TWI339125B - Aqueous solution of ascorbic acid and method for producing same - Google Patents

Description

Ϊ339125 V. INSTRUCTION DESCRIPTION (1) 1. TECHNICAL FIELD OF THE INVENTION The present invention relates to an aqueous solution of ascorbic acid. A commercially available use of a reducing ketone such as ascorbic acid, especially in terms of personal hygiene and food nutrition, and its use in preventive use, often becomes very difficult because of insufficient stability of ascorbic acid in aqueous solutions. Ascorbic acid solution, the ascorbic acid still present in about 30 days was only about 7 〇%. To this end, we have tried to improve the stability, instead of using ascorbic acid, instead of using one of the derivatives of U-ascorbic acid, for example, sodium ascorbate or ascorbyl acid paste. The active substance in the aqueous solution is kept for a long time. However, the price of a relatively pure ascorbic acid derivative is several times higher. In addition, at a higher concentration, the ascorbic acid derivative is easily crystallized to cause coloration of the final product. Second, [prior art]

, the stability of ascorbic acid β ^ European Patent Specification No. 660676 is known to contain a bismuth, 1 to 2.0 weight S% and a coloring class of carotenoids oil-soluble New Zealand ingredients, 2 to 20 weight 1 0 The emulsifier and 〇·1 to 1. 〇 % ^ ^ 充 充 充 充 、 、 、 、 聚 聚 聚 聚 聚 聚 聚 聚 聚 聚 聚 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 Thus, the use of this process should be able to produce a clean, stable beverage. However, about the final product

[Summary of the Invention]

!,· is to provide ascorbic acid with a fluid, water • form (for example: gelatin capsules). Ascorbic acid is stable, 1339125 V. Description of the invention (2) Sex can be maintained for many months without change and can be obtained in a high concentration form. According to the present invention, the object is to provide an aqueous solution of an acid resistant acid having an excess emulsifier having an HLB value of from 9 to 18, for example, a polysorbate, and preferably a polysorbate 80. The solution is pure at room temperature and is almost a gel. The solution can be diluted with water without becoming turbid, and when heated to about 35 C, without further processing, it can be taken without difficulty from the cosmetic or food field. The aqueous liquid or the aliphatic product is evenly mixed. According to the present invention, the portion of ascorbic acid in the solution can be as much as 2% by weight, and can be stored for at least half a year with almost no loss. As for the polysorbate portion, it is actually about 60% by weight. The remainder is water. According to the present invention, the anti-bad ▲ acid solubilized product can be easily added to cosmetics (skin, hair care products), food, medicine, pharmaceutical and nutrient solution for breeding of cells and bacteria, and for use in seaweed (microalgae) As a result, the stability of the product is greatly improved. The ascorbic acid is available in the form of micelles in the solubilized solution, and the 丨0% in the dilute solution of 1:100 ratio is examined under an electron microscope. When the ascorbic acid is solubilized, the diameter of the micelles is about 100 nm (nm). Since the emulsifier film which is slightly trapped releases the ascorbic acid only in a delayed (delayed manner), the above solvent is solubilized according to the present invention. The anti-sputum effect of the substance is combined with solubilized tocopherol (vitamin E) and, for example, ascorbyl palmitate, that is, a previously described ascorbic acid derivative is maintained for a longer period of time. In the aspect of the present invention, during the oral administration of the solubilizate of the present invention, the assimilation of the ascorbic acid by the emulsifier (micellati〇n) 1339125 5, the invention description (3) can prevent the ascorbic acid from taking effect It should be consumed in the central digestive tract, that is, in the stomach and duodenum. The micro-agglomerate is the first to be sucked back in the small intestine. In a particularly preferred embodiment of the invention, ascorbic acid Solubilized matter includes an increase in the mixture of the raw moons, especially a mixture of α _, cold _, γ - and occupant - vitamin E. Through the organic oil, for example: vegetable oil such as: sunflower oil 'lily oil, The addition of the above ascorbic acid tocopherol solubilized with linseed oil can greatly improve the stability of the above solvents. As a tocopherol, pure α-fertility or a particularly optimal 〇;-, cold-, γ_ and 5 can be considered. a tocopherol mixture, the recommended mixed tocopherol is from about 8. 〇 to about 2 〇. 〇% by weight of α-probiotics, about 1.5 to 4. 5 wt% of no tocopherol, about 55. 〇 to about 70% by weight of γ-tocopherol and about .5. 〇 to about 2 7. 〇% by weight of tocopherol. If added to the solution according to the invention, for example: α _ sub-linen (ren) oleic acid, gamma-linolenic acid, linoleic acid or oleic acid in the form of octadecatrienoic acid and / or octadecenoic acid, the viscosity of the solution is weakened. Obviously, the water can be diluted or viscous in the absence of turbidity at room temperature, without further processing steps. And / or aliphatic nutritional products 'cosmetic and drug mixture mixed. According to the invention, the polysodium succinate containing stem 'is an ointment and similar preparations can generally be easily oxidized composition ^

