AREA)
  • Epidemiology (AREA)
  • Zoology (AREA)
  • Immunology (AREA)
  • Animal Husbandry (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Pulmonology (AREA)
  • Biochemistry (AREA)
  • Birds (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)

Abstract

The application relates to a silkworm excrement extract and its preparation method and application in cosmetics, this silkworm excrement extract is to regard silkworm excrement as raw materials, after softening treatment, utilize the extractive solvent to heat reflux extraction, through filtering, get filtrate preparation, said extractive solvent is ethanol or pure water, the preparation method is to remove impurity of silkworm excrement, add pure water to soak, treat after it softens completely, mix extractive solvent and silkworm excrement after softening completely, heat reflux extraction, put cold filtration to get filtrate and filter residue, filter residue is extracted for 2-3 times repeatedly, mix filtrate, concentrate, place concentrate in vacuum freeze drier to make silkworm excrement lyophilized powder extract. The method has the advantages of simplicity, high efficiency, convenience, no use of toxic or harmful organic solvents and the like, can be widely applied to moisturizing, anti-aging, relieving, anti-allergy and skin care cosmetics, and provides a certain research basis for efficiently and systematically utilizing silkworm excrement resources, increasing the utilization rate of the silkworm excrement and better evaluating the application of the silkworm excrement in the cosmetic industry.

