CN110559391B - Eye patch containing polygonatum polysaccharide - Google Patents

Eye patch containing polygonatum polysaccharide Download PDF

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CN110559391B
CN110559391B CN201910968140.0A CN201910968140A CN110559391B CN 110559391 B CN110559391 B CN 110559391B CN 201910968140 A CN201910968140 A CN 201910968140A CN 110559391 B CN110559391 B CN 110559391B
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polygonatum
extract
polysaccharide
eye patch
parts
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CN110559391A (en
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彭腾
陈胡兰
何沛煜
张军银
吴明一
高天宇
王迎香
赵永艳
邓赟
谭玉柱
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Chengdu University of Traditional Chinese Medicine
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56—Materials from animals other than mammals
    • A61K35/618—Molluscs, e.g. fresh-water molluscs, oysters, clams, squids, octopus, cuttlefish, snails or slugs
    • A—HUMAN NECESSITIES
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    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8969—Polygonatum (Solomon's seal)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
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    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
    • A61K9/7023—Transdermal patches and similar drug-containing composite devices, e.g. cataplasms
    • A—HUMAN NECESSITIES
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    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention discloses an eye patch containing polygonatum polysaccharide, which is provided with a backing substrate layer, a gel layer and a protective film, wherein the gel layer is hydrogel taking sodium hyaluronate as a main component; the gel layer contains 3-20wt% of natural active ingredient extract; the natural active ingredient extract comprises rhizoma Polygonati polysaccharide extract and snail extract; the ratio of rhizoma Polygonati polysaccharide is more than or equal to 60 wt%. The eye patch containing the polygonatum polysaccharide is prepared into hydrogel by adopting natural active ingredients, is good in moisture retention and water retention, mild and non-irritant, can improve blood circulation of tissues around eyes, and has a remarkable effect of relieving eye tissue fatigue.

Description

Eye patch containing polygonatum polysaccharide
Technical Field
The invention relates to an eye patch, in particular to an eye patch containing polygonatum sibiricum polysaccharide, and belongs to the technical field of polygonatum sibiricum downstream industries.
Background
In modern life and work, the connection between various activities of human beings and displays is more and more compact, and the time of people facing the displays every day is greatly increased compared with the last century. The display is excited by voltage or current to display and emit different light rays to realize image display, and compared with natural environment light, the electronic display generates a large amount of blue light waves which easily cause visual cell fatigue in a spectrum, so that the visual fatigue problem of a user is more and more prominent.
Usually, people have a bad feeling of dizziness after watching the display for a long time, which is a physiological reason of human body on one hand and a limitation of the light-emitting spectrum characteristic of the display on the other hand. If not corrected in a timely manner, asthenopia can gradually develop into myopia, resulting in blurred images of the world viewed by the human eye.
The display technology in the prior art is slow in development and can only relieve the asthenopia problem by optimally adjusting the recovery of human body to the asthenopia. At present, the methods mainly adopted for relieving the visual fatigue comprise hot compress, cold compress, medicinal eye patches and the like, wherein the hot compress/cold compress belongs to the traditional visual fatigue relieving method, and the effects of promoting the blood circulation of eyes by mainly utilizing temperature stimulation and improving the visual fatigue are achieved.
The medicinal eye patch is classified into a gel eye patch containing an active ingredient and a gel eye patch containing no active ingredient. Wherein, the eye patch without medicinal components is similar to cold compress, stimulates the skin through gel to promote the eye blood circulation, and achieves the effect of improving asthenopia. The eye patch containing the active pharmaceutical ingredients can give consideration to both gel stimulation and pharmaceutical effects, commonly-used medicines comprise anthocyanin, taurine, lutein, beta-carotene, retinol and other known nutritional ingredients with positive effects on protecting eyesight, and the eye patch products are generally stated to be capable of providing necessary nutritional factor supplement for eyes so as to achieve the effects of relieving asthenopia and improving eyesight.
However, in these gel eye patch products containing drugs, the active ingredients of the drugs are solidified by the gel matrix, and the drugs are often difficult to penetrate the skin tissues of the eyes due to the skin barrier effect, and cannot be effectively absorbed and utilized. The effect that the medicine eye patch can actually achieve is only the conventional cold compress effect, and the effect of improving the visual fatigue is very limited.
The traditional Chinese herbal medicine science of China considers that eyes and twelve meridians are closely related, and if the eyes are well conditioned, the eye health care tea has good promoting effects on relaxing and activating the channels and collaterals, regulating qi and blood, promoting blood circulation and the like.
Rhizoma Polygonati (Polygonatum sibiricum), also called Kadsura japonica and Kadsura japonica, is the dried tuber of various plants in Polygonatum of Liliaceae. Rhizoma Polygonati has effects of replenishing kidney essence, nourishing yin, invigorating middle warmer, invigorating qi, and prolonging life. If the effects of the rhizoma polygonati for tonifying middle-jiao and Qi can be acted on eyes to relieve asthenopia, the method has prominent and excellent value significance for regulating and relieving asthenopia in modern life.
At present, no report about the application of intensive research on polygonatum sibiricum to eye patch products exists, if polygonatum sibiricum can be developed and applied to the eye patch industry, the eye patch can help to improve the asthenopia of a large number of sub-health people, can also help the polygonatum sibiricum planting industry to further develop new branch industry in a deepening manner, and has great significance for promoting the polygonatum sibiricum industry.
Disclosure of Invention
The invention aims to overcome the defect that active ingredients in a medicinal eye patch product in the prior art are difficult to permeate, absorb and utilize, and provides an eye patch containing polygonatum polysaccharides.