A type of hysteresis function that produces a conservative property against bad acid is produced, and thus the beneficial protective function time of the blood acid is retained and prolonged. The amount of anti-bad two == in the solution can be between 5% and about 15% by weight, and the solution contains from about 3% to about 20% by weight of octadecatrienoic acid and/or oleic acid.

1339125 V. Description of invention (4) Benefit. The polysorbate portion is preferably from about 60% by weight to about 75% by weight. If the proportion of water in the solution is reduced to between about 5% by weight and about 7% by weight, the proportion of polysorbate is increased accordingly. The solution which exhibits viscosity at room temperature can also be mixed with the active substance. Thereafter, the mixture is filled in gelatin capsules or gelatin-free capsules. Since the proportion of water in the solution is low, the capsule shell is intact, so that the ascorbic acid protects the active ingredient intact. A procedure for preparing a solution according to the present invention is to use an emulsifier having an HLB value of about 9 to 18, a polysorbate such as polysorbate 80, added to a hydrous septic acid solution. The mixture is heated briefly by stirring until it becomes pure and homogeneous. The formation of micelles in the solution and having a diameter of about 1000 nm, which results in a double-walled cladding of a radially oriented polysorbate molecule, such that the polysorbate molecules of the inner shell are aligned and their hydrophilic segments are oriented The ascorbic acid solution, while the hydrophilic segments of the polysorbate molecules in the outer shell are arranged outward. The solution obtained in this way can be diluted with water without turbidity and can be industrially employed without further processing steps. In a further development of the invention, the stability of the micelles is increased when a lightly oily oil consisting essentially of triglyceride, for example, prunus oil, together with an emulsifier, is added to the aqueous ascorbic acid solution. The resulting oil is slightly trapped and adheres to and protects the ascorbic acid micelles. Octadecyl tribasic acid and/or octadecenoic acid, for example, α-linolenic acid, quinone-linolenic acid, linoleic acid or oleic acid, before the actual addition of polysorbate Heat to about 5 (after TC is added to the solution for filling the capsule, the capsule is made of gelatin or the capsule can be free of

1339125 V. Description of the invention (5) Glue, if the ascorbic acid is dissolved in the same amount of distilled water, add the same amount or add up to twice the fatty acid and the polysorbate 8 under the slight heating. 0 about two to about three times the amount, the mixture is heated to about 80 ° C and stirred. 4. Embodiments The following examples are illustrative of the present invention. Example 1 20 g of ascorbic acid was completely dissolved in 20 g of degassed distilled water. If the water is heated to about 45 °, the dissolution phase can be accelerated. Thereafter, 60 g of polysorbate 80 was added to the solution while stirring and heating to about 80 °C. Stir until the added material becomes clear and uniform. The added material appears clear and almost gelatinous at room temperature, can be diluted in water without causing turbidity, and can be added without further processing steps. Preserved composition or food, beverage, cosmetics and pharmaceuticals. For the lower concentration solubilisate, 10 g of ascorbic acid was dissolved in 10 g of distilled water and 80 g of polysorbate was added, and the rest of the process was the same as described above. An electron micrograph of the copy reproduced in the first figure was prepared from the solubilized solution of the 10% ascorbic acid solubilized product prepared above after dilution with hydrazine water to 1:100. It can be seen that the ascorbate solubilized micelles have a diameter of about 100 nm. Place the solubilized material in paraffin to reduce the diameter of the micelle by half, as can be seen from the electron micrograph below in the first image. This phenomenon can be explained by the loss of the polysorbate outer membrane in the paraffin. Example 2 As in Example 1, 10% by weight of ascorbic acid (based on: ascorbic acid)

