CN112220784A - Grape seed hydrolyzed proanthocyanidin eye-protecting liquid for external application and preparation process thereof - Google Patents

Grape seed hydrolyzed proanthocyanidin eye-protecting liquid for external application and preparation process thereof Download PDF

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CN112220784A
CN112220784A CN202011201382.6A CN202011201382A CN112220784A CN 112220784 A CN112220784 A CN 112220784A CN 202011201382 A CN202011201382 A CN 202011201382A CN 112220784 A CN112220784 A CN 112220784A
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grape seed
eye
procyanidin
glycerol
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CN112220784B (en
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殷军
翟健秀
李嗣凯
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Changchun Nadian Biotechnology Co ltd
Shenyang Pharmaceutical University
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Shenyang Pharmaceutical University
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Abstract

The invention relates to an eye-protecting liquid for external application, which is prepared from grape seed and procyanidine through hydrolysis, and a preparation process and application thereof, and belongs to the technical field of medicines. The grape seed hydrolyzed procyanidin eye-protecting liquid for external application comprises grape seed hydrolyzed procyanidin, borneol, menthol, carboxymethyl thickening agent, glycerol and water, wherein the weight of each component is as follows: 100-300 parts of grape seed hydrolyzed proanthocyanidins, 1-30 parts of borneol, 1-30 parts of menthol, 2-50 parts of thickening agent, 300-1500 parts of glycerol and 0-50 parts of preservative. The thickening agent is sodium carboxymethyl starch or sodium carboxymethyl cellulose. The grape seed hydrolyzed procyanidin contained in the grape seed hydrolyzed procyanidin eye-protecting liquid has pharmacological effects of removing free radicals, resisting oxidation and improving blood microcirculation; the borneol and the menthol can enhance the cool feeling of the product and relieve the eye fatigue; the grape seed hydrolyzed procyanidin, sodium carboxymethyl starch and glycerol can moisten skin and have moisturizing effect. By applying the eye protection liquid externally, the beneficial effects of nursing skin around eyes and relieving visual fatigue can be achieved.

Description

Grape seed hydrolyzed proanthocyanidin eye-protecting liquid for external application and preparation process thereof
Technical Field
The invention relates to an eye-protecting liquid for external application, which is prepared from grape seed and procyanidine through hydrolysis, and a preparation process and application thereof, and belongs to the technical field of medicines.
Background
With the development of science and technology, the time for people to watch screens of electronic products such as televisions, computers or mobile phones is gradually increased, and the flickering screens can cause asthenopia, so that the people can generate symptoms such as dry eyes, sour and swollen eyes, blurred vision and even vision deterioration, and the quality of life is seriously affected. Hydrolyzed procyanidins are a polyphenolic compound that is widely found in the plant kingdom, named because they produce anthocyanins under hot acid conditions. Grape seed procyanidin is a hydrolyzed procyanidin mixture extracted from grape seeds, is one of the most efficient plant-derived antioxidants discovered so far, has strong antioxidant activity, and is a good free radical scavenger and lipid peroxidation inhibitor. Related researches in recent years prove that the grape seed hydrolyzed procyanidin has strong capacity of eliminating free radicals, can remarkably improve lipid peroxidation and DNA damage induced by the free radicals, and has the effect greatly stronger than common antioxidants such as vitamin E, vitamin C and the like. In addition, the hydrolyzed procyanidin has good protective effect on skin, can be used for shrinking pores and tightening skin, and can also effectively reduce excessive secretion of sebum in oily skin. Meanwhile, as a natural moisturizing substance, the hydrolyzed procyanidin has a good moisturizing effect, can form a compound moisturizing factor with protein, polypeptide, polysaccharide and the like, and can also inhibit the activity of hyaluronidase to achieve the moisturizing effect. In addition, the hydrolyzed procyanidin can improve microcirculation, enhance nutrition supply of retina, and has effects of improving vision, resisting lens injury, and relieving asthenopia.