Description

Silkworm excrement extract, preparation method thereof and application thereof in cosmetics
Technical Field
The application belongs to the field of natural product chemistry, and particularly relates to a silkworm excrement extract, a preparation method thereof and application thereof in cosmetics.
Background
Silkworm excrement, called the vector, is the dry feces of silkworm moth larvae of insects belonging to the family Bombycis, the family Bombydae. The medicine is firstly carried in Ming Yi Bie Lu, has long history of taking medicine, can be taken orally and externally, and has wide effects. The description of Ben Cao gang mu: for diabetes, mass, metrorrhagia, wind-cold head and eyes, it is indicated for wind-damp-heat. The silkworm excrement has pungent and warm nature, enters liver and spleen channels, and has the effects of dispelling wind and removing dampness, harmonizing stomach and eliminating turbid pathogen, activating blood and removing obstruction in collaterals and the like. It is used for treating rheumatalgia, limb paralysis, and rheumatism pruritus. Modern pharmacological researches show that silkworm excrement has the activities of reducing blood fat, resisting tumors, reducing blood sugar, resisting oxidation, inhibiting bacteria, diminishing inflammation, resisting viruses and the like. China is a large country of silkworm resources, silkworm excrement is one of silkworm industry byproducts, a large amount of silkworm excrement is produced each year, and how to efficiently and reasonably utilize the silkworm excrement resources and reduce waste is an important point of research of modern scientists. The comprehensive utilization research of silkworm excrement is continuously developed in the 50 s of the 20 th century in China, and the silkworm excrement can be used as fertilizer and animal feed, and is widely applied to the aspects of crop production, medicine, food, health care and the like. Silkworm excrement is a product discharged by fresh mulberry leaves along with metabolic products in the silkworm body after the fresh mulberry leaves are eaten by silkworm, has various active ingredients and mainly comprises chlorophyll, pectin, flavonoids, alkaloids, lutein, crude protein, carbohydrates and the like.
The skin is the first line of defense for blocking the invasion of external harmful substances, wherein the moisture content of the horny layer at the outermost layer influences the dryness of the skin, the moisture content is between 10% and 20%, the skin is considered as the best state, and if the moisture content is lower than 10%, the skin is rough and dry. Moisture in the horny layer has an indispensable effect on maintaining skin health, inhibiting or slowing down aging, reducing the generation of wrinkles, and resisting external invasion. Allergy is also called allergy, and is an immune response generated by people with allergic constitution after contacting an allergen. Skin allergy is one of the most common skin problems. In recent years, problems such as skin allergy and aging have occurred due to changes in dietary structure, air pollution, and increases in pressure of life and work.
The existing silkworm excrement extraction technology mainly extracts chlorophyll, pectin, flavonoids and other components, and has a plurality of preparation processes and methods of silkworm excrement extracts, but the extraction process generally has the problems of high energy consumption, large solvent consumption, large loss of target active ingredients, long extraction time and the like, and is difficult to be applied to mass production. At present, research on the application of the silkworm excrement extract in cosmetics is not reported, and therefore, the silkworm excrement extract, the preparation method and the application thereof in cosmetics are provided.
Disclosure of Invention
The application aims to solve the problems and provide a silkworm excrement extract, a preparation method thereof and application thereof in cosmetics.
The application realizes the above purpose through the following technical scheme:
a silkworm excrement extract is prepared from silkworm excrement through softening, reflux extracting in alcohol or pure water, filtering, and extracting in solvent under heating.
As a further optimization scheme of the application, the silkworm excrement is faeces of silkworm larvae of the silkworm moth insects.
A method for preparing the silkworm excrement extract according to any of the above, comprising the steps of:
(1) Removing impurities from silkworm excrement, adding pure water for soaking treatment, and fully softening the silkworm excrement for later use;
(2) Mixing the extraction solvent with the fully softened silkworm excrement, heating, refluxing and extracting, cooling and filtering to obtain filtrate and filter residues;
(3) Adding an extraction solvent into the filter residue, and repeating the step (2) for 2-3 times;
(4) Combining the filtrates extracted in the steps (2) and (3), and concentrating to obtain a concentrated solution;
(5) And (3) performing vacuum freeze drying on the concentrated solution to obtain silkworm excrement extract freeze-dried powder.
As a further optimization scheme of the application, the ratio between the silkworm excrement and the solvent in the step (2) is 1:10-50.
As a further optimization scheme of the application, the concentration in the step (4) adopts a vacuum decompression rotary evaporator, the water bath temperature is controlled at 40-60 ℃, the rotating speed is 20-65 r/min, and the pressure is controlled at 0.1Mpa.
An application of the silkworm excrement extract in preparing cosmetics for moisturizing, resisting aging and relieving allergy.
