KR100876308B1 - Manufacturing method of water-soluble tocopherol emulsion - Google Patents

Abstract

A method for preparing a water-dispersible tocopherol emulsion, a water-dispersible tocopherol emulsion prepared by the method, and a food containing the water-dispersible tocopherol emulsion are provided to allow the food or cosmetics containing tocopherol hardly soluble in water to be made. A method for preparing a water-dispersible tocopherol emulsion comprises the step of mixing 0.1-5 wt% of a hydrophobic surfactant, 0.1-5 wt% of a hydrophilic surfactant, 50-80 wt% of an aqueous solvent and the balance of tocopherol. Preferably the hydrophobic surfactant is at least one selected from the group consisting of polyglycerin polyricinoleate, glycerin monostearate and glycerin monooleate; and the hydrophilic surfactant is at least one selected from the group consisting of polyglycerin monostearate, polyglycerin monooleate, polyoxyethylene sorbitan monooleate, and polyoxyethylene sorbitan monolaurate.

Description

Manufacturing method of water dispersible tocopherol emulsion {Manufacturing method of water-soluble tocopherol emulsion}

1 is a graph showing the results of measuring the surface tension of 20 to 40% tocopherol and glycerin (or water) emulsions according to the composition of hydrophobic and hydrophilic surfactants,

Figure 2 is a graph showing the result of measuring the degree of destruction of the oil phase under a certain storage conditions in order to test the storage stability of the 20% tocopherol emulsion prepared according to an embodiment of the present invention,

Figure 3 is a graph showing the result of measuring the degree of destruction of the oil phase under a certain storage conditions in order to test the storage stability of the 30% tocopherol emulsion prepared according to an embodiment of the present invention,

Figure 4 is a graph showing the result of measuring the degree of destruction of the oil phase under a certain storage conditions in order to test the storage stability of the 40% tocopherol emulsion prepared according to an embodiment of the present invention.

The present invention relates to a process for producing a water dispersible tocopherol emulsion.

Tocopherol, commonly called vitamin E, is synthesized by green plants and photosynthetic bacteria and is contained in many plants.

It is reported that food is a natural antioxidant that prevents oxidation of food, and in vivo has physiological functions and nutritional activities such as prevention of circulatory disease and cancer, prevention of aging and degenerative diseases, and anti-fertility. It is known that regular administration of α-tocopherol has the effect of inhibiting the progression of atherosclerosis and preventing cataracts.

In addition, it is reported that taking tocopherol may lower blood cholesterol levels, promote wound healing, and have an excellent effect on treating scars of burns. In addition, it protects the respiratory mucosa from air pollution, and has various physiological effects such as detoxification, maintenance of intracellular membranes, skin eczema, edema, improvement of blood lesions, and enhancement of immune function.

Tocopherols having these various physiologically active functions cannot be synthesized directly in vivo, and therefore must be taken from food or food.

However, there is a problem that the use effect of tocopherol, which is oil-soluble (fat-soluble), is not large because our bodies are water phases containing about 70% water.

To date, many studies have been conducted on the mechanism of action of tocopherol in vivo and its antioxidant properties in foods. However, studies to increase the efficiency of use by solubilizing the oil solubility of tocopherol has been insufficient in the food field.

It is an object of the present invention to provide a method for preparing a water dispersible tocopherol emulsion for easily adding tocopherol which is not soluble in water to water-soluble foods, cosmetics and the like.

In order to achieve the object of the present invention,

The present invention can provide a method of preparing a water dispersible tocopherol emulsion by mixing a hydrophobic surfactant, a hydrophilic surfactant, an aqueous solvent and a tocopherol.

 According to the process of the invention, the water dispersible tocopherol emulsion comprises from 0.1 to 5% by weight of said hydrophobic surfactant, from 0.1 to 5% by weight of hydrophilic surfactant and from 50 to 80% by weight of aqueous solvent and an appropriate amount of tocopherol.

Here, when the hydrophobic surfactant is added less than 0.1% by weight, the stability of the emulsifier is lowered to cause oil separation, and when included in excess of 5% by weight, the amount of the hydrophilic surfactant is increased to increase the viscosity of the emulsion. There is a problem that the dispersion force in the water phase is lowered.

When the hydrophilic surfactant is added less than 0.1% by weight, the water dissipation capacity of the emulsifier is weakened, so that waste emulsification occurs quickly. When the hydrophilic surfactant is included in an amount of more than 5% by weight, the viscosity of the emulsion is not only increased sharply but also the manufacturing cost. There is a problem that rises.

When less than 50% by weight of the aqueous solvent is added, emulsions containing more than 50% of the oil-soluble component have a problem in that, as the viscosity rises sharply, a phase change occurs with W / O in the existing O / W type), and more than 80% by weight. If it is included in the (substantially effective amount of the active substance (tocopherol) is contained in the content is too small to expect the effect.

