JPH1118709A - Production of transparent oil-in-water type emulsion composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject composition not losing the sense of transparency at a normal temperature or even by preservation in cold storage, having excellent stability, by making the refractive index of a water phase coincident with that of an oil phase and adjusting the difference in refractive index between the water phase and the oil phase to a specific value or lower than it. SOLUTION: The difference in refractive index between a water phase and an oil phase is roughly preadjusted and both the phases are mixed and emulsified to prepare an emulsion. Then water is removed from an emulsion composition or wafer or a hydrophilic substance is added to the emulsion composition so that the refractive index of the water phase is adjusted, the refractive index of the water phase is made coincident with that of the oil phase at the same temperature in the range of 10-20 deg.C and the difference in refractive index between the water phase and the oil phase is adjusted to <=0.010, preferably <=0.005 to give the objective composition.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for producing a transparent oil-in-water emulsion composition.

[0002]

2. Description of the Related Art Various studies have been made on a method for producing a transparent emulsion composition.
The method described in Japanese Patent Application Laid-Open No. 6-59 or Japanese Patent Application Laid-Open No. Sho 59-15610 is known.

[0003] In any of these methods, the transparency of the emulsified composition is obtained by making the refractive index of the water phase and the refractive index of the oil phase close to each other. However, the method described in JP-A-49-9506 is disclosed. A change in the refractive index due to temperature is not taken into consideration, and there is a problem that the transparency of the emulsion composition changes depending on the storage temperature. On the other hand, the emulsion composition described in JP-A-59-15610 has a problem that, when a liquid emulsion composition is obtained, stability of emulsification over time cannot be obtained.

A method of obtaining a transparent feeling as ultrafine particles having an average particle diameter of emulsified particles of 0.2 μm or less in an emulsified composition is also known. In order to obtain fine emulsified particles, JP-A-4-5
As described in JP-A No. 1853 or JP-A-8-51928, a special device such as emulsification under reduced pressure or a complicated treatment step is required, and the production of a transparent emulsion composition can be easily performed. And it could not be performed stably.

[0005]

SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and to provide a method for easily producing a transparent and oil-in-water emulsion composition having good stability.

[0006]

The present inventors have conducted intensive studies in view of the above points and found that the refractive indices of the water phase and the oil phase were 10 ° C.
At the same temperature in the range of ２０20 ° C.,
In addition, by adjusting the difference between the refractive indices of the aqueous phase and the oil phase to 0.010 or less in the entire temperature range within the range of 5 ° C to 35 ° C, a target transparent oil-in-water emulsion composition is produced. It has been completed based on the knowledge that it can be done.

That is, the present invention provides that the refractive indices of the water phase and the oil phase are matched at the same temperature in the range of 10 ° C. to 20 ° C. Difference between the refractive index of the oil phase and that of the oil phase is 0.010
A method for producing a transparent oil-in-water emulsion composition, characterized by the following adjustment.

In the present invention, the aqueous phase is mainly composed of water. The refractive index of the aqueous phase can be adjusted by adding a substance which is transparently dissolved in the aqueous phase. Any material can be used as the refractive index adjusting material as long as it can be dissolved transparently. For example, in addition to sugars such as glucose, sucrose, starch syrup, sorbitol, etc., acids such as citric acid, phosphoric acid, ascorbic acid, salts such as salt, calcium lactate, and seasonings such as amino acids, etc. , Glycerin, alcohols such as ethanol, and the like.

The oil phase has a solid content measured at 5 ° C. as a preferred oil phase component in the measurement of SFI (solid fat index), which is a method for measuring the solid fat content of fats and oils.
Any oily substance can be used as long as it is 5% or less, and various triglycerides, essential oils, oleoresins, higher fatty acids, higher alcohols, waxes,
Examples include esters and ethers.