In order to achieve the above purpose, the invention provides the following technical scheme:
an eye patch containing rhizoma Polygonati polysaccharide comprises backing substrate layer, gel layer and protective film;
the gel layer is hydrogel taking sodium hyaluronate as a main component;
the gel layer contains 3-20wt% of natural active ingredient extract;
the natural active component extract comprises rhizoma Polygonati polysaccharide extract and snail extract; the ratio of rhizoma Polygonati polysaccharide is more than or equal to 60 wt%.
The eye patch product containing the polygonatum polysaccharide adopts a polygonatum polysaccharide extract as an active ingredient, wherein the polygonatum polysaccharide mainly comprises fructose, galactose and glucose, the MW molecular weight is 5000-.
The eye patch product containing rhizoma Polygonati polysaccharide has gel layer adhered to the backing substrate layer, and protective film adhered to the surface of the gel layer to form the eye patch product. When the eye-protecting mask is used, the protective film is removed, the gel layer is attached to eyes, the effect of relieving the asthenopia is exerted, and the eye-protecting mask simultaneously has the effect of relieving the asthenopia through the cold compress of the hydrogel and the effect of relieving the asthenopia through the natural active ingredients.
Wherein the snail extract, named as snail mucus extract, snail extract, and snail secreted mucus, contains collagen, elastin, glucuronic acid, and vitamins. The snail extract has effects of promoting skin penetration, healing skin, resisting bacteria and diminishing inflammation. When the snail moves and reduces friction, the secreted mucus has no biological activity, and when the snail is under pressure, the defense mechanism of the snail promotes the secreted mucus to be a polysaccharide complex, so that the injury of the epidermis can be repaired. Abundant complex actives can help to rapidly repair and maintain skin moisture.
The compendium of materia medica records that snails cure diseases, and modern traditional Chinese medicine also recognizes that snails have the functions of clearing heat, detoxifying, detumescence, treating diabetes and the like. Snail mucus was recorded by Hipporates, a father of ancient Greek medicine, as having moisturizing, red swelling eliminating, anti-inflammatory, and analgesic effects, and used with cow milk for treating skin scars. In the aspect of modern cosmetic application, the snail secretion filtrate can effectively lighten skin lines and scars, repair skin wounds, accelerate the synthesis of collagen, enhance the skin elasticity and increase the skin repair force. The independent application of the snail extract has a plurality of medical and cosmetic application values, and if the efficacy value of the snail extract can be deeply excavated, the whole value significance of the snails can be better exerted.
Further, the gel layer contains 6-16% of natural active ingredient extract, such as 7%, 8%, 10%, 12%, 13%, 14%.
Preferably, the content of polygonatum polysaccharide in the natural active ingredient extract is more than or equal to 60 wt%. For example, the content of the polygonatum polysaccharide is more than or equal to 70 wt%, or the content of the polygonatum polysaccharide is more than or equal to 80 wt%, or the content of the polygonatum polysaccharide is more than or equal to 90 wt%.
Further, the natural active ingredient extract further comprises at least one of: rhizoma Polygonati Odorati extract, and fructus Citri Sarcodactylis extract.
Preferably, the weight percentages of the various components in the natural active ingredient extract are as follows: 60-95% of rhizoma polygonati polysaccharide extract, 1-10% of snail extract, 0-15% of polygonatum extract and 0-10% of fingered citron extract.
Further, the polygonatum polysaccharide extract is a polygonatum polysaccharide extract extracted from the polygonatum which is steamed and dried in the sun.
Preferably, the rhizoma polygonati subjected to primary steaming and primary airing is the rhizoma polygonati subjected to primary steaming and primary airing.
Further, the polygonatum polysaccharide is a polygonatum polysaccharide component obtained by water extraction and alcohol precipitation.
Preferably, the polygonatum polysaccharide is a polygonatum polysaccharide component obtained by performing water extraction and alcohol precipitation on polygonatum and performing precipitation under the concentration of 60-80 v% ethanol.
Further, the extraction method of the polygonatum polysaccharide comprises the following steps:
s101, taking the rhizoma polygonati which is steamed and sun-dried once, adding 10 times of water for decocting for 2 times, each time for 30 minutes, combining extracting solutions, and concentrating the filtrate to 0.7-2 times of the weight of the rhizoma polygonati which is steamed and sun-dried once.
S102, adding ethanol to enable the content of the ethanol in the filtrate obtained after concentration in the step S101 to reach 60v%, and filtering to remove precipitates; and continuously adding ethanol into the filtrate to ensure that the content of the ethanol in the filtrate reaches 80v%, and collecting the precipitate to obtain the polygonatum polysaccharide extract.
The rhizoma polygonati polysaccharide extract added and applied in the rhizoma polygonati eye paste product is an active ingredient obtained by extracting and separating 60-80 v% ethanol, has high activity, and is more suitable for promoting the transfer of nutritional factors in the eye paste.
Further, the sealwort is polygonatum cyrtonema. The name learning: polygonatum cyrtonema Hua is a perennial herb of Polygonatum of Liliaceae.
Preferably, the rhizoma polygonati which is steamed and dried in the sun is obtained by processing the following steps: (1) cleaning fresh rhizoma Polygonati, removing beard, air drying or air drying; (2) slicing rhizoma Polygonati to 2-4mm thick; (3) and (3) putting the sliced rhizoma polygonati into a steamer to steam for 4h, then turning off the fire to stew for 2h, then taking out the slices to dry at the temperature of 40-80 ℃ to obtain the steamed and sunned rhizoma polygonati.
Further, the gel layer is hydrogel, and the main components of the hydrogel are the following components in parts by weight: 10-20 parts of sodium hyaluronate, 2-4 parts of sodium polyacrylate, 3-5 parts of carbomer, 10-15 parts of glycerol and 40-80 parts of water.