At present, the number of products for external application aiming at asthenopia is small, the selection of consumers is limited, and most of the products have undefined active ingredients or poor experience of the product body feeling. The grape seed hydrolyzed proanthocyanidin eye protection liquid for external application for relieving visual fatigue and nursing skin around eyes is clear in effective components, cool and comfortable in body feeling, can fill the market vacancy, and solves the problems of few product types and poor effect.
Disclosure of Invention
The invention solves the technical problem of providing the grape seed hydrolyzed procyanidin eye protection liquid for external application and a preparation process thereof, which can relieve visual fatigue and care skin around eyes.
Further, in order to achieve the above object, the present invention provides the following eye-protecting solution for external application containing grape seed hydrolyzed procyanidin, borneol, menthol, carboxymethyl thickening agent, glycerol and water, wherein the weight components of the components are as follows: 100-300 parts of grape seed hydrolyzed proanthocyanidins, 1-30 parts of borneol, 1-30 parts of menthol, 2-50 parts of thickening agent, 300-1500 parts of glycerol and 0-50 parts of preservative.
The thickening agent is sodium carboxymethyl starch or sodium carboxymethyl cellulose.
Further, the invention preferably selects the following grape seed hydrolyzed procyanidin eye-protecting liquid for external application:
100-300 parts of grape seed hydrolyzed proanthocyanidins, 1-30 parts of borneol, 1-30 parts of menthol, 2-50 parts of thickening agent, 300-1500 parts of glycerol and 2-50 parts of preservative.
Furthermore, the invention preferably uses the following grape seed hydrolyzed procyanidin eye-protecting liquid for external application:
100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 2-30 parts of sodium carboxymethyl starch and 300-600 parts of glycerol.
Or
100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 10-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-50 parts of potassium sorbate.
Furthermore, the invention preferably uses the following grape seed hydrolyzed procyanidin eye-protecting liquid for external application:
100-250 parts of grape seed hydrolyzed procyanidin, 5-30 parts of borneol, 5-30 parts of menthol, 2-30 parts of sodium carboxymethyl starch and 300-600 parts of glycerol.
Or
200-300 parts of grape seed hydrolyzed procyanidin, 10-25 parts of borneol, 10-25 parts of menthol, 20-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-50 parts of potassium sorbate.
The invention also provides a preparation process of the grape seed hydrolyzed procyanidine eye-protecting liquid, which comprises the following specific steps:
(1) weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the thickening agent and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the thickening agent and the glycerol into a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed into a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of borneol) and 2 (stock solution of menthol) with the weight percentage of 10-20% by respectively using 75-85% ethanol water solution; preparing 10-20 wt% of stock solution 3 from grape seed hydrolyzed procyanidin by pure water, and placing the stock solution in a light-tight container; preparing a stock solution 4 with the thickener accounting for 0.2-0.4% by weight by using pure water;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with glycerol and potassium sorbate, and the mixture was stirred for 5-20min at 300-. Mixing the two mixed solutions, adding a proper amount of pure water, and continuously stirring for 15-30min at a rotation speed of 300-. A light-shielded container was used during the stirring.
(4) And (3) degerming: and (5) bottling the obtained solution after radiation sterilization or filter membrane sterilization, wherein each bottle contains 5-50 ml of the procyanidine eye-protecting solution for external application.
The grape seed hydrolyzed procyanidine contained in the invention has the pharmacological effects of scavenging free radicals, resisting oxidation and improving blood microcirculation; the borneol and the menthol can enhance the cool feeling of the product and relieve the eye fatigue; the grape seed hydrolyzed procyanidin, sodium carboxymethyl starch (or sodium carboxymethyl cellulose) and glycerol can moisten skin and have moisturizing effect. In conclusion, the eye protection liquid disclosed by the invention is externally applied to the skin around the eyes, so that the beneficial effects of nursing the skin around the eyes and relieving the visual fatigue can be achieved.
The procyanidine eye protection liquid for external application has the effects of refreshing, moistening and resisting oxidation, wherein the effective components are clear, the vacancy of products for relieving visual fatigue for external application in the market at present can be filled, and the problems of unclear main components and poor use experience of the existing products can be solved. Meanwhile, the invention discovers the material proportion with the advantage of the anti-asthenopia effect by establishing an asthenopia rat animal model and comparing the influence of formulas with different proportions on the oxidative stress level of the eyeball of the rat.