As a further optimized scheme of the application, the silkworm excrement extract accounts for 1-10% of the total mass of the cosmetic composition.
As a further optimization scheme of the application, the cosmetics are facial masks, essence water, emulsion, cream, gel or spray.
The application aims at extracting silkworm excrement samples, firstly softens the silkworm excrement samples by water, and mainly aims to ensure that silkworm excrement active substances are extracted as much as possible.
The ratio of the solvent added in the application is most preferably 1:20-30.
The reflux extraction temperature of the present application is most preferably 85-90 ℃.
The application adopts the vacuum freeze dryer to prepare the silkworm excrement extract freeze-dried powder, and the method has high yield and good stability, and is convenient for long-term storage and transportation at normal temperature.
The silkworm excrement extract is used for preventing or treating skin wrinkles and fine lines caused by physiological or physical conditions.
The silkworm excrement extract is used for preventing or treating dry and rough skin.
The silkworm excrement extract is used for preventing or treating skin allergy.
The application has the beneficial effects that:
(1) The application adopts pure water or low concentration ethanol to extract silkworm excrement, can extract water-soluble active ingredient pectin and the like in silkworm excrement as much as possible, and prepares the freeze-dried powder through concentration and vacuum drying, has the advantages of simplicity, high efficiency, convenience, no use of toxic and harmful organic solvents and the like, and is easier to popularize and apply in production practice;
(2) The silkworm excrement extract obtained by the extraction method provided by the application has multiple biological effects of preserving moisture and resisting aging, relieving and resisting allergy and the like, and can be used for preparing cosmetics with the health care effects of preserving moisture and resisting aging, relieving and resisting allergy and the like.
Drawings
FIG. 1 shows DPPH radical elimination rate of silkworm excrement solution extracted by different solvents;
FIG. 2 shows the hyaluronidase inhibition rate of silkworm excrement solution extracted by using different solvents.
Detailed Description
The present application will be described in further detail with reference to the accompanying drawings, wherein it is to be understood that the following detailed description is for the purpose of further illustrating the application only and is not to be construed as limiting the scope of the application, as various insubstantial modifications and adaptations of the application to those skilled in the art can be made in light of the foregoing disclosure.
Example 1
The embodiment provides a preparation method of silkworm excrement extract, which comprises the following steps:
(1) Removing impurities from faeces Bombycis, adding 10 times of pure water, soaking, and softening completely;
(2) According to 1:10, mixing an extraction solvent (ethanol solution with volume concentration not exceeding 40% or pure water) with completely softened silkworm excrement, placing the mixture in a water bath kettle at 80 ℃ for heating reflux extraction for 1h, and cooling and filtering to obtain filtrate and filter residues;
(3) Adding 10 times of extraction solvent into the filter residue, and repeating the step (2) for 2 times;
(4) Mixing the filtrates obtained in (2) and (3), concentrating by vacuum reduced pressure rotary evaporator, controlling water bath temperature at 40deg.C, rotating speed 20 r/min, and pressure at 0.1Mpa to obtain concentrated solution;
(5) And (3) performing vacuum freeze drying on the concentrated solution to obtain silkworm excrement extract freeze-dried powder.
Example 2
The embodiment provides a preparation method of silkworm excrement extract, which comprises the following steps:
(1) Removing impurities from faeces Bombycis, adding 15 times of pure water, soaking, and softening completely;
(2) According to 1:20 (volume concentration of ethanol solution or pure water not exceeding 40%) and fully softened silkworm excrement are mixed, and then the mixture is placed in a water bath kettle at 85 ℃ for heating reflux extraction for 1h, and filtrate and filter residues are obtained after cooling and filtering;
(3) Adding 15 times of extraction solvent into the filter residue, and repeating the step (2) for 2 times;
(4) Mixing the filtrates obtained in (2) and (3), concentrating by vacuum reduced pressure rotary evaporator, controlling water bath temperature at 50deg.C, rotation speed 45 r/min, and pressure at 0.1Mpa to obtain concentrated solution;
(5) And (3) performing vacuum freeze drying on the concentrated solution to obtain silkworm excrement extract freeze-dried powder.
Example 3
The embodiment provides a preparation method of silkworm excrement extract, which comprises the following steps:
(1) Removing impurities from faeces Bombycis, adding 20 times of pure water, soaking, and softening completely;
(2) According to 1:50, mixing an extraction solvent (ethanol solution with volume concentration not exceeding 40% or pure water) with fully softened silkworm excrement, placing the mixture in a water bath kettle at 95 ℃ for heating reflux extraction for 1h, and cooling and filtering to obtain filtrate and filter residues;
(3) Adding 20 times of extraction solvent into the filter residue, and repeating the step (2) for 2 times;
(4) Mixing the filtrates obtained in (2) and (3), concentrating by vacuum reduced pressure rotary evaporator, controlling water bath temperature at 60deg.C, rotation speed 65 r/min, and pressure at 0.1Mpa to obtain concentrated solution;