Page 8 1339125 V. Description of the invention (6) Total amount of solubilized material = 100%) dissolved in 10% by weight of distilled water in an aqueous solution together with 1% by weight of light vegetable oil such as: \ϋ or flax The seed oil was added to 70% by weight of polysorbate. Then, the aqueous solution is heated to at least 60 ° C and mixed until the solubilized material becomes clear and homogeneous, and the solution is dissolved in water to be transparent and free of residue at room temperature. If the ascorbic acid content is reduced to about 7% by weight, the water content is also reduced to about 7% by weight, and the other ratios of the solubilized material are increased, because the ratio of water is low, and particularly suitable for use as A preservative that delays the formulation and is necessary to encapsulate the active material. The capsule sleeve is virtually completely eroded by the expected high water content solubilization. Example 3 10 g of ascorbic acid was dissolved in 10 g of distilled water, and 20 g of I, _fishing_. was added to the solution. To this mixture was added 1 1 gram of polysorbate 80, and the whole was stirred and heated to about 100 ° C to the whole anhydrous portion, i.e., until the boiling was terminated. After the solution is cooled to room temperature, 6. 5 ° / ascorbic acid solubilisate appears in the solubilizer, the water content of the solubilized solution is undoubtedly less than 5% by volume, and has water solubility and fat, oil Medium soluble. The ascorbic acid content of the test solution was carried out by an independent chemical laboratory at the time of solution generation and over a period of 5 months. The test results showed that the ascorbic acid loss was only about 3% throughout this period. Example 4 The starting point of this example is a solubilized material according to Example 2. A mixed tocopherol solubilized product prepared in the following manner is added to the solubilized material. 10% by weight of mixed tocopherol (based on: mixed tocopherol solubilizer = 1.0% by weight) 1339125 V. Description of the invention (7) By stirring and mixing with 90% by weight of polysorbate 20, Heating to about 60 °C speeds up the mixing process. Continue to stir until the mixture is clear and clear, and the solubilized material can be easily dissolved in the water. For mixed tocopherols, it is recommended to add 91 mg/g of α-tocopherol mixed tocopherol, 21 mg/g/3-tocopherol mixed tocopherol, 608 mg/g r-tocopherol mixed tocopherol and Mixed tocopherol of 209 mg/g <5-sodium phenol. Then, according to the first alternative in Example 2, 3 parts by weight of the solution was mixed with about 7 parts by weight of the mixed tocopherol solubilized, thereby slightly heating to about 50 ° C to accelerate the mixing process. Stirring is carried out under heating until a homogeneous and clear solubilized material is produced. Thus, 1 gram of product contains about 70 mg of mixed tocopherol and 30 mg of ascorbic acid. The present example solubilized material, as an effective antioxidant, can be used to improve the stability of food dyes, oils, cosmetics, pharmaceuticals and the like. Comparative tests have shown that no matter what is ultimately produced (hydrophilic or hydrophobic), the present solution can be directly incorporated into the final product without intermediate production stages, and provides a greater amount of an ascorbic acid derived organism, such as For example: ascorbic acid ascorbate has better anti-oxidation effect. Moreover, it is also advantageous to compare ascorbic acid derivatives with less pigment in the solubilized solution. In addition, depending on the requirements, about 1 000 g is finally produced. The product may be added, for example, from 1 to 10 g of solubilized material. From a nutritional point of view, a physiological advantage of the solubilized material of the present example is that the micelle stability in gastric acid is good and ascorbic acid is ensured ( Vitamin C) and (with α-tocopherol) vitamin E reach the small intestine without loss and is absorbed in the small intestine. This advantage can also be used in other vitamins, for example

Page 10 1339125 V. Description of the invention (8) For example: retinol (vitamin A) and phyto-carotene, and can be obtained as follows: a preparation comprising a multivitamin composition: _ Example 5 20% by weight of a Tocopherol is mixed with 80% by weight of polysorbate 20 at a heat necessary at about 50 ° C until it becomes clear, transparent and homogeneous by stirring the mixture. 10% by weight of retinol was mixed with 90% by weight of solubilized material 80 in the same manner. Finally, in a suitable way, 10% by weight contains about 30-carrots.

The concentrate (available from La Roche) was mixed with 90% by weight of polysorbate 80 to form a reddish brown transparent solubilized material which was clearly dissolved in warm water.