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FIG. 1: formula (I) grape seed hydrolyzed procyanidin eye-protecting solution has influence on MDA content level in eyeballs of asthenopia rats.
A: experimental results of example 1; b: experimental results of example 2; c: experimental results of example 3; d: the effect of high dose administration of the eye compress solution in example 2, example 3, example 4 and example 5 on reducing the MDA content in the eyeball of rats was compared. P <0.05 compared to blank; p <0.001 compared to blank group; p <0.05 compared to model group; # p <0.01 compared to model group; # p <0.001 compared to model group.
FIG. 2: the formula (I) is the effect of grape seed hydrolyzed procyanidin eye-protecting liquid on SOD activity level in eyeballs of asthenopia rats.
A: experimental results of example 1; b: experimental results of example 2; c: experimental results of example 3; d: comparison of the effect of high-dose administration of the eye compress solutions in examples 2, 3, 4 and 5 on enhancing the SOD activity of rat eyeball. P <0.05 compared to blank; p <0.001 compared to blank group; p <0.05 compared to model group; # p <0.01 compared to model group; # p <0.001 compared to model group.
FIG. 3: and (II) the grape seed hydrolyzed procyanidine eye-protecting liquid has the influence on the MDA content level in eyeballs of asthenopia rats.
A: experimental results of example 6; b: experimental results for example 7; c: experimental results for example 8; d: the effect of high dose administration of the eye compress solution in examples 8, 9 and 10 on reducing the MDA content in the eyeball of rats was compared. P <0.05 compared to blank; p <0.001 compared to blank group; p <0.05 compared to model group; # p <0.01 compared to model group; # p <0.001 compared to model group.
FIG. 4: : and (II) the effect of the grape seed hydrolyzed procyanidin eye-protecting liquid on the SOD activity level in eyeballs of asthenopia rats.
A: experimental results of example 6; b: experimental results for example 7; c: experimental results for example 8; d: comparison of the effect of high dosage administration of eye compress solution in example 8, example 9 and example 10 on enhancing SOD activity of rat eyeball. P <0.05 compared to blank; p <0.001 compared to blank group; p <0.05 compared to model group; # p <0.01 compared to model group; # p <0.001 compared to model group.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood in the art to which this invention belongs. In order to make the technical problems solved by the present invention clear, the present invention is further described below with reference to specific examples.
The invention relates to two kinds of externally applied grape seed hydrolyzed proanthocyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes and a preparation process thereof, wherein the externally applied grape seed hydrolyzed proanthocyanidin eye protection liquid comprises the following components: 100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 2-30 parts of sodium carboxymethyl starch and 300-600 parts of glycerol; 100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 10-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-50 parts of potassium sorbate.
Example 1
1.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 100 parts of grape seed hydrolyzed procyanidin, 1 part of borneol, 1 part of menthol, 2 parts of sodium carboxymethyl starch and 300 parts of glycerol.
(1) Weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol in a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed in a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10% from Borneolum Syntheticum and Mentholum with 75% ethanol water solution; preparing 20 wt% stock solution 3 from grape seed hydrolyzed procyanidin with pure water, and placing in a light-tight container; preparing stock solution 4 with the weight percentage of 0.4% by using pure water as sodium carboxymethyl starch;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with the corresponding parts by weight of glycerol, and the mixture was stirred for 15min in a constant speed stirrer at 300 rpm. Mixing the two mixed solutions, adding appropriate amount of pure water, and stirring with a constant speed stirrer at 300 rpm for 15 min. A light-shielded container was used during the stirring.
(4) And (3) degerming: sterilizing the obtained solution with filter membrane, and bottling 10ml per bottle to obtain topical procyanidin eye protecting liquid.
1.2 the product effect is as follows:
the product is reddish brown semitransparent, has high transparency, can feel cool feeling around eyes after being pasted for 2-3 minutes, has the duration of more than 10 minutes, has good moisturizing performance and moistening feeling, has a relatively mild and cool effect on the whole, and is suitable for people with sensitive skin or used for daily skin maintenance around eyes.