(5) And (3) performing vacuum freeze drying on the concentrated solution to obtain silkworm excrement extract freeze-dried powder.
Example 4
To verify the effect of different extraction solvents on the components of the silkworm excrement extract, the embodiment provides a preparation method for extracting the silkworm excrement extract by using the different extraction solvents, which comprises the following steps of:
(1) Adding 20 times of pure water into 6 parts of purified silkworm excrement with the same mass for soaking treatment, and after the silkworm excrement is completely softened, keeping the silkworm excrement for later use;
(2) According to 1:20 portions of extraction solvent is respectively added into 6 portions of fully softened silkworm excrement, and the extraction solvent is YP1:100% ethanol, YP2:80% ethanol with 20% pure water, YP3:60% ethanol with 40% pure water, YP4:40% ethanol with 60% pure water, YP5:20% ethanol with 80% pure water, YP6:100% pure water, then, placing the mixture in a water bath kettle with the temperature of 85 ℃ for reflux extraction for 1h, cooling and filtering;
(3) Respectively collecting filtrate, respectively adding 10 times of pure water into six parts of filter residues, and repeatedly extracting for 2 times in the same way as in (2);
(4) Combining the filtrates extracted in (2) and (3), concentrating by vacuum reduced pressure rotary evaporator, controlling water bath temperature at 50deg.C, rotating speed 45 r/min, and pressure at 0.1Mpa to obtain 6 parts of concentrated solution;
(5) And respectively carrying out vacuum freeze drying on 6 parts of concentrated solution to obtain 6 parts of silkworm excrement extract freeze-dried powder test samples.
To verify the efficacy of 6 test samples of silkworm excrement extract freeze-dried powder, a series of verification experiments were made as follows:
irritation evaluation test
To examine the application prospect of the silkworm excrement extract in cosmetics, the irritation of the silkworm excrement extract prepared in examples 1-4 was examined by the method of SN/T2329-2013 cosmetic eye irritation/corrosiveness chick embryo chorioallantoic membrane test, and the results are shown in Table 1:
TABLE 1 test results of chick embryo chorioallantoic membrane test of silkworm excrement extract
According to the results of the chick embryo chorioallantoic membrane test, the silkworm excrement extracts prepared in examples 1-4 are all non-irritating.
Moisture efficacy test
The moisture retention test is usually carried out by adopting a weighing method, and the water loss rate is tested to reflect the moisture retention capacity of the humectant. The experiment was performed with a volume of saturated potassium carbonate solution to maintain a relative humidity of about 43%. The weight of the samples before and after the drying environment was weighed and the water loss rate was calculated. The smaller the water loss rate is, the stronger the water retention of the humectant is, and the better the long-term moisturizing effect is.
(1) Preparing silkworm excrement samples: 6 parts of silkworm excrement freeze-dried powder extracted by using different extraction solvents in example 4 are accurately weighed, placed in 50ml volumetric flasks respectively, water is added to fix the volume to the scale, and shaking is carried out uniformly, so that silkworm excrement solutions (YP 1, YP2, YP3, YP4, YP5 and YP 6) are obtained respectively.
(2) The experimental method comprises the following steps: 3ml of each sample solution was uniformly coated on a glass plate on which a 3M tape was stuck, and after being placed in an environment with relative humidity rh=43% for 72 hours to maintain constant weight, transferred to a dryer containing 200g of dry silica gel, and weighed after being placed for 4, 8, 12, 24 hours, respectively, and calculated according to the following formula:
wherein M0 is the mass of water before placement; m1 is the mass of water after a period of time.
TABLE 2 moisture retention rates at different time points for different solvent silkworm excrement extracts
(3) Analysis of moisturizing efficacy results:
as is clear from the data in Table 2, the moisturizing rate of YP6 was higher at 4-24 hours than the other groups, and reached 72.6% after 4 hours of leaving, and reached 46.2% at 24 hours, and YP5 and YP4 times, with YP3, YP2 and YP1 being worst, and the moisturizing rate of YP1 was only 31.9% after leaving for 24 hours.
Therefore, silkworm excrement extracted by using pure water as a solvent has a good moisturizing effect, and in addition, the moisturizing effect is weakened along with the increase of the concentration of ethanol, and mainly because the silkworm excrement water extract component is mainly polysaccharide, the polyhydroxy and carboxyl structures in the polysaccharide can form a hydrogen bond network with water molecules to lock water, and the expression of aquaporin and intermediate silk polyprotein is promoted to be increased, so that the skin epidermis barrier structure and the hydration function are maintained, and the moisturizing effect is achieved.
Human skin moisturizing efficacy experiment
Transepidermal water loss refers to water evaporating through the epidermis. TEWL an important parameter for evaluating skin barrier function, the more intact the skin barrier, the higher the moisture content and the lower the TEWL value, the test used the CK company Tewameter TM 300 to determine the transepidermal water loss rate of the skin surface in g/hm 2