The hydrogel adopts sodium hyaluronate, sodium polyacrylate and carbomer as main gel material components, and the sodium hyaluronate is a natural moisturizing lubricant component, has a good moisturizing effect on skin, and can play a role in promoting eye blood circulation through cold compress. In addition, sodium hyaluronate is often used as a cosmetic material, can well promote skin smoothness and tenderness, and has a good effect on caring eye skin. On the basis of the sodium hyaluronate, carbomer and sodium polyacrylate are also applied, and the carbomer has good skin affinity and good fitting property, is more favorable for fitting lubrication of an eye gel-sticking layer and eye skin, and is favorable for releasing active ingredients to act on the eye skin.
Preferably, the main components of the hydrogel are the following components in parts by weight: 12-18 parts of sodium hyaluronate, 2-3 parts of sodium polyacrylate, 3-4 parts of carbomer, 5-13 parts of glycerol and 50-60 parts of water.
Further, the Sodium Hyaluronate (Sodium Hyaluronate) is at least one of food grade Sodium Hyaluronate and injection grade intermediate Sodium Hyaluronate. Sodium hyaluronate, CAS No.: 9067-32-7 in the form of white or white-like granule or powder, adding water, mixing to obtain sodium hyaluronate gel, coating on the substrate layer of the backing to obtain sodium hyaluronate gel layer, and adding rhizoma Polygonati polysaccharide extract into the sodium hyaluronate gel to obtain eye patch active ingredient.
Preferably, the sodium hyaluronate has a nitrogen content of 2.8-4.0 wt%, a glucuronic acid content of more than or equal to 37.0%, preferably, a glucuronic acid content of more than or equal to 40% (mass fraction), and more preferably, a glucuronic acid content of 45-51%. Is widely used in the field of cosmetics and has the function of moisturizing.
Preferably, the pH value of the sodium hyaluronate is 6.0-7.5.
Preferably, the sodium hyaluronate has an intrinsic viscosity of 2.0-5.0 m3/kg。
Preferably, the carbomer is carbomer 940, and the 0.5% concentration of carbomer is within about 63000mpa.s ± 20%.
Compared with the prior art, the invention has the beneficial effects that:
1. the eye patch containing the polygonatum polysaccharide adopts 3-20% of polygonatum polysaccharide extract as an active ingredient in the gel layer, has excellent promotion effect on relieving eye tissue fatigue, and tests show that the polygonatum polysaccharide eye patch product can improve blood circulation of periocular tissues and relieve visual fatigue.
2. The eye patch product of the invention is added with natural active ingredients and also comprises snail extracting solution, and the snail extracting solution is rich in active ingredients such as polysaccharide, protein, glycogen and the like, and has the effects of promoting wound healing, integrating effect restoration, deeply nourishing and the like. The compound active component is formed by adding a small amount of snail extracting solution and the polygonatum polysaccharide extract, so that the effect of improving the visual fatigue is better exerted, and compared with the effect of improving the tissue blood flow rheology which is not achieved by singly applying the snail extracting solution, the snail extracting solution and the polygonatum polysaccharide extract can play a good role in promoting and enhancing after being compounded and combined.
3. The gel material adopted by the eye patch product has high moisture content, good moisture retention and water retention, is mild and non-irritant, and can well improve the dry and water-deficient state of tissues around eyes.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.
In the present invention, the percentage of ethanol concentration is a volume percentage, and the other percentages not specifically mentioned are weight percentages.
Injection grade intermediate sodium hyaluronate, guanong biological products factory of carumurus city.
Superoxide dismutase (SOD) test KIT, SOD (HY-60001) KIT, Shanghai Yubo Biotech Co., Ltd.
The reagent used in the invention is preferentially analytically pure, and the analytically pure chemical purity cannot be obtained.
The basic information on the reagents, raw materials and the like used in the following examples and comparative examples is as follows:
carbomer, carbomer 940, the 0.5 wt.% concentration carbomer was about 63000 mpa.s.
Sodium polyacrylate, MW 8000.
Medical breathable non-woven fabric, BJS 12cm, Shandong Xiaokang Biotech Co., Ltd.
Fingered citron extract, brand koman organism. Appearance: a brown-yellow powder; the effective components are as follows: caprolactone, lemon lactone, hesperidin, buciloside, etc. Production enterprises: shanxi Korman Biotech Co., Ltd.
The snail extract used in the invention is sold as snail mucus extract, and the production area is as follows: korea, brand: bairand Bioland, the content is more than or equal to: 99.5 (%); pH value: 6.5-8.5, solubility: dissolving in water.
< example 1>
Hydrogel formulation
The preparation method comprises the following steps: adding sodium hyaluronate into about 1/2 water, soaking for 24h, and dissolving completely to obtain sodium hyaluronate gel. Adding sodium hydroxide into the residual 1/2 water to prepare sodium hydroxide solution with the concentration of about 5 wt%, uniformly mixing sodium polyacrylate and carbomer 940, adding the mixture into the sodium hydroxide solution, and swelling overnight to obtain carbomer gel. And mixing the dissolved sodium hyaluronate solution with carbomer gel, adding glycerol, fully and uniformly stirring, and defoaming in vacuum to obtain the hydrogel.
Formulation of hydrogel a 1: weighing the following components, 15 g of sodium hyaluronate, 2.5 g of sodium polyacrylate, 3g of carbomer, 13 g of glycerol and 58 g of water. The hydrogel was prepared according to the above hydrogel preparation method.
Formulation of hydrogel a 2: weighing the following components, 15 g of sodium hyaluronate, 2g of sodium polyacrylate, 3.5 g of carbomer, 12.5 g of glycerol and 55 g of water. The hydrogel was prepared according to the above hydrogel preparation method.