The present inventors prepared a stabilized tocopherol emulsion by water-oxidizing a tocopherol having an oil-soluble solubility using hydrophilic and hydrophobic surfactants in order to be able to express many physiologically active functions of the fat-soluble tocopherol.

The molecular weight of tocopherol is about 340, so the hydrophilic group is very low in chemical structure, and HLB (hydrophilic lipophilic balance) value of general tocopherol is 0.7 ~ 0.8, which is a strong nonpolar substance (wherein HLB value of surfactant is hydrophilic-hydrophobic balance, And the size and length balance of the hydrophilic (polar) group and the hydrophobic group (nonpolar) of the surfactant).

Therefore, a suitable emulsification model for preparing fat-soluble tocopherols into water-soluble emulsions was O / O / W / W type. Specifically, in the embodiment of the present invention, as a hydrophobic surfactant, polyglycerol polyricinoleate [HLB value: 1.2], glycerin monostearate [HLB value: 4.1], glycerin monooleate [HLB value: 4.1] is applied. As the hydrophilic surfactant, polyglycerol monostearate [HLB value: 15.0], polyglycerol monooleate [HLB value: 15.0], polyoxyethylene (20) sorbitan monooleate [HLB value: 16.0], poly Oxyethylene (20) sorbitan monolaurate [HLB value: 16.0] was applied.

As the aqueous phase solvent, sugar alcohols having excellent emulsification stability as compared with general aqueous phase emulsification are preferable, but are not limited thereto. The sugar alcohol includes glycerin, sorbitol, propylene glycol, ethylene glycol, and the like. In the embodiment of the present invention, glycerin was applied.

On the other hand, in the case of water-based emulsions, regardless of hydrophobic and hydrophilic surfactants, all of the emulsion stability was 40 dyne / cm or less, but the D-phase emulsions using glycerin had a much higher emulsion stability than water.

In addition, the emulsion having the highest stability among the 20-40% tocopherol glycerin emulsion prepared in the present invention had the highest emulsification stability when the polyglycerol polyrisinate was applied as a hydrophobic surfactant, and polyglycerol monostea as hydrophilic surfactant. Rate> polyglycerin monooleate> polyoxyethylene (20) sorbitan monooleate> polyoxyethylene (20) sorbitan monolaurate.

As described above, the present invention provides a tocopherol in a form that can be easily consumed as a method for increasing the availability of tocopherol, which has nutritional activity as a variety of physiological functions and vitamins.

According to the method of the present invention, tocopherol, which is hardly soluble in water, may be easily added to water-soluble foods or drinks by using hydrophobic and hydrophilic surfactants, and thus may be usefully used for the prevention of heart disease and aging. In addition, it is possible to apply such as application to cosmetics and livestock feed.

On the other hand, the tocopherol emulsion prepared by the method of the present invention can be freeze-dried to be conveniently used for the production of various products.

       Hereinafter, the present invention will be described in detail by the following examples. The following examples merely illustrate the invention and are not intended to limit the scope thereof. Unless stated otherwise, the units are% by weight.

Example 1 Preparation of Water Dispersible Tocopherol Emulsion

As hydrophobic surfactants, polyglycerol polylysinolate (a), glycerin monooleate (b) and glycerin monostearate (c) are used as hydrophilic surfactants, polyglycerol monostearate (d) and polyglycerol monooleate. (e), polyoxyethylene (20) sorbitan monooleate (g) and polyoxyethylene (20) sorbitan monolaurate (f) were used, and glycerin (h) or water (i) was used as an aqueous solvent. The water-soluble emulsion containing 20%, 30% and 40% of the tocopherol content was prepared by the application.

Table 1, Table 2 and Table 3 below are a table summarizing the composition of the emulsion containing 20%, 30% and 40% tocopherol, respectively.

Example 2 Measurement of Surface Tension of Tocopherol Emulsion

The affinity to the aqueous phase was tested by measuring the surface tension of each tocopherol emulsion prepared in Example 1.

Specifically, the surface tension of the tocopherol emulsion of the example prepared to contain 20 to 40% tocopherol content was measured by using a surface tension meter after changing each emulsion to a 10% aqueous phase. The platinum-iridium ring used was used a 6cm ring.

As shown in FIG. 1, the surface tension of the 20-40% water soluble tocopherol emulsion was evaluated, and a value of 33-46 dyne / cm was shown. When the surface tension of the emulsion is 40 ~ 46 dyne / cm there is an emulsion stability, when the surface tension is 40 dyne / cm or less was confirmed that the emulsion stability is lowered.