The moisture content in the skin is primarily closely related to the ability of the stratum corneum to retain moisture, typically between 10% and 60%. The higher the moisture content, the lower the MMV value, for detection analysis using a Corneometer CM 825 type skin moisture detection probe.
(1) Preparing a test solution: 6 parts of silkworm excrement freeze-dried powder extracted by using different extraction solvents in the embodiment 4 are accurately weighed, 50mg of the silkworm excrement freeze-dried powder is respectively placed in 50ml volumetric flasks, water is added to fix the volume to scale, and shaking is carried out uniformly. Silkworm excrement solutions (YP 1, YP2, YP3, YP4, YP5, YP 6) were obtained, respectively.
(2) The experimental method comprises the following steps: skin transdermal moisture loss conditions and skin moisture levels were tested using the Tewameter TM 300, corneometer CM 825 test system, respectively. The room temperature of the test room is controlled at about 25 ℃, the relative humidity is constant between 35-55%, and the subjects should keep the organism in a stable state before the test, and 60 healthy volunteers are randomly divided into 3 groups. After wiping the arms of the subject with clear water at about 35 ℃, the test was started after sitting still for 30min in the test environment. Drawing a circular mark with the diameter of 3cm as a detected area by taking the position 8cm away from the wrist on the inner side of the arm of the subject as the center; respectively smearing 1ml of each sample solution to be measured on the three groups of left arm areas; 1ml of distilled water was applied to the same position of the right forearm as a blank group, and the skin moisture loss value and the skin moisture content value of the test area were measured before use, 0.5h, 1h, 2h, 4h, and 8h, respectively, and the average value was calculated for each group. The specific data are shown in Table 3:
TABLE 3 skin moisture loss values before and after application of silkworm excrement solution
(3) Analysis of water loss results:
the results of the variation of the skin-penetrating epidermis dispersion values before and after application are shown in Table 3, and the skin-penetrating epidermis dispersion values before and after application are changed, wherein the YP6 water-penetrating epidermis dispersion value reaches 6.11, and the water-penetrating epidermis dispersion value is reduced by 20.5% compared with that before application. Therefore, the silkworm excrement extract obtained by using pure water as an extraction solvent has a good moisturizing effect.
TABLE 4 moisture content of skin before and after application of silkworm excrement solution
(4) Skin moisture content results analysis:
the results of the change of the skin moisture content before and after application are shown in Table 4, the skin moisture content reaches the maximum and is more than 48 after each silkworm excrement liquid is used for 0.5h, wherein the skin moisture content of YP6 group reaches 53.43, and the skin moisture content is respectively increased by 58.8% compared with the skin moisture content before use. After 8h of application, the skin moisture content of YP6 group was 47.24, and the skin moisture content was increased by 40.2%. Therefore, the silkworm excrement extract obtained by extracting silkworm excrement with pure water as a solvent has a good moisturizing effect.
In vitro antioxidant experiment (DPPH free radical method)
DPPH is a nitrogen-centered stable radical whose absolute ethanol solution exhibits a maximum absorption at a wavelength of 517 nm. In the presence of a radical scavenger, DPPH may be combined or replaced to reduce the number of radicals resulting in a decrease in absorbance.
(1) Preparing a test solution: accurately weighing DPPH 3.0mg, placing into a 10ml volumetric flask, adding a small amount of absolute ethyl alcohol to dissolve, fixing volume to scale, and shaking uniformly. And (3) putting the mixture into a volumetric flask with volume ranging from 2ml to 100ml, and shaking uniformly to obtain DPPH with the concentration of 0.006 mg/ml.
6 portions of silkworm excrement freeze-dried powder extracted by using different extraction solvents in example 4 are accurately weighed, and 50ml of each of the silkworm excrement freeze-dried powder is placed for later use, and the solutions are marked as YP1, YP2, YP3, YP4, YP5 and YP 6.
(2) The experimental method comprises the following steps: 3.0ml DPPH solution and 0.5ml each sample solution are added into the sample tube; 3.0ml of ethanol solution and 0.5ml of each sample solution were added to the control tube; the positive control group was added with 3.0ml DPPH solution and 0.5ml vitamin C solution 15. Mu.g/ml; 3.0ml of DPPH solution and 0.5ml of pure water are added into a blank tube, after being uniformly mixed and protected from light for 30min, 3.0ml of ethanol and 0.5ml of distilled water are used for zeroing, and the light absorption value is measured at the wavelength of 517 nm; let 3 replicates, average and calculate radical clearance (%) as follows:
(3) In vitro antioxidant results analysis:
as shown in FIG. 1, the DPPH of YP6 has the best effect of scavenging free radicals, YP5, YP4 and YP3 times, and YP2 and YP1 are the worst, so that the silkworm excrement extract prepared by using pure water as an extraction solvent has strong free radical scavenging ability and strong oxidation resistance.
Hyaluronidase activity inhibition assay
Hyaluronidase is a participant of type I allergic reaction, has strong correlation with inflammation and allergy, and researches report that various medicines for releasing histamine from fat large cells can regulate the activity of the hyaluronidase, and some anti-allergic medicines have strong inhibition of the activity of the hyaluronidase, so that the inhibition of the activity of the hyaluronidase is used as an index for researching anti-allergic effect.