Formulation of hydrogel a 3: the following ingredients, sodium hyaluronate 16 g, sodium polyacrylate 3g, carbomer 2.5 g, glycerin 10 g, and water 53 g, were weighed. The hydrogel was prepared according to the above hydrogel preparation method.
Formulation hydrogel B1: weighing the following components, 15 g of sodium hyaluronate, 3g of carbomer, 13 g of glycerin and 58 g of water. The hydrogel was prepared according to the above hydrogel preparation method.
The hydrogel A1, A2, A3 and B1 are prepared according to the hydrogel preparation method, the amount of sodium hydroxide is added according to the need of neutralizing carbomer, and the gel is neutral (pH is approximately 7.0) after the carbomer 940 is fully swelled.
Formulation hydrogel B2: the following ingredients, 15 g of sodium hyaluronate, 2.5 g of sodium polyacrylate, 13 g of glycerol and 58 g of water, were weighed. Adding sodium hyaluronate into about 1/2 water, soaking for 24h, and dissolving completely to obtain sodium hyaluronate gel. The sodium polyacrylate was added to the remaining about 1/2 water and dissolved thoroughly to give a sodium polyacrylate gel. And mixing the dissolved sodium hyaluronate solution with the sodium polyacrylate gel, adding glycerol, fully and uniformly stirring, and performing vacuum defoaming to obtain the hydrogel B2.
The hydrogels A1, A2, A3, B1 and B2 all present transparent uniform gel forms and have better uniformity. In order to examine the water retention performance of different hydrogels, the gel materials were placed in a hot air oven at 80 ℃ and dried for 2h, and the water retention performance of the hydrogels was compared.
The water retention rate was calculated from the change in weight before and after the drying treatment, i.e., m1 after the drying treatment/m 0 × 100% before the drying treatment, and the water retention properties of the respective hydrogels were as shown in the following table.
TABLE 1 hydrogel Water holding Properties
Weight m0 before drying treatment Weight m1 after drying treatment Water retention rate
Hydrogel A1 10.12 7.89 78％
Hydrogel A2 11.02 8.92 81％
Hydrogel A3 10.35 8.17 79％
Hydrogel B1 10.12 7.28 72％
Hydrogel B2 10.21 7.75 76％
The test result of the water retention performance of the hydrogel shows that the water retention of the hydrogels with different formulas are slightly different, and the hydrogel has good water retention performance on the whole and can be used as the basic gel material of the eye patch. The gel materials applied by the components selected from the hydrogel B1 and the hydrogel B2 lack sodium polyacrylate and carbomer respectively, the water retention performance of the gel is reduced, and the gel matrix material is compounded by multiple components, so that the overall water retention performance and stability are facilitated.
< example 2>
Preparation method of sealwort by steaming and sun drying
The specific processing method for steaming and sunning the polygonatum sibiricum comprises the following steps: cleaning fresh rhizoma Polygonati, removing beard, air drying or air drying. Slicing rhizoma Polygonati to 2-4mm thick. Steaming in a steamer for 4h, stewing for 2h with a closed fire, taking out and drying at 60 ℃ to obtain the steamed and dried rhizoma polygonati.
Extraction of polygonatum polysaccharide
Taking 100 g of steamed and sun-dried rhizoma polygonati, adding 10 times of water for decocting for 2 times, each time for 30 minutes, combining extracting solutions, concentrating to 100 ml, adding absolute ethyl alcohol for precipitation until the alcohol content reaches 60v%, and filtering to remove the precipitate. Adding anhydrous ethanol into the filtrate to make the ethanol content of the filtrate reach 80v%, collecting the precipitate, and drying to obtain rhizoma Polygonati polysaccharide N1(60-80 v% ethanol precipitate).
Taking 100 g of steamed and sun-dried rhizoma polygonati, adding 6 times of water for decocting for 3 times, each time for 60 minutes, combining extracting solutions, concentrating to 100 ml, adding absolute ethyl alcohol for precipitation until the alcohol content reaches 40 v%, and filtering to remove the precipitate. Adding anhydrous ethanol into the filtrate to make the ethanol content of the filtrate reach 60v%, filtering, collecting precipitate, and drying to obtain rhizoma Polygonati polysaccharide N2(40-60 v% ethanol precipitate). Adding anhydrous ethanol into the filtrate to make the ethanol content of the filtrate reach 80v%, filtering, collecting precipitate, and drying to obtain rhizoma Polygonati polysaccharide N3 (60-80 v% ethanol precipitate).
< animal experiment 1>
The influence of the external application of the polygonatum polysaccharide component on the tissue blood flow is analyzed through mouse test research.
1. Test animals:
ICR was a clean-grade mouse, half of 50 males and females in total, and used to determine the effect of auricular blood flow.
2. Testing the polygonatum polysaccharide extract:
the polygonatum polysaccharide extract N1 prepared in the example 1 is diluted by adding 5 times, 10 times and 20 times of distilled water by weight to obtain high, medium and low dosages respectively.
3. Testing an instrument:
laser doppler blood flow meter, available from BIO corporation, usa.
4. The test method comprises the following steps:
measurement of mouse auricular blood flow:
4.1 the 50 mice were randomly divided into 4 groups, 14 mice per group (male and female halves) for the experimental group and 8 mice (male and female halves) for the control group.
4.2 mice were anesthetized with an intraperitoneal injection of 10wt% chloral hydrate at a dose of 350 mg/kg. The lying position is fixed, and the right auricle is fixed. And (4) measuring the blood flow of tissues at the far-end of the auricle on the right side by using a laser Doppler blood flow meter, and tracing a normal blood flow curve.