1.3 anti-asthenopia effect on rats:
in this example, rats were used as experimental animals, each group had 6 animals, and the animals were divided into a blank control group, a model control group, a positive drug group, a procyanidin eye-protecting solution low dose group, and a procyanidin eye-protecting solution high dose group, and subjected to a dosing experiment (free diet) for a period of 7 days. The positive medicine is Zhenshiming eye-protecting paste (general type, Jiangxi Zhenshiming pharmaceutical Co., Ltd.). Except for the blank control group, other groups use a strobe lamp for molding, and the specific molding method comprises the following steps: day and night light cycles (12 h each) were used with a day light intensity of 30lux and a night light intensity of 0 lux. After the end of daily light exposure, rats were placed in a closed environment with ether immersion for anesthesia and the eyes were applied for 15min during the time that anesthesia was effective. Cutting the eyesight-protecting plaster or non-woven fabric into 1cm x 1cm square, applying 1ml physiological saline soaked non-woven fabric to the model control group, applying the eyesight-protecting plaster to the positive medicine group, and applying 0.5ml and 1ml grape seed hydrolyzed proanthocyanidin eye-protecting liquid soaked non-woven fabric to the proanthocyanidin eye-protecting liquid low-dose and high-dose groups respectively. The blank control group was anesthetized only and no other treatments were performed. After the application at 7d was finished, the rats were sacrificed and the eyeballs were removed, quickly placed in an ice bath environment and treated with saline at volume: the weight ratio is 9: 1, centrifuging the homogenate at 5000rpm, and measuring the contents of SOD and MDA in supernatant of each group of eyeball homogenate by using a kit.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the procyanidine eye-protecting liquid high-dose group has the advantages that the SOD activity is increased, the MDA content is reduced, but the two data have no significant difference (shown in figures 1 and 2 and A) compared with the model control group, and are slightly weaker than the positive medicine group.
The experimental result shows that the prescription mildly reduces the oxidative stress level of eyes and has certain anti-asthenopia effect.
Example 2
2.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 250 parts of grape seed hydrolyzed procyanidin, 5 parts of borneol, 10 parts of menthol, 15 parts of sodium carboxymethyl starch and 400 parts of glycerol.
(1) Weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol in a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed in a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10% from Borneolum Syntheticum and Mentholum with 75% ethanol water solution; preparing 20 wt% stock solution 3 from grape seed hydrolyzed procyanidin with pure water, and placing in a light-tight container; preparing stock solution 4 with the weight percentage of 0.4% by using pure water as sodium carboxymethyl starch;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with the corresponding parts by weight of glycerol, and the mixture was stirred in a constant speed stirrer at 400 rpm for 20 min. Mixing the two mixed solutions, adding appropriate amount of pure water, and stirring with a constant speed stirrer at a rotation speed of 400 rpm for 20 min. A light-shielded container was used during the stirring.
(4) And (3) degerming: sterilizing the obtained solution with filter membrane, and bottling 30ml per bottle to obtain topical procyanidin eye protecting liquid.
2.2 the product effect is as follows:
the product is clear, dark reddish brown, can feel cool feeling around eyes after being applied for 1-2 minutes, has the duration of more than 20 minutes, the strength of more than example 1 and the moistening feeling and the viscosity of more than example 1, has more obvious effect on relieving the visual fatigue, and is suitable for people with higher visual fatigue degree and stronger skin adaptability.
2.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 1.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with a model control group, the procyanidine eye protection liquid high-dose group has the advantages that the SOD activity is increased by 32.5%, the MDA content is reduced by 41%, the two data are both significantly different (p is less than 0.001) (shown in figures 1 and B, and shown in figures 2 and B) compared with the model control group, and the antioxidant stress effect is better than that of a positive control. The procyanidine eye protection solution low-dose group can increase SOD activity and reduce MDA content to a certain extent, but the data has no significant difference with the model control group.