(1) Preparing a test solution: acetic acid buffer: solution a: 11.55ml of acetic acid is dissolved in 1000ml of distilled water; solution B:27.2g of sodium acetate trihydrate are dissolved in 1000ml of distilled water. Respectively taking 48ml of solution A and 45.2ml of solution B, mixing and diluting to 1L, and preparing an acetic buffer solution with PH=5.6;
hyaluronidase: 16.5mg of 303U/mg of hyaluronic acid are weighed into a 10ml volumetric flask, dissolved by adding acetic acid buffer and the volume is fixed to the scale. Can not be used for a night after being newly manufactured;
sodium hyaluronate: weighing 50mg of sodium hyaluronate, placing in a 100ml volumetric flask, adding acetic acid buffer solution to dissolve and fixing the volume to the scale;
acetylacetone solution: 50ml of 1.0mol/L sodium carbonate solution and 3.5ml of acetylacetone solution were mixed uniformly and used for fresh preparation.
DAB color developer: 0.8g of p-dimethylaminobenzaldehyde is dissolved in 15ml of concentrated hydrochloric acid and 15ml of absolute ethyl alcohol and uniformly mixed.
Calcium chloride solution: 27.75g of calcium chloride is weighed and placed in a 100ml volumetric flask, distilled water is added to dissolve the calcium chloride and the volume is fixed to the scale, and the calcium chloride is obtained.
Sodium hydroxide solution: weighing 20g of sodium hydroxide, placing in a 100ml volumetric flask, adding distilled water to dissolve and fixing the volume to a scale; obtaining the product.
(2) The experimental method comprises the following steps: 6 parts of silkworm excrement freeze-dried powder extracted by using different extraction solvents in example 4 were accurately weighed and respectively placed in 50ml for later use, and the solutions marked as YP1, YP2, YP3, YP4, YP5 and YP6 were marked. The specific experimental steps are as follows:
the corresponding test solutions were added to the test tubes as shown in the table, thoroughly shaken, left at 30℃for 30min, transferred to 96-well plates, and absorbance was measured at 530 nm. The specific formula is as follows:
a: (hyaluronidase + sample + sodium hyaluronate) OD value of the sample solution;
b: (acetate buffer + sample + acetate buffer) OD value of sample blank;
c: OD value of (hyaluronidase + deionized water + sodium hyaluronate) control solution;
d: (acetate buffer + deionized water + acetate buffer) to control the OD value of the blank;
(3) Analysis of hyaluronidase activity inhibition results:
as shown in FIG. 2, the results of the test show that YP6 has the best hyaluronidase inhibitory effect, YP5, YP4 and YP3 times, and YP2 and YP1 are the worst, and the hyaluronidase inhibitory rate decreases with increasing ethanol concentration. The silkworm excrement hyaluronidase inhibition rate prepared by taking pure water as an extraction solvent is high and reaches 84.4%, so that the silkworm excrement extract extracted by taking pure water as the solvent has high antiallergic capability.
Phosphoric acid itch threshold test
Histamine is released when the skin is damaged or an inflammatory, allergic reaction occurs. Histamine has a strong vasodilating effect, increasing the permeability of the capillary walls, leading to local tissue oedema.
(1) The experimental method comprises the following steps: guinea pigs were randomly divided into 8 groups of 10 animals each, a blank control group, a positive control group and a sample group. The day before the test, the right hind dorsum of each group of guinea pigs was sampled once. On the day of the test, the animals were scratched with coarse sand paper at the shaved parts of the backs of the right feet, about 1cm 2 Around the range, the sample was applied once more, and the blank group was given an equal amount of distilled water. After 10 minutes, 0.01% histamine phosphate 0.05 ml/dose was initially applied to the wound surface, and the concentration was increased by 0.01%,0.02%,0.03%, and 0.04% … … every 3 minutes thereafter, each 0.05 ml/dose. Until the right hind paw is licked by the guinea pig, the total amount of the histamine phosphate which is given when the right hind paw is licked by the guinea pig finally is taken as the itching threshold. The itch threshold of each group was recorded and compared.
TABLE 5 influence of samples on the itching response of histamine phosphate
(2) Analysis of the results of the phosphoric acid itch threshold:
as is apparent from the data in Table 5, the silkworm excrement extract prepared by using pure water as an extraction solvent according to the present application has a good antipruritic effect on itch caused by allergy.
As shown in experimental results, the silkworm excrement extract prepared by heating and reflux extraction with pure water as an extraction solvent has higher moisture retention rate, DPPH free radical rate, hyaluronidase inhibition rate and influence on itching reaction of the histamine phosphate than silkworm excrement extracts prepared by other extraction solvents;
the extraction method provided by the application has the advantages of simplicity, high efficiency, convenience, no toxic or harmful organic solvent, and the like, the production practice is easier to popularize and apply, and the silkworm excrement extract obtained by the method has multiple biological effects of preserving moisture, resisting aging, relieving allergy and the like, and can be used for preparing cosmetics with the health care effects of preserving moisture, resisting aging, relieving allergy and the like.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application.