In the present invention, it is necessary that the refractive indices of the water phase and the oil phase be the same at any one of the same temperatures within the range of 10 ° C. to 20 ° C. If the respective refractive indices do not match each other within the range of 10 ° C. to 20 ° C., the emulsion composition loses transparency by being stored at room temperature or refrigerated. Further, even if the respective refractive indices are matched in any of the range of 10 ° C. to 20 ° C., the difference between the refractive indices of the two phases is set to 0.1 in the entire temperature range of 5 ° C. to 35 ° C. 010 must be kept below. This is because, depending on the type of the water phase and the oil phase, the refractive index of each may be greatly affected by a change in temperature, and the difference between the refractive indices of the two phases is 0.0
If it exceeds 10, similarly, the emulsion composition may lose its transparency by being stored at room temperature or refrigerated, and may become cloudy during storage throughout the year or during distribution. According to the present invention, the difference between the refractive indices of both phases is 0.005 in the entire temperature range within the range of 5 ° C. to 35 ° C.
It is more preferable to hold the following.

It is customary to adjust the refractive index of both phases before mixing and emulsifying both phases.
In some cases, the refractive index of both phases is roughly adjusted in advance, for example, the difference in the refractive index of both phases is adjusted to about 0.150 or less, and after mixing and emulsifying both phases, water is removed from the emulsion. Alternatively, the desired transparent oil-in-water emulsion composition can be obtained by adjusting the refractive index of the aqueous phase by adding water or a hydrophilic substance to the emulsion. If the difference between the refractive indices of the two phases exceeds 0.150 and has an excessively large difference, it becomes difficult to adjust the refractive index later. Therefore, it is preferably about 0.150 or less.

As a method for adjusting the difference in the refractive index between the oil phase and the aqueous phase at the same temperature, the refractive index of the prepared emulsified composition is measured as the sugar content, and the sugar content does not match the sugar content of the oil phase. Achieved by adjusting to 0.010 or less. In order to match or adjust the sugar content, remove water in the aqueous phase by heating or the like, or increase the concentration of the aqueous phase by adding a solution having a higher sugar content than the aqueous phase before adjustment, or
This is achieved by adding water to the aqueous phase to reduce the concentration of the aqueous phase.

In the present invention, the average particle size after the emulsification treatment is preferably set to 0.4 μm to 5.0 μm, and when the average particle size exceeds 5.0 μm, the prepared emulsified composition Of the emulsified particles during storage indicates a tendency of creaming, aggregation, coalescence and the like and emulsification destruction. On the other hand, higher stability is obtained when the particle size of the emulsified composition is fine, but the average particle size is 0.4
In order to reduce the particle size to less than μm, a special emulsifying device or the like is required as described above, which is complicated. In the oil-in-water emulsion composition of the present invention, the average particle diameter is preferably set to 0.4 μm to 5.0 μm.

As the emulsifier necessary for emulsifying the aqueous phase and the oil phase, any emulsifier can be used as long as it can be transparently dissolved in the aqueous phase or the oil phase, and glycerin fatty acid ester, propylene glycol fatty acid ester, sorbitan fatty acid ester, lecithin Various surfactants, water-soluble soy polysaccharides,
Water-soluble polysaccharides such as gum arabic; water-soluble proteins such as casein and whey protein; These emulsifiers may be used alone or in combination depending on the case.

The oil-in-water emulsion composition obtained in the present invention has very high stability even when stored for a long period of time, and has no change in transparency when the temperature changes in a normal temperature range.

[0016]

EXAMPLES Hereinafter, embodiments of the present invention will be described in detail with reference to examples, but these are examples and do not limit the scope of rights. The parts and percentages in the examples are on a weight basis.

Example 1 A medium-chain fatty acid triglyceride having a SFI measurement value of 5% at 5 ° C. and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%) (trade name: MCT-B, Fuji 10 parts of an oil phase, 5 parts of a water-soluble soybean polysaccharide, and a refractive index of 1.449 at 20 ° C. by sucrose.
Using 90 parts of the solution adjusted to 6 (sugar content of 63.4%) as an aqueous phase, the mixture was emulsified with a high-pressure homogenizer to obtain a transparent oil-in-water emulsion composition having an average particle diameter of 0.8 μm. This emulsified composition had a clarity in the range of 5 ° C. to 35 ° C., and no change was observed in the emulsified state and the clarity even after storage at room temperature for one month.