The experimental result shows that the prescription can obviously reduce the oxidative stress level of eyes and has a more obvious anti-asthenopia effect.
Example 3
3.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 250 parts of grape seed hydrolyzed procyanidin, 10 parts of borneol, 5 parts of menthol, 15 parts of sodium carboxymethyl starch and 400 parts of glycerol.
(1) Weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol in a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed in a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10% from Borneolum Syntheticum and Mentholum with 75% ethanol water solution; preparing 20 wt% stock solution 3 from grape seed hydrolyzed procyanidin with pure water, and placing in a light-tight container; preparing stock solution 4 with the weight percentage of 0.4% by using pure water as sodium carboxymethyl starch;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with the corresponding parts by weight of glycerol, and the mixture was stirred in a constant speed stirrer at 400 rpm for 20 min. Mixing the two mixed solutions, adding appropriate amount of pure water, and stirring with a constant speed stirrer at a rotation speed of 400 rpm for 20 min. A light-shielded container was used during the stirring.
(4) And (3) degerming: sterilizing the obtained solution with filter membrane, and bottling 30ml per bottle to obtain topical procyanidin eye protecting liquid.
3.2 the product effect is as follows:
the product is clear, dark reddish brown, can feel cool feeling around eyes after being applied for 1-2 minutes, has the duration of more than 20 minutes and the strength of more than examples 1 and 2, has the moistening feeling and the viscosity of more than examples 1 and similar to example 2, and has the effect of relieving the asthenopia similar to example 2.
3.3 anti-asthenopia Effect on rats
The experimental procedure was as in example 1.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the proanthocyanidin eye-protecting liquid high-dose group has the advantages that the SOD activity is obviously improved, the MDA content is obviously reduced (figures 1 and C; figures 2 and C), and the antioxidant stress effect is similar to that of the example 2.
The experimental result shows that the prescription can slightly reduce the oxidative stress level of eyes, and the anti-asthenopia effect is weaker than that of the examples 1 and 2.
Example 4
4.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 250 parts of grape seed hydrolyzed procyanidin, 20 parts of borneol, 20 parts of menthol, 15 parts of sodium carboxymethyl starch and 400 parts of glycerol. The procedure was as in example 2.
4.2 the product effect is as follows:
the product is clear, dark reddish brown, and has refreshing feeling in 1 min, duration longer than 25 min, intensity greater than examples 1 and 2, and moistening and viscosity greater than example 1 and similar to example 2.
4.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 1. The experimental results show that compared with a model group, the proanthocyanidin eye-protecting liquid high-dose group has an ascending trend of SOD activity and a descending trend of MDA content, but both data have no significant difference compared with a model control group (figures 1 and D; figures 2 and D), and the antioxidant stress effect of the proanthocyanidin eye-protecting liquid high-dose group is significantly weaker than that of the control group and the example 2 (figures 1 and D; figures 2 and D).
Example 5
5.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 250 parts of grape seed hydrolyzed procyanidin, 30 parts of borneol, 30 parts of menthol, 15 parts of sodium carboxymethyl starch and 400 parts of glycerol. The procedure was the same as in examples 2 and 4.
5.2 the product effect is as follows:
the product is clear, dark reddish brown, and has strong refreshing feeling around eyes within 1 min, lasting for more than 25 min, intensity greater than examples 2 and 4, moistening feeling, and viscosity greater than example 1 and similar to example 2.
5.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 1. The experimental results show that compared with a model group, the proanthocyanidin eye-protecting liquid high-dose group has an ascending trend of SOD activity and a descending trend of MDA content, but both data have no significant difference compared with a model control group (figures 1 and D; figures 2 and D), and the antioxidant stress effect of the proanthocyanidin eye-protecting liquid high-dose group is significantly weaker than that of the control group, the example 2 and the example 4.
Example 6
6.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 100 parts of grape seed hydrolyzed procyanidin, 1 part of borneol, 1 part of menthol, 10 parts of sodium carboxymethylcellulose, 750 parts of glycerol and 5 parts of potassium sorbate.