In the case of water-based emulsions, regardless of hydrophobic and hydrophilic surfactants, the emulsion stability was less than 40 dyne / cm. However, D-phase emulsions using glycerin had much higher emulsion stability than water. Here, the D-phase emulsification, when the oil in water (O / W) emulsion is prepared, by lowering the interfacial tension of the emulsion by using a sugar alcohol instead of water in the aqueous solvent to remove the cause of the oil is broken to separate the oil It is applied to exp-12 to exp-1 of Tables 1-3 as an emulsification method to increase the emulsion stability.

Judging from the above experimental results, the most stable emulsion among 20-40% tocopherol glycerin emulsion was the highest in the case of applying polyglycerin polyricinoleate as hydrophobic surfactant, polyglycerol mono as a hydrophilic surfactant Stearate> Polyglycerin Monooleate> Polyoxyethylene (20) sorbitan monooleate> polyoxyethylene (20) sorbitan monolaurate.

Example 3: Storage Stability Test of Tocopherol Emulsion

Storage stability experiment of the emulsion prepared in Example 1 was measured by converting the emulsion phase (oil phase and water phase separation) in accordance with the following equation while diluting each emulsion in a 10% aqueous solution. The storage conditions at this time were divided into cycles and analyzed. One cycle was maintained at 5 ° C for 24 hours and then experimented at 20 ° C for 24 hours.

Storage stability (%) = (oil height-separated oil height) / (oil height) × 100

3-1: Determination of Storage Stability of 20% Tocopherol Emulsion

The 20% tocopherol glycerin emulsion prepared in Example 1 was prepared as a 10% aqueous solution, and the results of evaluating the emulsion stability while storing and storing at 1 cycle (24 hours at 20 ° C. and 24 hours at 20 ° C.) are shown in FIG. 2. . Looking at the emulsifying efficacy of the hydrophobic surfactant, polyglycerin polyricinolate> glycerin monostearate glycerin monooleate was found in order, the hydrophilic surfactant emulsification polyglycerol monostearate> polyglycerol monooleate> polyoxy Ethylene (20) sorbitan monolaurate ≧ polyoxyethylene (20) sorbitan monooleate.

In the case of the emulsifier to which polyglycerol polyricinoleate was applied, oil separation was confirmed when polyoxyethylene (20) sorbitan monolaurate was used as a hydrophilic surfactant in 2 cycles, and polyglycerol monostearate and polyglycerol monool In emulsions using latex, polyoxyethylene (20) sorbitan monooleate, oil separation occurred from 3 cycles.

In the emulsion with glycerin monooleate, oil separation was observed in polyoxyethylene (20) sorbitan monolaurate and polyoxyethylene (20) sorbitan monooleate in 1 cycle, and polyglycerol monooleate was used in 2 cycle. , Polyglycerol monostearate was able to confirm the oil separation phenomenon in three cycles.

The same results were obtained for the emulsions to which glycerin monostearate was applied. The difference was the emulsions to which polyoxyethylene (20) sorbitan monolaurate and polyoxyethylene (20) sorbitan monooleate were applied. At the same time, it was confirmed that the emulsion stability decreased sharply with oil separation.

From the above results, it was found that when the 20% tocopherol glycerin emulsion was prepared, polyglycerin polyrisinate as a hydrophobic surfactant and polyglycerol monostearate or polyglycerol monooleate as a hydrophilic surfactant were relatively emulsified. .

On the other hand, in the 20% tocopherol water-soluble emulsion, the emulsion stability was very poor and the measurement of the emulsification capacity was impossible.

3-2: Determination of Storage Stability of 30% Tocopherol Emulsion

The 30% tocopherol glycerin emulsion prepared in Example 1 was prepared as a 10% aqueous solution, and stored at 1 cycle (24 hours at 20 ° C. after 24 hours at 5 ° C.). . Emulsification stability results of 30% tocopherol glycerin emulsions showed a similar tendency to 20% tocopherol glycerin emulsions.

In the emulsion using polyglycerin polylysinolate, oil separation was observed in a product using polyoxyethylene (20) sorbitan monolaurate as a hydrophilic surfactant in 2 cycles, and polyglycerol monostearate and polyglycerol monooleate Oil separation was not observed even after 4 cycles, and polyoxyethylene (20) sorbitan monooleate was found to be oil separation in 3 cycles, but the rate was very slow.

In the emulsion using glycerin monooleate as a hydrophobic surfactant, oil separation was observed between polyoxyethylene (20) sorbitan monolaurate and polyoxyethylene (20) sorbitan monooleate in one cycle, and polyoxyethylene (20 ) Sorbitan monooleate could not measure the emulsion stability from 1 cycle. Polyglycerol monooleate was slightly separated in 2 cycles, but polyglycerol monostearate did not show oil separation after 4 cycles.

In the emulsion with glycerin monostearate, the same result as the emulsion with glycerin monooleate was obtained. The difference was the emulsion with polyoxyethylene (20) sorbitan monolaurate and polyoxyethylene (20) sorbitan monooleate. Emulsification stability was higher than when the glycerin monooleate was applied.