4.3 after the blood flow is stable, recording the average blood flow for 5min as a reference value. Then, 0.1ml of rhizoma Polygonati polysaccharide extract liquid medicine is added dropwise to the proximal end of the right auricle, and equivalent drinking water is added dropwise to the control group. Preserving the temperature of the liquid medicine/drinking water in a 37 ℃ water bath for more than 10min in advance, and keeping the constant temperature of the dripped liquid medicine/drinking water at 37 ℃.
4.4 continue to trace the blood flow curve for 25min, recording the blood flow values of 5, 10, 15 and 20 after the addition of the drug/drinking water (5 min average blood flow values are recorded per time point).
The rate of change of blood flow from baseline at 5, 10, 15 and 20 post-dose was calculated and the mean, standard deviation, was calculated for each group.
5. Statistical treatment
Statistical analysis of the data was performed using SSPS17.0 statistical software, and statistical results of the rate of change of the auricular blood flow of mice at different times are shown in the following table.
TABLE 2 change in blood flow in mouse auricles (%)
Group of 0-5min 5-10min 10-15min 15-20min
Control group -9.05±11.37 -17.59±12.55 -13.85±13.16 -14.74±15.29
High dose group -7.26±13.34* -4.72±15.83* -5.02±17.65* -5.27±18.65*
Middle dose group -5.46±12.32* -4.88±17.39* -4.07±19.45* -3.65±21.24*
Low dose group -6.85±11.26* -4.67±13.27* -4.76±20.67* -4.63±19.38*
Note: the data in the table are recorded in the form of mean ± standard deviation.
P <0.05 compared to control group
In 0-5min, the blood flow reduction rate of the auricle parts of the mice is lower by the polygonatum polysaccharide extract liquid medicine compared with that of a control group, which shows that the effect of the polygonatum polysaccharide-containing liquid medicine on inhibiting the blood flow of the auricle parts of the mice is lower than that of drinking water. And when the time is 5-20 min, the blood flow reduction and change of the auricle parts of the mice tend to be stable, the polygonatum polysaccharide extract effectively reduces the blood flow reduction caused by the dropping of drinking water on the auricle parts of the mice, the effect is very obvious, and the difference of the polygonatum polysaccharide extract and a control group has statistical significance (P is less than 0.05).
The reduction and improvement of the auricle blood flow of the mouse are obvious under the conditions of high, medium and low doses of the polygonatum polysaccharide extract, and the mouse has the characteristic of higher local blood flow compared with a control group. The mechanism is presumed to be: the polysaccharide molecules of rhizoma Polygonati are combined on the surface of local tissue to form an adhesion layer, and partially permeate into the skin to expand blood vessels. The water in auricle part is volatilized and cooled to cause the reduction of blood flow in the drinking water of the control group, and the polygonatum polysaccharide extract well offsets the influence of partial reduction of blood flow, so that the polygonatum polysaccharide extract can promote blood circulation, enhance the activity of local tissues and has the potential of relieving visual fatigue.
Based on the above test results, the method of preparing polygonatum polysaccharide extract N1 in example 1 was tried, and 10 times of distilled water was added to dilute the solution to obtain a medium-dose polygonatum polysaccharide solution. Adding 0.5%, 1% and 2% snail extract into the medium-dose rhizoma Polygonati polysaccharide medicinal liquid to prepare mixed active ingredient compound group 1, compound group 2 and compound group 3. And a1 wt% aqueous solution of snail extract was used as control 2.
The resulting compound groups 1 to 3 were tested by selecting ICR-series clean-grade mice of substantially equivalent body weight according to the test method 4 described above. The total number of mice was 40, half male and half female, and 10 mice per group. The test results were statistically analyzed using SPSS17.0 statistical software, and the statistics of the test results are shown in the table below.
TABLE 3 change in blood flow in mouse auricle under the action of Polygonatum polysaccharide extract (%)
Group of 0-5min 5-10min 10-15min 15-20min
Control group 2 -10.06±13.58 -18.32±13.65 -14.35±14.85 -15.65±17.82
Compound group 1 -4.34±11.24* -3.67±17.41* -3.13±16.95* -4.52±16.52*
Compound group 2 -5.36±10.59* -3.55±13.35* -3.82±20.28* -3.42±17.6*
Compound group 3 -6.28±12.55* -3.95±15.56* -4.28±17.52* -4.35±16.75*
Note: the data in the table are recorded in the form of mean ± standard deviation.
Experimental results show that the proportion of reduction of blood flow of auricles of mice is further reduced by compounding the medicinal liquids of the groups 1 to 3, the influence of the snail extracting solution on the blood flow of auricles of the mice is smaller, the snail extracting solution is different from specific vasoconstriction caused by volatilization of drinking water, the polygonatum polysaccharide extracting solution is attached to form a protective film layer under the cooperation effect of the snail extracting solution, and the blood flow of auricles of the mice is improved. The snail extract is added, so that the activity of the polygonatum polysaccharide can be fully exerted, and the effect is more obvious. In addition, the compound group 3 is added with 2 percent of snail extract, does not achieve better effect of more contents, but has no better effect than the other two compound groups 1-2 in 0-5 min.
The polygonatum polysaccharide extract and the snail extract are combined, so that the blood flow reduction phenomenon of the auricle of the mouse can be further improved, and the polygonatum polysaccharide extract and the snail extract are supposed to form a protective film to optimize the transdermal penetration effect of the polygonatum polysaccharide. In contrast, when the snail extract liquid with the concentration of 1% is singly used for preparing the liquid medicine, the blood flow of the auricle part of the mouse is reduced more, and the snail extract liquid alone does not have the effect of improving the blood flow.