Claims (4)

1. The application of silkworm excrement extract in preparing cosmetics with functions of moisturizing, resisting aging and relieving allergy is characterized by comprising the following steps: the preparation method of the silkworm excrement extract specifically comprises the following steps:
(1) Removing impurities from silkworm excrement, adding pure water for soaking treatment, and fully softening the silkworm excrement for later use;
(2) Mixing pure water with fully softened silkworm excrement, heating, reflux-extracting, cooling and filtering to obtain filtrate and filter residue, wherein the ratio of the silkworm excrement to the pure water is 1:20-30 parts;
(3) Adding pure water into the filter residue, and repeating the step (2) for 2-3 times;
(4) Combining the filtrates extracted in the steps (2) and (3), and concentrating to obtain a concentrated solution; wherein, the concentration adopts a vacuum decompression rotary evaporator, the water bath temperature is controlled at 40-60 ℃, the rotating speed is 20-65 r/min, and the pressure is controlled at 0.1Mpa;
(5) Vacuum freeze drying the concentrated solution to obtain silkworm excrement extract.
2. The application of silkworm excrement extract in preparing cosmetics with moisturizing, anti-aging, and anti-allergy effects according to claim 1, wherein the application is characterized in that: the faeces Bombycis is faeces Bombycis larva of Bombycis mori.
3. The application of silkworm excrement extract in preparing cosmetics with moisturizing, anti-aging, and anti-allergy effects according to claim 1, wherein the application is characterized in that: the silkworm excrement extract accounts for 1-10% of the total mass of the cosmetic composition.
4. The application of silkworm excrement extract in preparing cosmetics with moisturizing, anti-aging, and anti-allergy effects according to claim 1, wherein the application is characterized in that: the cosmetic is facial mask, essence water, lotion, cream, gel or spray.
CN202110802651.2A 2021-07-15 2021-07-15 Silkworm excrement extract, preparation method thereof and application thereof in cosmetics Active CN113398055B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110802651.2A CN113398055B (en) 2021-07-15 2021-07-15 Silkworm excrement extract, preparation method thereof and application thereof in cosmetics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110802651.2A CN113398055B (en) 2021-07-15 2021-07-15 Silkworm excrement extract, preparation method thereof and application thereof in cosmetics