From the above results, it was confirmed that 30% of tocopherol glycerin emulsification was emulsified when polyglycerin polyrisinate was used as a hydrophobic surfactant and polyglycerol monostearate or polyglycerol monooleate was used as a hydrophilic surfactant. . In addition, when the hydrophobic surfactant was used glycerin monooleate or glycerin monostearate and the hydrophilic surfactant polyglycerine monostearate was found to have an emulsion stability.

On the other hand, in the 30% tocopherol water-soluble emulsion, as in 20% tocopherol water-soluble emulsion, the emulsion stability was very poor, it was found that the measurement of the emulsification capacity is impossible.

3-3: Storage Stability Measurement of 40% Tocopherol Emulsion

The 40% tocopherol glycerin emulsion prepared in Example 1 was prepared as a 10% aqueous solution, and the results of evaluating the emulsion stability while storing and storing at 1 cycle (24 hours at 20 ° C. and 24 hours at 20 ° C.) are as shown in FIG. 4. . 40% tocopherol glycerin emulsion showed the same tendency as 20% and 30% tocopherol glycerin emulsion.

When polyglycerin polyricinoleate was applied as a hydrophobic surfactant, oil separation occurred in the product using polyoxyethylene (20) sorbitan monolaurate as a hydrophilic surfactant in 2 cycles. Tan monooleate was identified as oil separation in 4 cycles. However, no oil separation was observed after 4 cycles of polyglycerol monostearate and polyglycerol monooleate.

In the emulsion using glycerin monooleate, oil separation was confirmed in polyoxyethylene (20) sorbitan monolaurate and polyoxyethylene (20) sorbitan monooleate in one cycle, and polyoxyethylene (20) sorbitan mono Olate could not measure the emulsion stability from 1 cycle. When polyglycerol monooleate was added, emulsion stability began to decrease from 2 cycles. However, polyglycerol monostearate was found to have emulsion stability because no oil separation occurred after 4 cycles. When glycerin monostearate was used as a hydrophobic surfactant, the same result was obtained as for the emulsion to which glycerin monooleate was applied.

As a result, 40% of tocopherol glycerin emulsion was prepared by using polyglycerol polylysinate as hydrophobic surfactant and polyglycerin monostearate or polyglycerol monooleate as hydrophilic surfactant, as in 30% tocopherol glycerin emulsion. It was confirmed that the emulsion had stability. In addition, when the hydrophobic surfactant was used glycerin monooleate or glycerin monostearate and the hydrophilic surfactant polyglycerine monostearate was found to have an emulsion stability.

In 40% tocopherol water-soluble emulsions, as in 20% and 30% tocopherol water-soluble emulsions, the emulsion stability was so poor that it was impossible to measure the emulsification capacity.

Judging from the experimental results, the most stable emulsion of 20-40% tocopherol glycerin emulsion was the case of applying polyglycerol polylysinolate as a hydrophobic surfactant, polyglycerol monostearate> polyglycerol mono in hydrophilic surfactant Oleate> polyoxyethylene (20) sorbitan monooleate> polyoxyethylene (20) sorbitan monolaurate in order of emulsion stability.

While the embodiments of the present invention have been described with reference to the accompanying tables, the present invention is not limited to the above embodiments but can be embodied in various forms, and a person of ordinary skill in the art to which the present invention belongs It is to be understood that the invention may be embodied in other specific forms without changing the technical spirit or essential features. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive.

As described above, the method for preparing the water-dispersible tocopherol emulsion of the present invention can be easily applied to food, feed, cosmetics, etc. by effectively oxidizing tocopherol by using a mixed surfactant system including hydrophobic and hydrophilic surfactants. .

Claims (10)

A method for producing a water dispersible tocopherol emulsion by mixing 0.1 to 5% by weight hydrophobic surfactant, 0.1 to 5% by weight hydrophilic surfactant, 50 to 80% by weight aqueous solvent and the remaining amount of tocopherol. delete The method of claim 1, wherein the hydrophobic surfactant is used at least one selected from the group consisting of polyglycerol polylysinolate, glycerin monostearate and glycerin monooleate. The group of claim 1, wherein the hydrophilic surfactant comprises polyglycerol monostearate, polyglycerol monooleate, polyoxyethylene (20) sorbitan monooleate, and polyoxyethylene (20) sorbitan monolaurate. Using at least one selected from. The method according to claim 1, wherein sugar alcohol is used as the aqueous solvent. The method according to claim 5, wherein the sugar alcohol uses at least one selected from the group consisting of glycerin, sorbitol, propylene glycol and ethylene glycol. A water dispersible tocopherol emulsion prepared by the method of claim 1. A food comprising the water dispersible tocopherol emulsion of claim 7. delete delete

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