(1) Weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethylcellulose and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethylcellulose and the glycerol in a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed in a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10% from Borneolum Syntheticum and Mentholum with 75% ethanol water solution; preparing 20 wt% stock solution 3 from grape seed hydrolyzed procyanidin with pure water, and placing in a light-tight container; preparing 0.4 percent stock solution 4 by weight percent of sodium carboxymethylcellulose with pure water;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with the corresponding parts by weight of glycerol and potassium sorbate, and the mixture was stirred for 15min in a constant speed stirrer at 300 rpm. Mixing the two mixed solutions, adding appropriate amount of pure water, and stirring with a constant speed stirrer at 300 rpm for 15 min. A light-shielded container was used during the stirring.
(4) And (3) degerming: sterilizing the obtained solution with filter membrane, and bottling 10ml per bottle to obtain topical procyanidin eye protecting liquid.
6.2 product Effect
The product is reddish brown semitransparent, has high transparency, can feel cool feeling around eyes after being pasted for 2-3 minutes, has the duration of more than 10 minutes, has good moisturizing performance and moistening feeling, has a relatively mild and cool effect on the whole, and is suitable for people with sensitive skin or used for daily skin maintenance around eyes.
6.3 anti-asthenopia Effect on rats
The experimental procedure was as in example 1.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 40%, and the SOD activity is obviously reduced. Compared with the model control group, the procyanidine eye-protecting liquid high-dose group has SOD activity similar to and slightly lower than that of the model control group, and MDA content is reduced, and the two data have no significant difference (shown in figures 3 and 4 and A) compared with the model control group, and the effect is obviously weakened compared with a positive medicine group.
The experimental result shows that the prescription mildly reduces the oxidative stress level of eyes and has certain anti-asthenopia effect.
Example 7
7.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 200 parts of grape seed hydrolyzed procyanidin, 10 parts of borneol, 10 parts of menthol, 50 parts of sodium carboxymethylcellulose and 1500 parts of glycerol.
(1) Weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the sodium carboxymethyl starch and the glycerol in a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed in a lightproof vessel.
(2) Dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10% from Borneolum Syntheticum and Mentholum with 75% ethanol water solution; preparing 20 wt% stock solution 3 from grape seed hydrolyzed procyanidin with pure water, and placing in a light-tight container; preparing 0.4 percent stock solution 4 by weight percent of sodium carboxymethylcellulose with pure water;
(3) mixing: stock solutions 1, 2 and 4 were mixed, stock solution 3 was mixed with the corresponding parts by weight of glycerol and potassium sorbate, and the mixture was stirred in a constant speed stirrer at 400 rpm for 20 min. Mixing the two mixed solutions, adding appropriate amount of pure water, and stirring with a constant speed stirrer at a rotation speed of 400 rpm for 20 min. A light-shielded container was used during the stirring.
(4) And (3) degerming: sterilizing the obtained solution with filter membrane, and bottling 30ml per bottle to obtain topical procyanidin eye protecting liquid.
7.2 the product effect is as follows:
the product is clear, dark reddish brown, has a color deeper than that of example 6, can feel cool feeling around eyes after being applied for 2-3 minutes, has a duration longer than 20 minutes and a degree higher than that of example 6, has a moistening feeling and viscosity greater than that of example 6, has a more obvious effect on relieving visual fatigue, and is suitable for people with high visual fatigue degree and strong skin adaptability.
7.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 1.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the procyanidine eye-protecting liquid high-dose group has the advantages that the SOD activity is increased by 38%, the MDA content is reduced by 23%, the two data are both remarkably different from the model control group (shown in figures 3 and B, and shown in figures 4 and B), and the antioxidant stress effect is better than that of a positive control.
The experimental result shows that the prescription with high dose can obviously reduce the oxidative stress level of eyes and has more obvious anti-asthenopia effect.
Example 8
8.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 300 parts of grape seed hydrolyzed procyanidin, 10 parts of borneol, 10 parts of menthol, 50 parts of sodium carboxymethylcellulose and 1500 parts of glycerol. The procedure was as in example 7.