Publications (2)

Publication Number Publication Date
CN113398055A CN113398055A (en) 2021-09-17
CN113398055B true CN113398055B (en) 2023-08-22

Family

ID=77686556

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110802651.2A Active CN113398055B (en) 2021-07-15 2021-07-15 Silkworm excrement extract, preparation method thereof and application thereof in cosmetics

Country Status (1)

Country Link
CN (1) CN113398055B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100781553B1 (en) * 2006-11-30 2007-12-03 김애정 Composition of beauty soap and process of it
CN106265445A (en) * 2016-09-13 2017-01-04 广西顺帆投资有限公司 Exfoliation pore refining facial film and preparation method thereof
CN109157486A (en) * 2018-11-07 2019-01-08 长沙浩然医疗科技有限公司 A kind of Anti-hair loss promotes the composition and preparation method thereof of hair tonic
CN110934810A (en) * 2019-12-13 2020-03-31 广州市永添生物科技有限公司 Preparation method of whitening and freckle-removing cream

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100781553B1 (en) * 2006-11-30 2007-12-03 김애정 Composition of beauty soap and process of it
CN106265445A (en) * 2016-09-13 2017-01-04 广西顺帆投资有限公司 Exfoliation pore refining facial film and preparation method thereof
CN109157486A (en) * 2018-11-07 2019-01-08 长沙浩然医疗科技有限公司 A kind of Anti-hair loss promotes the composition and preparation method thereof of hair tonic
CN110934810A (en) * 2019-12-13 2020-03-31 广州市永添生物科技有限公司 Preparation method of whitening and freckle-removing cream

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
高学敏等.《中华医学百科全书 中药学》.中国协和医科大学出版社,2017,第121页. *

Also Published As

Publication number Publication date
CN113398055A (en) 2021-09-17

Similar Documents

Publication Publication Date Title
CN107349170B (en) Folium artemisiae argyi mosquito-repelling itching-relieving floral water and preparation method thereof
CN104306358B (en) Antipruritic scar liniment of dispelling
CN111388376B (en) Jasmine herbal anti-allergy soothing mask and preparation method thereof
CN113476368A (en) Soothing and repairing composition and preparation method thereof
CN115919722A (en) Pandanus communis leaf extract and preparation method and application thereof
CN111494466A (en) A topical composition containing Cannabis sativa extract and its application
CN113398055B (en) Silkworm excrement extract, preparation method thereof and application thereof in cosmetics
JP5196416B2 (en) Cosmetic composition containing Limnocitrus litoritalis extract
CN115154363B (en) Mulberry resource oligosaccharide moisturizing composition and preparation method and application thereof
CN110711161A (en) Leave-on allergy-relieving repair essence mask
CN115919686A (en) Skin soothing lotion for enhancing skin barrier and preparation method thereof
CN113940896B (en) Anti-aging skin repair liquid containing vitamin A alcohol and preparation method thereof
CN115770209A (en) Rod-shaped lithospermum ointment containing three-purple oil and preparation method thereof
CN114404466A (en) Izodin-based nasal cavity repairing composition and preparation method thereof
CN115177975A (en) A method for extracting polysaccharides, polyphenols and triterpenes from medicinal fomes fomentarius by supramolecular process
CN108078868A (en) A kind of antiallergic composition for skin care item
JP4450406B2 (en) A topical skin preparation containing Benicami kirifras as an active ingredient
KR101463841B1 (en) Cosmetic composition containing fermented extracts with salt
CN114886794B (en) Composition with anti-inflammatory and antioxidant effects and application thereof
TWI838291B (en) Use of extract of pilea microphylla for manufacturing anti-inflammatory preparations
EP2841079B1 (en) New compositions for the treatment of chronic ulcers
CN113368164B (en) Anti-allergy traditional Chinese medicine formula leavening, preparation method and application thereof in cosmetics
CN114886807B (en) Composition with omnibearing skin barrier repairing function and preparation method and application thereof
CN115282168B (en) Soothing skin cream for relieving infant eczema symptoms and preparation method and application thereof
CN114762709B (en) Plant essential oil for improving sleep and preparation method and application method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant