WO2021133284A1

WO2021133284A1 - A composition of hyaluronic acid and hydrolyzed collagen with vitamins and its production method

Info

Publication number: WO2021133284A1
Application number: PCT/TR2020/050083
Authority: WO
Inventors: Ahmet Meli̇koğlu; Yusuf GÜNDOĞDU
Original assignee: Melikoglu Ahmet
Priority date: 2019-12-25
Filing date: 2020-02-07
Publication date: 2021-07-01

Abstract

The invention is a liquid food supplement composition that strengthens the connective tissue and holds the joints, tendons and organs together and enables body integrity, as well as providing the skin with volume, flexibility and firmness and it is characterized by the fact that it comprises Type I and Type III hydrolyzed collagen peptides homogenized in deionized water, hyaluronic acid, Vitamin E, and trisodium citrate (pH regulator). In addition, the invented composition contains antimicrobial agent, anti-degrading components, emulsifier, antioxidant, vegetable oil, sweetening agent and various excipients selected from a group consisting of perfuming components.

Description

A COMPOSITION OF HYALURONIC ACID AND HYDROLYZED COLLAGEN WITH VITAMINS AND ITS PRODUCTION METHOD

Technical Field

The invention concerns with a composition of hyaluronic acid and hydrolyzed collagen in liquid form enriched with vitamin complexes for use as a food supplement, and with its method of production thereof.

The invention specifically concerns with a food supplement composition which strengthens the connective tissue with the help of hydrolyzed Type I and Type III collagen peptides homogenized in hyaluronic acid and deionized water to keep the joints, tendons and organs together and support physical integrity as well as improve skin volume, flexibility and firmness, and with the production process of this mixture thereof.

Prior Art

Today, people's living and working conditions, as well as dietary habits are changing. People take supplements for many reasons such as supplementing their regular diets, feeling more vitalized, strengthening the immune system with vitamins and minerals that they are deficient, and meeting the requirements of their body when they cannot eat a balanced and healthy diet.

In the state of the art, hyaluronic acid and/or collagen components are generally included in supplements that are used for purposes such as skin regeneration and anti-aging. Hyaluronic acid is one of the components in the form of a polysaccharide called glucosaminoglycan, which is naturally present in all connective tissues, joints and skin in our body. These components provide the connective tissue with flexibility, strength and moisture. Hyaluronic acid is a miraculous molecule that can hold up to 1000 times its own weight in water.

Similarly, collagen is a type of protein produced by the fibroblasts and other cells. The main function of collagen found in skin and muscle cells is to strengthen connective tissue and maintain physical integrity. Collagen contributes to the connective tissue which protects the muscle and skin cells to provide the skin with flexibility and vitality. It is also responsible for holding joints, tendons and organs together.

In the literature, there is a patent EP1707578A2 for the preparation of low molecular weight hyaluronic acid for use as a food supplement. This patent facilitates the digestion and absorption of collagen by the human body, as well as aims to control its molecular weight and purity. Another document with publication no. EP2983691 B1 relates to a synergistic combination of alanine glutamine, hyaluronic acid and an oat extract, and its use in a compound for cicatrization and in the treatment of cutaneous lesions. In these two patents, hyaluronic acid is combined with components other than collagen. Another document is the patent no. 2017/23070 “Collagen Peptide Used as a Food Additive and its Production Method”. This invention relates to collagen peptide sourced from cattle skin with particle sizes in the range of 2 to 80 daltons, which can be used as an anti-crystallization, homogenization, thickener, emulsifier, and texture and cooking enhancement agent in foods. This patent document contains collagen alone and does not contain any hyaluronic acid.

Another document is the application with the patent no. TR 2019/00114, which relates to the production of a lyophilized (freeze-dried) product which specifically aims to improve skin, hair and nail health where any or all of the ingredients (collagen, hyaluronic acid and vitamin C) is combined with a fruit or vegetable and freeze-dried in any shape (cube, cylinder, triangle, prism, star, heart, etc.) and consumed orally in the final product form or as a powder, in dry form, or mixed with a hot or cold drink.

As can be seen in the state of the art, food supplements containing hyaluronic acid and/or collagen components in the prior art are generally in tablet or powder form. Food supplements that are in the tablet or powder form adversely affect liver enzymes during absorption. In the state of the art, liquid collagen can be provided. Flowever, if the body is vitamins deficient, merely taking liquid collagen is not enough. In addition, anti-aging products that solely contain hyaluronic acid do not provide the desired effect on skin tightening without any vitamins. Apart from these issues, the shelf life of the products in the prior art is not at the desired level. There is a need for a product that has antimicrobial properties, odorless and easy to consume.

As a result, due to the above-mentioned disadvantages, an improvement to the technique was required due to the need for liquid form compositions containing hyaluronic acid and collagen which strengthen the connective tissue, ensure physical integrity and improve skin health. The Object of the Invention

The present invention intends to develop a food supplement composition in liquid form which strengthens the connective tissue that keeps the joints, tendons and organs together, ensures physical integrity, as well as improves the volume, flexibility and firmness of the skin.

The primary object of the invention is to develop a food supplement composition with powerful anti-aging effects which can be consumed directly without dissolving in water to facilitate easy consumption, use and absorption.

Another object of the invention is to develop a composition which combines herbal and animal molecules with vitamins to meet the daily vitamin requirements of the body to a certain extent.

Another object of the invention is to develop a food supplement composition that provides maximum benefit through its formula that nourishes the skin and joints while meeting the daily vitamin requirements.

Another object of the invention is to develop a food supplement composition that does not contain any dyes and/or coloring agents and thus free of side effects caused by active chemical substances.

Another object of the invention is to develop a composition with improved production method which provides with a longer shelf life than food supplements in the prior art.

Another object of the invention is to develop a food supplement composition that has longer shelf life due to its single-use dosage form that prevents oxidation of the remaining products.

One of the objects of the invention to develop a food supplement composition that is easy to consume due to being odorless and tasteless when mixed with water.

In order to achieve the said objects, a food supplement composition which contains Type I and Type III hydrolyzed collagen peptides, hyaluronic acid, Vitamin E and trisodium citrate as PH regulator and buffering agent, as well as a method of production thereof have been developed. To achieve the said objects, in a preferred application of the invention, the composition contains Vitamin E in the form of a dry powder and sodium benzoate as an antimicrobial agent.

To achieve the said objects, in a preferred application of the invention the composition contains Vitamin E dissolved in vegetable oil, polysorbate 20 as emulsifier and butyl hydroxy toluene as antioxidant

To achieve the said objects, the said composition also contains individual elements or combinations selected from the group consisting of Vitamin C, Vitamin B6, Vitamin B3 and Vitamin B2.

To achieve the said objects, the said composition contains sodium saccharin as flavoring agent and D-Limonene which gives a pleasant odor.

The production method developed to achieve the objects of the invention consists of the following process steps:

Heating the deionized water filled into a vessel with a suitable stirrer and homogenizer to 95-1 OOO,

- Cooling the heated deionized water to 25-350,

- Under homogenizer and stirrer operation, adding pH regulators trisodium citrate, Vitamin E and hyaluronic acid, respectively, into deionized water, and stirring after each addition,

- Then addition of Type I and Type III hydrolyzed collagen peptides to the mixture followed by stirring,

- Cooling the mixture to 20-350,

Filtering the cooled homogenized mixture,

To achieve the invention objects, heated deionized water is cooled to 300 and nitrogen gas is passed through it.

To achieve the invention objects, vitamin E is in dry powder form, or, fat or water soluble form. To achieve the said objects, in a preferred application of the invention, the antimicrobial agent sodium benzoate and Vitamin E in the form of a dry powder is added into deionized water after the addition of trisodium citrate and stirred for 15 minutes after each addition

To achieve the invention objects, trisodium citrate, sodium benzoate, vitamin E in the form of a dry powder and hyaluronic acid are each stirred for 15 minutes.

To achieve the said objects, in an alternative application of the invention, trisodium citrate is added to deionized water which is followed by butyl hydroxy toluene as an antioxidant, and stirred for 15 minutes. Also, polysorbate 20 and Vitamin E dissolved in vegetable oil are added to the same mixture as emulsifier and each is stirred for at least 60 minutes until a homogeneous mixture is obtained.

To achieve the invention objects, in a preferred application of the invention, individual elements or combinations selected from the group consisting of Vitamin C, Vitamin B6, Vitamin B3, Vitamin B2 are added after the addition of trisodium citrate and stirred for 15 minutes after each addition.

To achieve the said objects, in a preferred application of the invention, hyaluronic acid followed by sodium saccharin as a sweetening agent is added to the mixture and stirred for 15 minutes.

To achieve the said objects, in a preferred application of the invention, hydrolyzed collagen peptides are stirred for 180 minutes and then the mixture is cooled to 25TT

To achieve the said objects, in a preferred application of the invention, D-Limonene is added to the mixture before filtration.

To achieve the said objects, in a preferred application of the invention, the composition is filled into monodose strips to 5 ml per dose and the opening is closed with automatic machines.

To achieve the said objects, in a preferred application of the invention, pH of the composition is 5.8.

To achieve the said objects, in a preferred embodiment of the invention, the homogenized mixture is filtered through 1.0 micron filters. Detailed Description of the Invention

The invention relates to a food supplement composition in liquid form which strengthens the connective tissue that keeps the joints, tendons and organs together, ensures physical integrity, as well as improves the volume, flexibility and firmness of the skin, and its method of production thereof. The said food supplement composition comprises a liquid form enriched with vitamin complexes of hyaluronic acid and hydrolyzed collagen. In addition, the invented composition contains pH regulating and buffering agent, antimicrobial agent, anti degrading components, emulsifier, antioxidant, vegetable oil, sweetening agent and various excipients selected from a group consisting of perfuming components.

The said composition contains Type I and Type III hydrolyzed collagen peptides obtained from cowhide. In the invented method, collagen peptides are homogenized by dissolving in deionized water. However, collagen marinade may also be used within the scope of the invention. Collagen gives skin flexibility, firmness and strength. It supports the flexibility and healing of the muscles and ligaments. It reduces wrinkles and cracks on the skin, strengthens hair and nails, reduces the fat in the blood vessels and heart.

Hyaluronic acid is a high molecular weight, negatively charged linear that resides in the extracellular matrix of connective tissue. It is the simplest and only sulfate-free member of the connective tissue proteins group called glycosaminoglycans. It is found in vitreous fluid of the eye, hyaline cartilage, joint fluid, dermis and epidermis. Compared to other natural and synthetic polymers, it has a high degree of moisture retention. Hyaluronic acid plays an important role in hydration and moistening of tissues, transfer of substances through tissues, movement and differentiation of cells. Hyaluronic acid is obtained from either animal sources or bacteria by fermentation and direct isolation methods. Hyaluronic acid is mostly dispersed in the dermis layer of the skin. However, it can also be found in the epidermis, which is vital for moisturizing the skin. It revitalizes and gives volume to the skin which has a dull and pale appearance because of dehydration. It helps to heal sun burns and skin wounds faster, and protects the mouth tissue by keeping the moisture in the injured tissues (e.g., herpes and aphthae). Thanks to its anti-aging properties, it helps to eliminate fine lines. Hyaluronic acid is a kind of antioxidant and thus has the ability to reduce inflammation.

In this invention, Vitamin E is in dry powder form or dissolved in vegetable oil. Water-soluble Vitamin E can also be used. Vitamin E strengthens the immune system, contributes to the formation of red blood cells, prevents blood clotting and regulates blood circulation. It helps prevent cardiovascular diseases and contributes to faster healing of wounds. It also protects the composition of the invented food supplement thanks to its antioxidant properties.

In addition, Vitamin C and vitamin B complex (Vitamin B6, Vitamin B3, Vitamin B2) can be used for the invention. Vitamin C (Ascorbic Acid) increases the production of collagen in the body. It also increases the number of antioxidant molecules in the blood and reduces risks such as clots and heart attacks by helping to stabilize blood pressure. It reduces the risk of infection and protect the body against diseases such as influenza and colds. It should be taken from the body as an external supplement.

Vitamin B complex of vitamins (Vitamins B6, B6, B3 and B2) contribute to the normal energy formation metabolism. Vitamin B6 (Pyridoxine HCI) contributes to normal protein and glycogen metabolism and cysteine synthesis. In addition to the formation of red blood cells, it helps to fight fatigue and asthenia. Vitamin B3 (Nicotinamide) contributes to the maintenance of normal skin structure, and helps to fight fatigue and asthenia. Vitamin B2 (Riboflavin) is involved in the structure of two important enzymes, FAD and FMN, which are involved in energy metabolism. It helps to protect red blood cells, and maintain normal skin structure and eye health.

Trisodium citrate which is included in the invented formulation is a salt of citric acid and maintains the food supplement composition at the desired pH of 5.8. It serves as a pH regulator and buffering agent.

In a preferred application of the invention, the composition contains sodium benzoate as an antimicrobial agent when Vitamin E in the form of a dry powder is included. Sodium benzoate is a food additive obtained by neutralizing benzoic acid with sodium bicarbonate, sodium carbonate or sodium hydroxide.

In an alternative application of the invention, when the said composition contains Vitamin E, it contains polysorbate 20 as emulsifier, butyl hydroxy toluene (BHT) as antioxidant, and vegetable oil. Butyl hydroxy toluene (BHT) is used as a food antioxidant in the state of the art, and these phenol derivatives react with free radicals, slowing down the rate of autoxidation, which leads to changes in the color and flavor of food. In other words, it extends the shelf life of the invented food additive. Also, Polysorbate 20 is used as an emulsifier

The invention contains sodium saccharin as sweetening agent and D-Limonene which gives a pleasant odor. Having ideal physical properties for use as a sweetener, saccharin is extremely stable under all conditions to which food may be exposed. D-Limonene is a terpene group compound which is obtained from citrus peel and gives the smell of lemon peels. Pure water, which is used as a solvent, dissolves all components. The contents of the composition and the amounts in kg are given in Table 1 and Table 2 for illustration purposes. Table 1 shows the composition containing Vitamin E, sodium benzoate and polyvinylpyrrolidone in dry powder form and Table 2 shows the content ratios and amounts of the composition containing fat-soluble Vitamin E, polysorbate 20, butyl hydroxy toluene and vegetable oil. The amounts in the content are not limiting but may be used in wider ranges.

Table 1 : Content and percentage amounts (in kg) of the invented food supplement composition

Table 2: Content and percentage amounts (in kg) of an alternative application of the invented food supplement composition

Production method:

The production method of the invented food supplement composition according to the content of Table 1 comprises following process steps:

- Cooling the heated deionized water to 25-350, pr eferably to 300,

- Passing nitrogen gas through cooled deionized water,

- Addition of trisodium citrate, sodium benzoate, Vitamin B6 (Pyridoxine HCI), Vitamin B2 (Riboflavin), Vitamin B3 (Nicotinamide), Vitamin E (50% dry powder), Vitamin C (Ascorbic Acid), hyaluronic acid and sodium saccharin into deionized water, respectively, under homogenizer and stirrer, followed by stirring for 15 minutes after each addition,

- Then addition of Type I and Type III hydrolyzed collagen peptides to the mixture followed by stirring for 180 minutes,

- cooling the mixture to 20-350, preferably to 25° C,

Finally addition of D-Limonene to the mixture,

Filtration of the cooled homogenized mixture through 1.0 micron filters,

- Filling the resulting composition into monodose strips to 5ml per dose and closing with automatic machines.

The alternative production method of the composition according to the content of Table 2, somewhat differs from the method of production of the composition in Table 1. The first of these differences is the addition of butyl hydroxy toluene (BHT) without the addition of sodium benzoate after adding trisodium citrate. Since fat-soluble Vitamin E and vegetable oil are used instead of dry form in this method, polysorbate 20 is added after adding and stirring sodium saccharin to the composition. After polysorbate 20, fat-soluble Vitamin E is added to the mixture. The method of production is the same after the addition of collagen peptides.

The alternative production method of the invented composition according to the content of Table 2 comprises the following process steps: - heating the deionized water filled into a vessel with a suitable stirrer and homogenizer to 95-1 OOO,

- cooling the heated deionized water to 25-35^tC, pr eferably to 30Ό,

- passing nitrogen gas through cooled deionized water,

- adding trisodium citrate, butyl hydroxy toluene, Vitamin B6 (Pyridoxine HCI), Vitamin B2 (Riboflavin), Vitamin B3 (Nicotinamide), Vitamin C (Ascorbic Acid), hyaluronic acid and sodium saccharin into deionized water, respectively, under homogenizer and stirrer, stirring for 15 minutes after each addition,

- once the said vitamins are completely dissolved, polysorbate 20 is added to the mixture and stirred for at least 60 minutes until a homogeneous mixture is achieved,

- depending on the amount of fat-soluble vitamin E, dissolving in the appropriate amount of vegetable oil,

- adding the Vitamin E dissolved in vegetable oil into the mixture and stirring for at least 60 minutes until a homogeneous mixture is obtained,

- cooling the mixture to 20-35‘C, preferably to 25° C,

Finally adding D-Limonene to the mixture,

- filtering the cooled homogenized mixture through 0.2 micron filters,

If the targeted density and viscosity is high in the final product, it is diluted with deionized water. pH, density, and viscometer temperature is 25Ό for filtration, filling and analysis.

The invented food supplement composition can be taken three times a day before or after meals. However, it is advisable to consume in fed condition whenever possible. It can be consumed by adding to a glass of water or directly. Drinking one glass of water is advisable if taken directly. It has been observed that when used regularly, it provides maximum benefit after a minimum of 15 days of use.