< animal experiment 2>
The influence of the polygonatum polysaccharide component on free radicals is analyzed through mouse test research.
1. Test animals:
clean grade ICR mice, 60 total, male and female halves, were used to determine tail free radical changes.
2. Testing the polygonatum polysaccharide extract:
the polygonatum polysaccharide extract N1 prepared in example 1 is diluted with 10 times of distilled water to obtain a medium-dose polygonatum polysaccharide liquid medicine. Then, the snail extract liquid with the weight percentage of 0.25 percent, 0.5 percent and 1 percent is added to prepare a mixed active component compound group 1, a compound group 2 and a compound group 3. In addition, a 0.5% aqueous solution of snail extract was prepared as a negative control.
3. Testing an instrument:
laser doppler blood flow meter, available from BIO corporation, usa.
4. The test method comprises the following steps:
determination of mouse tail skin superoxide dismutase (SOD) Activity
4.1 the 60 mice were randomly divided into 6 groups, 10 mice per group (hermaphrodite).
4.2 the mouse is put into a cage, the mouse is limited to move, and the tail of the mouse is ensured to fall into a tray which is filled with the polygonatum polysaccharide liquid medicine, the compound group 1, the compound group 2, the compound group 3 and the negative control group (0.5 percent of snail extract solution aqueous solution) at the rear part of the cage. In the control group, the same amount of drinking water was introduced into the tray. After three days, the mice were sacrificed, and the tail skin was homogenized and stored in a refrigerator at 20 ℃.
4.3 determination of mouse tail skin SOD activity according to the superoxide dismutase (SOD) test kit instructions.
5. Statistical treatment
SPSS17.0 statistical software is adopted to carry out statistical analysis on data, and the influence of the externally applied polygonatum polysaccharide component on the free radical scavenging capacity is analyzed through mouse test of tail skin SOD activity and experimental research. The polygonatum polysaccharide extract can obviously increase the SOD activity of the tail skin of the mouse, and has statistical significance (P is less than 0.05) compared with the contrast group. The specific test results are shown in the following table.
TABLE 4 Effect of different drugs on SOD activity of mouse tail skin (mean. + -. standard deviation)
Group of SOD activity (U/mg protein)
Control group 9.75±5.71
A Chinese medicinal liquid containing rhizoma Polygonati polysaccharide 12.21±4.35
1% snail extract water solution 9.92±6.18
Compound group 1 13.66±9.58*
Compound group 2 15.45±6.63*
Compound group 3 14.98±7.32*
Note: p <0.05 compared to control group
The experimental result of the tail tissue of the mouse shows that the tail tissue soaked in the polygonatum polysaccharide extract liquid is cleared of free radicals, and the polygonatum polysaccharide can clear the free radicals in the tissue and improve the activity of SOD superoxide dismutase. The rhizoma polygonati polysaccharide extract is supposed to play a role in eliminating free radicals and relieving visual fatigue. Compared with the single application of the polygonatum polysaccharide liquid medicine, the compound liquid medicine containing the polygonatum polysaccharide extract has more outstanding protection effect and higher SOD activity, which shows that the snail extracting solution and the polygonatum polysaccharide extract can better play a role in removing. In addition, the results of the mouse experiments using the single aqueous solution of the 0.5% snail extract solution showed that the conventional snail extract solution itself did not have the effect of enhancing the SOD activity.
Free radicals can seriously harm the self-repairing ability of tissues, and the self anti-fatigue ability of the organisms can be activated by removing the free radicals. According to the animal experiments, the polygonatum polysaccharide extract can enhance the blood flow of subcutaneous tissues and eliminate free radicals, and has the potential of application in relieving visual fatigue.
< example 3>
Hydrogel containing polygonatum polysaccharide:
hydrogel raw materials are weighed according to the formula of the hydrogels A1, A2 and A3 prepared in the example 1, and then 5 wt%, 10wt% and 20wt% of the polygonatum polysaccharides N1, N2 and N3 prepared in the example 2 are respectively added to prepare the gel materials containing different polygonatum polysaccharides.
TABLE 5 hydrogel materials containing natural active ingredients
Numbering Hydrogel substrate Natural active ingredient extract
301 Hydrogel A1 0
302 Hydrogel A1 5% Polygonatum polysaccharide N1
303 Hydrogel A1 10% Polygonatum polysaccharide N1
304 Hydrogel A1 20% Polygonatum polysaccharide N1
305 Hydrogel A1 10% Polygonatum polysaccharide N2
306 Hydrogel A1 10% of polygonatum polysaccharide N1 and 0.5% of snail extract
307 Hydrogel A1 12% of polygonatum polysaccharide N1 and 0.3% of snail extract
308 Hydrogel A1 12% of polygonatum polysaccharide N1 and 0.4% of snail extract
309 Hydrogel A2 0
310 Hydrogel A2 5% of rhizoma polygonati polysaccharide N3 and 0.5% of snail extract
311 Hydrogel A2 10% of polygonatum polysaccharide N3 and 0.5% of snail extract
312 Hydrogel A2 0.5% snail extract
< adhesion Performance test >
The hydrogel material containing polygonatum obtained in the above example 3 is subjected to adhesion performance test according to the method a of slope rolling ball method in the initial adhesion performance test method of the pressure-sensitive adhesive tape of GB/T4852, and the test results are shown in the following table according to the method of measuring 180 ° peel strength of the pressure-sensitive adhesive tape of GB 2792.