Subsequently, 85 wt% of the ascorbic acid solubilized according to the first choice in Example 2 and 10% by weight of the above <2 - fertility solubilized solution and 2% by weight of the above retinol solubilized product And the last 3 wt% of the/5-carotene solubilized material is effectively mixed under gentle agitation until a homogeneous and transparent mixed solubilized material is obtained. The water-soluble vitamin solubilizer can be enclosed in gelatin capsules or gelatin-free capsules, or the vitamin solubilized product can be directly incorporated into the water-soluble and/or fat-soluble end product without additional processing steps. The vitamin solubilisate according to the present invention, unlike emulsions or liposomes, forms a stable, clear solution when placed in water and/or clear juice. The product micelles have good stability in gastric acid. The absorption of fat-soluble substances in the micelles such as vitamin A, vitamin E and /3 - carotene occurs in the small intestine and does not involve bile salts and enzymes. Therefore, this piece of micelle

Page 11 1339125 V. INSTRUCTIONS (9) The active substances cited in the shape are more rapidly bioacquired. '1 gram of vitamin solubilized material of the aforementioned composition, incorporated into food or encapsulated capsules can replenish the daily essential vitamins A, C, E and /3 - carotene. The composition of the vitamin solubilized material with the previous figures is cited to prepare for this application. Taking into account the daily essential vitamin C, the fact is higher than the requirements for other vitamins. However, the scope of the present invention is that the vitamin solubilizing agent can also be selected from other compositions and/or intended use. If a certain vitamin needs to be removed or is not necessary, the vitamin or other vitamin may be omitted altogether. The second, third and fourth graphs show the average micelle radius (or radiation) of α-fertility solubilized, /3 - guaranin solubilisate and retinol solubilized. As can be seen, the average micelle radius is 10 nanometers, and the retinol solubilisate is reduced to just about 8 nanometers. All measurements were performed using field flow fractionation by Wyatt Technologies. The fifth image shows an electron microscope image of a vitamin A micelle, and the sixth image shows an electron microscope image of a vitamin E micelle. The sample was a 1:1000 aqueous solution of the solubilized solution described above.

1339125 Simple description of the figure ~~~- ~ The third part shows the micro-cluster map of vitamin C, which is the first time that the scientific community can observe through electron microscopy (authorized by AQUANOVA at the Technical University of Darmstadt, Germany) Liquid stable anti-adhesive acid vitamin C micro-difficulties: 1 〇% ascorbic acid and acid addition, diluted 1: 1 〇〇〇 above a) Under water b) Paraffin paraffin, double-walled ascorbic acid micelle Remove the outer shell. The first, second and fourth graphs show the mean microsphere radius (radiation) of 01 - fertility plus dissolved matter 'cold_carotene solubilisate and retinol solubilized matter. The fifth picture shows the finished micro-cluster map (produced by AQUAN〇VA at the Da Shitat University of Technology in Laos) for the first time by electron microscopy; as seen in aqueous solution (1:1 0 0 0), in the figure From left to right: a picture is a figure of vitamin eight micro-clusters in water-soluble AQUANOVA retinol added. Figure b is a graph of tocopherol micelles in AQUANOVA. The ε image is a probiotic substrate. Path..., micro Figure 6 shows the radial distribution of the micelle AQUAN〇VA vitamin E and the vitamin A addition in the aqueous solution. μ

Claims (1)