8.2 the product effect is as follows:
the product is clear, dark reddish brown, has a color deeper than that of the product obtained in examples 6 and 7, can feel cool feeling around eyes after being applied for 2-3 minutes, lasts for more than 20 minutes, is higher than that of the product obtained in example 6 in degree, has similar moistening feeling and viscosity as those of the product obtained in example 7, has a more obvious effect on relieving visual fatigue, and is suitable for people with higher visual fatigue degree and stronger skin adaptability.
8.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 1.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the procyanidine eye-protecting liquid high-dose group has SOD activity increased by 108% and MDA content decreased by 53%, and the two data have significant difference compared with the model control group (figure 3, C; figure 4, C), and the antioxidant stress effect is better than that of the positive control.
The experimental result shows that the prescription with high dose can obviously reduce the oxidative stress level of eyes and has more obvious anti-asthenopia effect.
Example 9
9.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 300 parts of grape seed hydrolyzed procyanidin, 25 parts of borneol, 25 parts of menthol, 50 parts of sodium carboxymethylcellulose and 1500 parts of glycerol. The procedure was as in example 7.
9.2 the product effect is as follows:
the product is clear, dark reddish brown, has a color similar to that of example 8, can feel a strong cooling feeling around eyes after being applied for 2-3 minutes, lasts for more than 25 minutes, is higher than that of example 8 in degree, is similar to that of examples 7 and 8 in moistening feeling and viscosity, has a more obvious effect on relieving visual fatigue, and is suitable for people with high visual fatigue degree and strong skin adaptability.
9.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 7.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the proanthocyanidin eye-protecting liquid high-dose group has the SOD activity increased by 39 percent and the MDA content decreased by 46 percent, and the two data have significant difference compared with the model control group (figures 3 and D; figures 4 and D), the antioxidant stress effect of the proanthocyanidin eye-protecting liquid high-dose group is better than that of the positive control group, and the comparison is similar to that of the example 8.
The experimental result shows that the prescription with high dose can obviously reduce the oxidative stress level of eyes and has more obvious anti-asthenopia effect.
Example 10
10.1 sample preparation:
an externally applied grape seed hydrolyzed procyanidin eye protection liquid for relieving visual fatigue and nursing skin around eyes comprises the following components in parts by weight: 300 parts of grape seed hydrolyzed procyanidin, 10 parts of borneol, 10 parts of menthol, 20 parts of sodium carboxymethylcellulose and 700 parts of glycerol. The procedure was as in example 7.
10.2 the product effect is as follows:
the product is a clear dark reddish brown color similar to example 8, and has a cooling sensation around the eyes after being applied for 2-3 minutes, a duration of more than 20 minutes, and a degree similar to example 8, with a slightly less moist and sticky feel than example 8.
10.3 anti-asthenopia effect on rats:
the experimental procedure was as in example 7.
The experimental result shows that compared with the blank control group, the MDA level of the model control group is increased by about 50%, and the SOD activity is obviously reduced. Compared with the model control group, the proanthocyanidin eye-protecting liquid high-dose group has the SOD activity increased by 43 percent and the MDA content decreased by 42 percent, and the two data have significant difference compared with the model control group (figures 3 and D; figures 4 and D), the antioxidant stress effect of the proanthocyanidin eye-protecting liquid high-dose group is better than that of the positive control group, and the two data are similar to the examples 8 and 9.
Comparison of Effect of examples 1 to 10
Figure BDA0002755429530000111
As shown in the table, the results of comparing the examples with the effect of reducing the level of oxidative stress in the eyeballs of rats in the asthenopia model revealed that examples 2 and 3 in the formula (one) and examples 8, 9 and 10 in the formula (two) were superior.
Therefore, the more preferable formula of the invention is as follows: 100-250 parts of grape seed hydrolyzed procyanidin, 5-10 parts of borneol, 5-10 parts of menthol, 10-20 parts of sodium carboxymethyl starch and 300-500 parts of glycerol.
Or 200-300 parts of grape seed hydrolyzed procyanidin, 10-25 parts of borneol, 10-25 parts of menthol, 20-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-5 parts of potassium sorbate.

Claims (8)

1. An external application type grape seed hydrolyzed procyanidin eye protection liquid is characterized by comprising grape seed hydrolyzed procyanidin, borneol, menthol, carboxymethyl thickening agent, glycerol and water, wherein the weight of each component is as follows: 100-300 parts of grape seed hydrolyzed proanthocyanidins, 1-30 parts of borneol, 1-30 parts of menthol, 2-50 parts of thickening agent, 300-1500 parts of glycerol and 0-50 parts of preservative.
2. The externally-applied eye-protecting solution containing grape seed hydrolyzed procyanidin as claimed in claim 1, wherein the weight composition of each component is as follows:
100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 2-30 parts of sodium carboxymethyl starch and 300-600 parts of glycerol;
or 100-300 parts of grape seed hydrolyzed procyanidin, 1-30 parts of borneol, 1-30 parts of menthol, 10-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-50 parts of potassium sorbate.
3. The topical eye drop of claim 1, wherein the eye drop comprises grape seed hydrolyzed procyanidin,
100-250 parts of grape seed hydrolyzed procyanidin, 5-30 parts of borneol, 5-30 parts of menthol, 2-30 parts of sodium carboxymethyl starch and 300-600 parts of glycerol;
or
200-300 parts of grape seed hydrolyzed procyanidin, 10-25 parts of borneol, 10-25 parts of menthol, 20-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-50 parts of potassium sorbate.
4. The topical eye drop of claim 1, wherein the eye drop comprises grape seed hydrolyzed procyanidin,
100-250 parts of grape seed hydrolyzed procyanidin, 5-10 parts of borneol, 5-10 parts of menthol, 10-20 parts of sodium carboxymethyl starch and 300-500 parts of glycerol.
Or 200-300 parts of grape seed hydrolyzed procyanidin, 10-25 parts of borneol, 10-25 parts of menthol, 20-50 parts of sodium carboxymethylcellulose, 700-1500 parts of glycerol and 0-5 parts of potassium sorbate.
5. The method of preparing the externally applied eye-protecting solution containing hydrolyzed procyanidin from grape seeds of claim 1, wherein the method comprises the following steps:
(1) weighing: weighing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the thickening agent and the glycerol according to the weight part ratio, and respectively placing the grape seed hydrolyzed procyanidin, the borneol, the menthol, the thickening agent and the glycerol into a clean vessel, wherein the grape seed hydrolyzed procyanidin is placed into a lightproof vessel;
(2) dissolving and preparing stock solution: preparing stock solutions 1 (stock solution of Borneolum Syntheticum) and 2 (stock solution of Mentholum) with weight percentage of 10-20% from 75-85% ethanol water solution; preparing 10-20 wt% of stock solution 3 from grape seed hydrolyzed procyanidin by pure water, and placing the stock solution in a light-tight container; preparing a thickener into stock solution 4 with the weight percentage of 0.2-0.4% by using pure water;
(3) mixing: mixing the stock solutions 1, 2 and 4, mixing the stock solution 3 with glycerol in corresponding parts by weight, and stirring for 5-20min at a rotation speed of 300-; mixing the two mixed solutions, adding a proper amount of water, and continuously stirring for 15-30min at a constant speed stirrer at a rotating speed of 300-;
(4) and (3) degerming: sterilizing the obtained solution by irradiation or with filter membrane, and bottling.
6. The use of the topical eye drop of grape seed hydrolyzed procyanidin of any one of claims 1 to 4 in the preparation of a medicament or health product for improving dry eye, eye dryness, eye soreness, blurred vision, and visual deterioration caused by asthenopia.
7. The use of the topical grape seed hydrolyzed procyanidin eye protection solution of any one of claims 1 to 4 in the preparation of a medicament or health care product for moisturizing and repairing skin around the eyes, and improving skin darkness around the eyes, fine wrinkles around the eyes, dark circles around the eyes, and bags around the eyes caused by ultraviolet irradiation, long-term computer radiation, and bad living habits.
8. The use of claim 6 or 7, wherein the eye drop is prepared by applying the grape seed hydrolyzed procyanidin eye drop to the skin around the eyes.
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