Comparative Example 1 10 parts of a medium-chain fatty acid triglyceride (same as in Example 1) having an SFI measurement value at 5 ° C. of 0% and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%). The oil phase was used, and 90 parts of a solution containing 5 parts of water-soluble soybean polysaccharide and adjusted to a refractive index of 1.4370 (56.8% sugar content) at 20 ° C. with sucrose was used as the aqueous phase. An oil-in-water emulsion composition was obtained in the same manner as in Example 1. This emulsion composition was cloudy and did not have a transparent feeling.

Comparative Example 2 10 parts of a medium-chain fatty acid triglyceride (same as in Example 1) having an SFI measurement value at 5 ° C. of 0% and a refractive index at 40 ° C. of 1.4417 (sugar content of 59.9%) was used. On the other hand, the oil phase contains 5 parts of a water-soluble soybean polysaccharide and has a refractive index at 40 ° C. of 1.4417 (59.9% sugar content) by sucrose.
Using 90 parts of the prepared solution as the aqueous phase, a transparent oil-in-water emulsion composition was obtained in the same manner as in Example 1. This emulsion composition had a transparent feeling in the range of 30 ° C. or higher, but became turbid when cooled to 20 ° C. Further, after storage at room temperature for one month, the emulsification was kept in a good state, but the transparency was lost.

Comparative Example 3 The SFI measurement value at 5 ° C. was 23.1%,
The oil phase contains 10 parts of hardened rapeseed oil (melting point: 22 ° C.) having a refractive index of 1.4694 (sugar content: 71.6%), while containing 5 parts of water-soluble soybean polysaccharide at 20 ° C. with fructose-glucose liquid sugar. Has a refractive index of 1.4694 (sugar content of 71.6)
%) Was used as the aqueous phase, and emulsification was carried out in the same manner as in Example 1. Immediately after emulsification, the obtained oil-in-water emulsified composition had transparency at 20 ° C., but became turbid when cooled to 5 ° C. In addition, 1 at room temperature
After storage for months, the emulsification remained in a good state, but the transparency was lost.

Example 2 10 parts of a medium-chain fatty acid triglyceride (same as in Example 1) having an SFI measurement value at 5 ° C. of 0% and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%) was used. An oil phase was used, and 90 parts of a solution containing 5 parts of water-soluble soybean polysaccharide and having a refractive index adjusted to 1.4400 (59.3% sugar content) at 20 ° C. with sucrose was used as an aqueous phase. Emulsification was carried out as in Example 1. The obtained oil-in-water emulsion composition was heated to remove water, and the refractive index of the aqueous phase at 20 ° C was adjusted to 1.4496 (63.4% sugar content). The average particle size of this emulsified composition is 0.9 μm,
It had transparency in the range of ° C. In addition, 1 at room temperature
No change was observed in the emulsified state and transparency even after storage for months.

Example 3 10 parts of a medium-chain fatty acid triglyceride (same as in Example 1) having an SFI measurement value at 5 ° C. of 0% and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%). Emulsification was performed in the same manner as in Example 1 except that 20 parts of an aqueous solution containing 1 part of casein was used as an oil phase, as an aqueous phase (refractive index at 20 ° C., 1.3413). The obtained oil-in-water emulsion composition was added to starch syrup having a sugar content of 77% (refractive index at 20 ° C. of 1.4).
830) to give a refractive index of the aqueous phase at 20 ° C. of 1.4.
It was adjusted to 496 (sugar content: 63.4%). The average particle size of this emulsified composition was 1.2 μm, and the emulsion composition was transparent in the range of 5 ° C. to 35 ° C. No change was observed in the emulsified state and the transparency even after storage at room temperature for one month.

Example 4 Medium-chain fatty acid triglyceride having a measured SFI at 5 ° C. of 0% and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%) 9.9 (same as in Example 1) The oil phase (refractive index at 20 ° C. 1.4498) obtained by adding 0.1 part of glycerin fatty acid ester to the
A mixture of 70 parts of fructose-glucose liquid sugar having a sugar content of 75.5% and 0.5 part of sucrose fatty acid ester and 9.5 parts of water was added to the aqueous phase (2).
Emulsification was carried out in the same manner as in Example 1 except that the refractive index at 0 ° C. was 1.4568). Water is added to the obtained oil-in-water emulsion composition, and the refractive index of the aqueous phase at 20 ° C. is 1.449.
Adjusted to 6. The average particle size of this emulsion composition is 0.6μ
m and had a transparent feeling in the range of 5 ° C. to 35 ° C. No change was observed in the emulsified state and the transparency even after storage at room temperature for one month.