TABLE 6 gel adhesion Properties
Numbering Initial adhesion Peel strength (N/mm)
301 8.6 0.36
302 8.6 0.35
303 8.5 0.34
304 7.9 0.31
305 8.7 0.37
306 8.6 0.35
307 8.4 0.33
308 8.0 0.31
309 8.5 0.36
310 8.4 0.35
311 8.3 0.33
312 7.8 0.32
The gel material of the eye patch has good adhesive property and higher peel strength, and meets the application requirement of the eye patch structure. When the corresponding eye patch is tested for human body adhesive performance, a subject shows that the gel and the skin have good adhesive performance, and the peeling strength is moderate, so that discomfort cannot be caused.
< example 4>
Eye patch containing rhizoma Polygonati polysaccharide
The gel material prepared in example 3 was coated on the surface of a medical air-permeable nonwoven fabric as a backing substrate layer at a coating density of 3g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 40-50 ℃ to obtain the eye patch product containing the polygonatum polysaccharide. The eye patches containing the polygonatum polysaccharides are obtained according to the different gel materials 301-312 in the embodiment 3, which are respectively corresponding to 401-412.
< fatigue Release test >
The eye patch products containing polygonatum rhizome prepared in the above examples and comparative examples are tested for asthenopia alleviation, and the testing method is to invite people who need to face a computer display to work for more than 3 hours in life and work. After the testee receives the corresponding eye patch product, the working time of the testee starting to face the display is recorded, when the time of continuously facing the computer display reaches 3 hours, the corresponding eye patch product is used, the eye patch is closed and attached, and the eye patch is removed after the eye patch product is used for 15 min.
The number of people participating in the eye patch visual fatigue relieving test is 78 in total, and the examinee mainly evaluates the adhesion performance, the peeling pain feeling and the visual fatigue relieving effect of the eye patch product. The eye patch product comprises the code 401-412 prepared in the above example 3, and the brand relieving eye patch of the commercially available eye patch product H is used as a positive reference.
Evaluation criteria for adhesion properties: 0 minute of stripping, more than half of stripping is 1-4 minutes; stripping a little and not more than half 5-8 minutes; the edge part is stripped for 8-9 minutes, and no stripping is carried out for 10 minutes.
Evaluation criteria for pain sensation in exfoliation: difficult to exfoliate and produce a strong pain score of 0; the stripping process generates 1-5 minutes of strong pain feeling; slight pain of 6-9 minutes and no pain of 10 minutes in the stripping process.
Evaluation standard of asthenopia relieving effect:
a) the visual fatigue is not obviously improved, the red blood streak is not obviously changed, the fine lines around the eyes are not changed or the application comfort is not good, 1-3 minutes.
b) Improving the visual fatigue part, reducing red blood streak, relieving fine lines around eyes and having poor application comfort level for 4 to 7 minutes.
c) The eye fatigue is obviously improved, the red blood streak is eliminated, the fine lines around the eyes are reduced or disappeared, and the application is comfortable for 8 to 10 minutes.
The test results were subjected to data analysis using EXCEL, and the final scoring evaluations were as shown in the following table.
Eye pad of table 7 asthenopia relieving performance test
Numbering Adhesion Properties Pain sensation of exfoliation Asthenopia relieving effect
401 9.59±0.83 9.6 6.2
402 9.27±0.81 9.5 7.9
403 9.34±1.59 9.7 8.4
404 8.54±1.31 9.6 8.3
405 9.87±0.91 9.6 7.4
406 9.51±1.46 9.4 8.7
407 9.38±0.73 9.4 9.1
408 8.43±0.94 8.9 8.8
409 9.52±1.18 9.3 6.5
410 9.24±1.11 9.2 8.8
411 9.06±1.62 9.4 8.7
412 8.42±1.23 9.5 6.2
H brand soothing eye protection patch 9.22±1.86 9.5 8.0
Test results show that the eye patch product containing rhizoma polygonati can well relieve asthenopia and reduce red blood streak, and has good effect on improving the skin state of eye tissues. The gel eye patch is added with the polygonatum polysaccharide, compared with a simple gel patch product, the gel eye patch can better play a role of relieving the visual fatigue, the polygonatum polysaccharide is controlled to be 5-20 wt%, and the effect of relieving the visual fatigue is enhanced by increasing the addition amount within a certain addition ratio range. But the effect is reduced after a certain proportion is exceeded, probably because the addition amount of the polygonatum polysaccharide is too high, the stability of the gel matrix is influenced, the bonding performance is not good, and the natural active ingredients are not bonded to act on eye skin.
Wherein, the selection of the water extraction and alcohol precipitation part of the polygonatum polysaccharide also influences the efficacy of the polygonatum polysaccharide hydrogel eye patch material for relieving the asthenopia, and if the polygonatum polysaccharide precipitated by 40-60 v% ethanol is applied to the hydrogel material corresponding to 305 as an additive component, the effect of relieving the asthenopia is obviously reduced compared with the polygonatum polysaccharide precipitated by 60-80 v% ethanol, and the optimal effect cannot be achieved. Preferably, the active ingredient obtained by water extraction and alcohol precipitation of polygonatum polysaccharide with concentration of 60-80 v% is used as the active ingredient for relieving the visual fatigue, and the effect is better.
The effect of relieving the asthenopia of the polygonatum polysaccharide can be further enhanced by adding the snail extracting solution into the polygonatum polysaccharide, and the effect of enhancing the asthenopia relieving is not achieved by adding the snail extracting solution into the hydrogel. The snail extract is shown to have the effect of promoting and enhancing the effect of the polygonatum polysaccharide extract in the hydrogel material, and the snail extract does not have the effect of relieving the asthenopia.
In general, the gel eye patch containing polygonatum polysaccharide can achieve the basically equivalent fitting performance of the existing commercially available soothing eye patch products and the effect of relieving visual fatigue, and provides an excellent novel industrial path for the development of polygonatum downstream industries.