The invention contains Type I and Type III bovine collagen. However, collagen marinade may also be used. In addition to these vitamins, additional vitamin complexes can be included individually or in combination as needed.

Claims

1. A liquid food supplement composition that strengthens the connective tissue and holds the joints, tendons and organs together and enables body integrity, as well as providing the skin with volume, flexibility and firmness and it is characterized by the fact that it comprises Type I and Type III hydrolyzed collagen peptides homogenized in deionized water, hyaluronic acid, Vitamin E, and trisodium citrate (pH regulator).

2. The composition according to Claim 1 characterized by the fact that nitrogen is passed through deionized water.

3. The composition according to Claim 1 characterized by the fact that vitamin E is in dry powder, or, fat or water soluble form.

4. The composition according to Claim 3 characterized by the fact that it contains Vitamin E in the form of dry powder and sodium benzoate as an antimicrobial agent.

5. The composition according to Claim 3 characterized by the fact that it contains Vitamin E dissolved in vegetable oil, polysorbate 20 as emulsifier and butyl hydroxy toluene as antioxidant.

6. The composition according to Claim 1 characterized by the fact that it contains individual elements or combinations selected from the group consisting of Vitamin C, Vitamin B6, Vitamin B3 and Vitamin B2.

7. The composition according to Claim 1 characterized by the fact that the pH of the said composition is 5.8.

8. The composition according to any of the previous claims characterized by the fact that it contains sodium saccharin as sweetening agent.

9. The composition according to any of the previous claims characterized by the fact that it contains D-Limonene which gives a pleasant odor.

10. The production method for a food supplement composition in liquid form which strengthens the connective tissue that keeps the joints, tendons and organs together, ensures physical integrity, as well as improves the volume, flexibility and firmness of the skin characterized by;

- heating the deionized water filled into a vessel with a suitable stirrer and homogenizer to 95-1 OOO,

- the heated deionized water is cooled down to 25-35^tC,

- under homogenizer and stirrer operation, pH regulators trisodium citrate, Vitamin E and hyaluronic acid, respectively, are added into deionized water, and stirred after each addition, - Then addition of Type I and Type III hydrolyzed collagen peptides to the mixture followed by stirring,

- the mixture is cooled down to 20-35^tC,

- the cooled homogenized mixture is filtered

11. The method according to Claim 10 characterized by the fact that the said heated deionized water is cooled down to 300.

12. The method according to Claim 10 characterized by the fact that the said cooled deionized water is passed through nitrogen.

13. The method according to Claim 10 characterized by the fact that vitamin E is in dry powder, or fat- or water-soluble form.

14. The method according to Claim 13 characterized by the fact that sodium benzoate as antimicrobial agent and dry powder Vitamin E after trisodium citrate is added into deionized water.

15. The method according to Claim 14 characterized by the fact that the said trisodium citrate, sodium benzoate, polyvinylpyrrolidone, dry powder Vitamin E and hyaluronic acid are added and each is stirred for 15 minutes after addition.

16. The method according to any of Claim 10 to 13 characterized by the fact that trisodium citrate is added to deionized water which is followed by butyl hydroxy toluene as an antioxidant, and stirred for 15 minutes.

17. The method according to Claim 16 characterized by the fact that polysorbate 20 and Vitamin E dissolved in vegetable oil are added to the same mixture as emulsifier and each is stirred for at least 60 minutes until a homogeneous mixture is obtained.

18. The method according to Claim 10 characterized by the fact that individual elements or combinations selected from the group consisting of Vitamin C, Vitamin B6, Vitamin B3, Vitamin B2 are added after the addition of trisodium citrate and stirred for 15 minutes after each addition.

19. The method according to Claim 10 characterized by the fact that hyaluronic acid followed by sodium saccharin as a sweetening agent is added to the mixture and stirred for 15 minutes.

20. The method according to Claim 10 characterized by stirring the said hydrolyzed collagen peptides for 180 minutes.

21. The method according to Claim 10 characterized by addition of the hydrolyzed collagen peptides to the said mixture followed by stirring and then cooling down to 250.

22. The method according to Claim 10 characterized by the fact that D-Limonene is added to the mixture before filtration.

23. The method according to Claim 10 characterized by the fact that the resulting composition is filled into monodose strips to 5ml per dose and closing with automatic machines.

24. The method according to Claim 10 characterized by the fact that the pH of the said composition is 5.8.

25. The method according to Claim 10 characterized by the fact that the homogenized mixture is filtered through 1.0 micron filters.