1339125 , ' 〇 ':: 6-1, patent application range 1 · An aqueous solution of ascorbic acid containing an excess of emulsifier having an HLB value of about 9 to 18, the aqueous solution containing ascorbic acid content of up to about 20% by weight, including The emulsifier is a polysorbate in the range of about 60 to 80% by weight, and the rest is water; the aqueous solution is used as an additive in various foods, cosmetics, pharmaceutical agents, and for cell and bacterial culture or In the nutrient solution of algae cultivation. 2. The aqueous solution of claim 1, wherein the aqueous solution contains polysorbate 80 as an emulsifier. 3. If the aqueous solution of claim 1 or 2 is applied, the aqueous solution is added with α-fertility. 4. If the aqueous solution of claim 1 or 2 is applied, the aqueous solution is mixed with tocopherol. 5至4. 5重量%的/3 - 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 Tocopherol, from about 50.5 to about 70.0% by weight of 7-tocopherol and about 15.0 to 27.0% by weight of 5-tocopherol. 6. The aqueous solution according to any one of claims 1 to 5, wherein the aqueous solution contains octadecatrienoic acid and/or oleic acid. 7. The aqueous solution of claim 6, wherein the aqueous solution contains 10 to 20% by weight of octadecanoic acid and/or octadecyl acid. 8. The aqueous solution of claim 6, wherein the aqueous solution comprises: alpha-linolenic acid, gamma-linolenic acid, linoleic acid or oleic acid. 9. If the aqueous solution of claim 1 is applied, the aqueous solution has an ascorbic acid content of 10% by weight, a water content of 10% by weight, and a polysorbate 80. Page 14 1339125 VI. Patent application The content is 80% by weight. 1 0. The aqueous solution of claim 1, wherein the aqueous solution has an ascorbic acid content of 10% by weight, a water content of 10% by weight, and a content of 10% by weight of light vegetable oil, including plum oil, Sesame oil, and polysorbate 80 in an amount of 70% by weight. 1 1. An aqueous solution according to claim 10, wherein the aqueous solution contains three parts by weight of a solution and seven parts by weight of a mixed tocopherol solubilizing agent, wherein the solubilizing substance contains 10% by weight of mixed tocopherol And 90% by weight of polysorbate 20. 1 2 . The aqueous solution of claim 1 of the patent scope, the aqueous solution containing 85 wt% of the solution, 10 wt% of < 2 - fertility solubilisate (solubilized matter), 2 wt% of vitamin A increase a solution and a 3% by weight cold-carotene solubilizate; wherein the α-tocopherol solubilizate contains 20% by weight of α-tocopherol and 80% by weight of polysorbate 20, and the vitamin Α solubilizer Containing 10% by weight of vitamin A and 90% by weight of polysorbate 80, and the ruthenium-carotene solubilizer contains 90% by weight of polysorbate 80 and 10% by weight of concentrated liquid, and The concentrate contains 30% by weight of /3 - carotene. An aqueous solution of the third or fourth aspect of the patent application is used as an additive for organic oils of sunflower oil, hazelnut oil, and linseed oil. 1 4. An aqueous solution according to claim 12, which is used as a filling for a capsule or as an additive for fruit juice. 1 5. The aqueous solution of claim 1 of the patent scope, the aqueous solution contains 10 weight Page 15 1339125 VI. Patent application range % ascorbic acid, 10% by weight of water, 20% by weight of hazelnut oil, and 11% by weight of polysorbate 80. 1 6. A method for preparing an aqueous solution of ascorbic acid according to claim 1, wherein the method comprises: adding polysorbic acid to the aqueous solution, and stirring the mixture under mild heat until it becomes clear and uniform. step. 17. The preparation method of claim 16, wherein the method comprises the step of adding polysorbate 80 directly to the aqueous solution. 18. The preparation method according to claim 16, wherein the method comprises the steps of: adding a natural oil having a main component of triacetin to the aqueous solution, and simultaneously mixing the emulsifier. 19. The preparation method of claim 18, wherein the method comprises the step of adding eucalyptus oil to the aqueous solution. 2 0. The preparation method of claim 16 to 19, which comprises: adding eighteen carbons before adding the polysorbate to the aqueous solution and slightly heating to about 50 ° C with stirring The step of trienoic acid and/or oleic acid. 2 1. The preparation method according to claim 20, wherein the method comprises: adding to the aqueous solution an 18-carbon three in the form of α-linolenic acid, 7-linolenic acid, linoleic acid or oleic acid. The step of an enoic acid and/or oleic acid. 2 2. The preparation method of claim 17, wherein the method comprises: dissolving 20% by weight of ascorbic acid in 20% by weight of water, followed by stirring 60% by weight of polysorbate 80 And heated to about 80 ° C Page 16 1339125 VI. Scope of Application The procedure is to add it to its mixed solution and then stir until the mixture becomes clear and homogeneous. 2 3 . The preparation method of claim 2, wherein the method comprises the step of slightly heating the water to about 45 ° C in order to accelerate the dissolution process. 2 . The preparation method of the ascorbic acid solution of claim 15 in the patent application scope, wherein the method comprises: dissolving 10% by weight of ascorbic acid in 10% by weight of water, and in solution 20% by weight of hazelnut oil was added, and 110% by weight of polysorbate sorbate 80 was added, heated to about 1000 ° C and stirred until the end of the cooking process.