< example 5>
Eye patch containing rhizoma Polygonati polysaccharide
Preparation of Polygonatum odoratum extract
Taking the polygonatum odoratum raw material, pulverizing into powder, adding 10 times of water for reflux extraction for 30min, repeatedly extracting for 3 times, combining the extracting solutions, and concentrating to 100 times of the weight of the raw material. Adding active carbon for adsorption and decolorization, filtering, and rotary evaporating the filtrate to dryness to obtain rhizoma Polygonati Odorati extract.
Preparation of eye mask
The hydrogel A2 prepared in example 1 was heated to 50 deg.C, and 8 wt% of rhizoma Polygonati polysaccharide extract, 1 wt% of rhizoma Polygonati Odorati extract, and 0.6 wt% of snail mucus extract (9.6 wt% in total, relative to the weight of hydrogel A2) were added, and stirred and mixed uniformly. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 2g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 42 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.
< example 6>
Eye patch containing rhizoma Polygonati polysaccharide
The hydrogel A3 prepared in example 1 was heated to 50 deg.C, and 11% of rhizoma Polygonati polysaccharide extract and 1% of snail extract (12 wt% in total) were added, and stirred and mixed well. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 1.5g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 45 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.
< example 7>
Eye patch containing rhizoma Polygonati polysaccharide
The hydrogel A3 prepared in example 1 was heated to 50 deg.C, and then added with 8% of rhizoma Polygonati polysaccharide extract, 0.5% of snail extract, and 1% of fructus Citri Sarcodactylis extract (9.5 wt% in total), and stirred and mixed well. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 1.8g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 50 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.
< example 8>
Eye patch containing rhizoma Polygonati polysaccharide
Taking hydrogel A3 prepared in example 1, heating to 50 deg.C, adding rhizoma Polygonati polysaccharide extract 12%, snail extractive solution 0.5%, and fructus Citri Sarcodactylis extract 1% (13.5 wt% in total), stirring, and mixing. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 1.8g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 50 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.
< example 9>
Eye patch containing rhizoma Polygonati polysaccharide
Taking hydrogel A2 prepared in example 1, addHeating to 50 deg.C, adding rhizoma Polygonati polysaccharide extract 8%, snail extractive solution 0.2%, and fructus Citri Sarcodactylis extract 0.8% (9 wt% in total), stirring, and mixing. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 2.0g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 50 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.
< example 10>
Eye patch containing rhizoma Polygonati polysaccharide
The hydrogel A2 prepared in example 1 was heated to 50 deg.C, and then 15% of rhizoma Polygonati polysaccharide extract and 0.5% of snail extract (15.5 wt% in total) were added, and the mixture was stirred and mixed well. The medical air-permeable non-woven fabric is used as a backing substrate layer, the hydrogel material containing the natural active ingredients is coated on the surface of the non-woven fabric, and the coating density is 2.1g/cm2And covering with an electrostatic protection film after coating, and transferring to an oven to be dried for 12h at 50 ℃ to obtain the eye patch containing the active ingredients such as polygonatum polysaccharide.

Claims (7)

1. An eye patch containing rhizoma Polygonati polysaccharide for relieving asthenopia, which comprises a backing substrate layer, a gel layer and a protective film,
the gel layer is hydrogel taking sodium hyaluronate as a main component;
the hydrogel comprises the following components in parts by weight: 10-20 parts of sodium hyaluronate, 2-4 parts of sodium polyacrylate, 3-5 parts of carbomer, 10-15 parts of glycerol and 40-80 parts of water;
the gel layer contains 3-20wt% of natural active ingredient extract;
the natural active component extract consists of a polygonatum polysaccharide extract and a snail mucus extracting solution; the ratio of rhizoma Polygonati polysaccharide is more than or equal to 60 wt%.
2. The eye patch for relieving asthenopia comprising polygonatum polysaccharide according to claim 1, wherein the gel layer contains 5-16wt% of natural active ingredient extract.
3. The eye patch containing polygonatum polysaccharide for relieving visual fatigue as claimed in claim 1, wherein the content of the polygonatum polysaccharide in the natural active ingredient extract is not less than 90wt%, and the snail mucus extract is 1-10 wt%.
4. The eye patch containing polygonatum polysaccharide for relieving visual fatigue according to claim 1, wherein the polygonatum polysaccharide extract is a polygonatum polysaccharide extract extracted from polygonatum which is steamed and sun-dried.
5. The eye patch containing polygonatum polysaccharides for relieving visual fatigue according to claim 4, wherein the polygonatum that is steamed and aired once is obtained by steaming and airing once.
6. The eye patch containing polygonatum polysaccharides for relieving visual fatigue according to claim 4, wherein the extraction method of the polygonatum polysaccharides is as follows:
s101, taking the rhizoma polygonati which is steamed and sun-dried once, adding 10 times of water for decocting for 2 times, each time for 30 minutes, combining extracting solutions, and concentrating the filtrate to 0.7-2 times of the weight of the rhizoma polygonati which is steamed and sun-dried once;
s102, adding ethanol to enable the content of the ethanol in the filtrate obtained after concentration in the step S101 to reach 60v%, and filtering to remove precipitates; and continuously adding ethanol into the filtrate to ensure that the content of the ethanol in the filtrate reaches 80v%, and collecting the precipitate to obtain the polygonatum polysaccharide extract.
7. The eye patch containing polygonatum polysaccharides for relieving visual fatigue according to claim 1, wherein the hydrogel comprises the following components in parts by weight: 12-18 parts of sodium hyaluronate, 2-3 parts of sodium polyacrylate, 3-4 parts of carbomer, 10-13 parts of glycerol and 50-60 parts of water.
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