Example 5 10 parts of a medium-chain fatty acid triglyceride (same as in Example 1) having an SFI measurement value at 5 ° C. of 0% and a refractive index at 20 ° C. of 1.4496 (having a sugar content of 63.4%) was used. On the other hand, the oil phase contains 5 parts of a water-soluble soybean polysaccharide and has a refractive index at 20 ° C. of 1.4496 (sugar content: 63.4%) by sucrose.
Using 90 parts of the prepared solution as an aqueous phase, a high-speed stirrer was used to obtain a transparent oil-in-water emulsion composition having an average particle size of 5.8 μm. This emulsion composition had a clear feeling in the range of 5 ° C. to 35 ° C., but after storage at room temperature for one month, some creaming of the emulsion was observed, and the stability of the emulsified state over time was determined in Example 1. Was better.

Comparative Example 4 230 parts of fructose were dissolved in 100 parts of water, and 3.3 parts of sucrose fatty acid ester was further added.
The mixture was emulsified with a homomixer while gradually adding 770 parts of cottonseed oil previously heated to 70 ° C. to obtain a transparent oil-in-water emulsion composition (similar to Example 1 described in JP-A-49-9506). Operation of). This emulsion composition had a transparent feeling at 30 ° C. or higher, but became cloudy when stored in a refrigerator.

Comparative Example 5 10 parts of water was added to 5 parts of β-cyclodextrin, and 5 parts of soybean oil was further added and kneaded to obtain a β-cyclodextrin paste. 70 parts of cottonseed oil, 0.2 parts of lecithin and 0.3 parts of sorbitan fatty acid ester are added to this paste and mixed well, and then, while gradually adding 30 parts of sorbitol, mixing and stirring are carried out to obtain a transparent and transparent emulsion composition. A product was obtained (the same operation as in Example 3 described in JP-A-59-15610). This emulsified composition showed a good emulsified state immediately after emulsification, but after storage at room temperature for one month, the emulsification was destroyed, and separation of oil was observed.

[0027]

As described above, according to the present invention, it is possible to easily produce a transparent oil-in-water emulsion composition in which no change in the emulsified state and transparency is observed even after long-term storage at room temperature. Has an effect.

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Junko Tobe 4-3 Kinudai, Taniwahara-mura, Tsukuba-gun, Ibaraki Prefecture Inside Tsukuba Research & Development Center, Fuji Oil Co., Ltd. (72) Inventor Yuichi Maeda Yawahara-mura, Tsukuba-gun, Ibaraki Prefecture 4-3 silk stand Fuji Oil Co., Ltd. Tsukuba Research & Development Center

Claims (6)

[Claims] 1. The method of claim 1, wherein the refractive indices of the water phase and the oil phase are matched at the same temperature in the range of 10 ° C. to 20 ° C. A method for producing a transparent oil-in-water emulsion composition, wherein the difference in the refractive index of the phases is adjusted to 0.010 or less. 2. After roughly adjusting the difference in refractive index between an aqueous phase and an oil phase at the same temperature in advance, mixing and emulsifying both phases to prepare an emulsion, and thereafter removing water from the emulsion composition. The production method according to claim 1, wherein water or a hydrophilic substance is added to the emulsified composition to adjust the refractive index of the aqueous phase. 3. The method according to claim 1, wherein the difference between the refractive index of the aqueous phase and the refractive index of the oil phase is adjusted to 0.005 or less over the entire temperature range of 5 ° C. to 35 ° C. 4. The method according to claim 1, wherein a substance which is transparently dissolved in an aqueous phase or an oil phase is used as the emulsifier. 5. The emulsified particles having an average particle size of 0.4 μm to 5.
The emulsification treatment is performed so as to be within a range of 0 μm.
5. The method according to any one of items 1 to 4. 6. The process according to claim 1, wherein the solid content at 5 ° C. of the oil phase measured by SFI is 5% or less.