JP3752767B2 - High oil content oil-in-water emulsified composition and method for producing the same - Google Patents

Description

【００３５】
【表２】

【００３６】
【発明の効果】
従来の水中油型乳化組成物では困難とされていた油性成分が９０重量％以上の高含油条件下での安定性が得られると共に、食品添加物として広く使用されている界面活性剤のみで、使用量も対水相０．５〜４０重量％と、極少量でも油性成分を安定に配合できるため、安全性や機械的な側面でも実用性の高いものであると言える。
また、工業分野では、特に、クレンジングクリーム、マッサージクリーム、エモリエントクリーム、ヘアクリーム等のクリーム乳液類の他、食品、医薬品等の製品に使用することができ、クリーム乳液類に応用した場合、連続相が水性成分であるため、油性成分を多量に配合していても皮膚に適用した際のべたつき感がなく、適用後のしっとり感が得られる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a highly oil-containing oil-in-water emulsion composition and a method for producing the same. Specifically, the present invention relates to a highly oil-in-water-in-water emulsion composition having a ratio of oily components of 90% by weight or more and a method for producing the same.
The composition of the present invention is used for pharmaceuticals, cosmetics, foods and the like.
[0002]
[Prior art]
High oil-containing oil-in-water emulsified systems with a large amount of oil components are applied to creams in the pharmaceutical and cosmetic fields, mayonnaise-like foods in the food field, and the like. Among them, a high oil content system in which the weight ratio of the oil component exceeds 90% is generally difficult to emulsify and disperse, but the polyoxyethylene interface is said to have a strong emulsifying power among nonionic active agents. It is known that an active agent easily emulsifies and disperses more than 90% of oily components (H. Kunieda et al., Colloid and Surfaces, 47, 35 (1990), Kajitani et al., Oil Chemistry, 35, 102 (1986)).
[0003]
However, since polyoxyethylene surfactants have high monodisperse solubility in oil components, in order to obtain a stable oil-in-water emulsion composition having a high proportion of oil components, The blending amount is at least 20% by weight based on the total amount of the active agent and the aqueous component. Furthermore, polyoxyethylene surfactants have a problem in safety because the polyoxyethylene chain decomposes over time to produce formalin, and cannot be applied to foods, etc. When applied to creams and the like, there is a problem that the obtained emulsion composition is highly irritating to the skin.
[0004]
[Problems to be solved by the invention]
An object of the present invention is a highly oil-containing oil-in-water solution that can be used in the fields of medicine, cosmetics and foods, stably emulsify and disperse a large amount of oily components with a small amount of an active agent, and has high safety and no irritation to the skin. It is in providing a type | mold emulsion composition.
[0005]
[Means for Solving the Problems]
As a result of earnest research to obtain an emulsion excellent in emulsion stability even with a small amount of an active ingredient component in an oil-in-water emulsion composition, the present inventors have used a specific sucrose fatty acid ester as an emulsifier, thereby increasing the oil content. The inventors have found that an oil-in-water emulsion composition can be obtained, and have completed the present invention.
[0006]
That is, the present invention provides an emulsion composition comprising (a) a sucrose fatty acid ester, (b) water, and (c) an oil component as essential components. (1) (a) component, (b) component, and (c) (C) Component is 90% by weight or more with respect to the total amount of components, (2) At least 20% by weight of the constituent fatty acids of component (a) is a saturated fatty acid having 8 to 16 carbon atoms or 16 to 22 carbon atoms. A highly oil-containing oil-in-water emulsion composition, (a) component, (b) component, and (c), wherein the monoester in component (a) is 60% by weight or more High oil content, characterized in that 0.01 to 10% by volume of a solid insoluble in the mixture is added to a mixture system containing components and the solid is removed after emulsification with stirring. It exists in the manufacturing method of an oil-in-water type emulsion composition.
Hereinafter, the composition of the present invention and the production method thereof will be described in detail.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
1. High oil content oil-in-water emulsion composition (sucrose fatty acid ester)
In the sucrose fatty acid ester used in the present invention, 20% by weight or more, preferably 30% by weight or more of the constituent fatty acid is a saturated fatty acid having 8 to 16 carbon atoms or an unsaturated fatty acid having 16 to 22 carbon atoms.
[0008]
Specific examples of sucrose fatty acid esters of saturated fatty acids having 8 to 16 carbon atoms and unsaturated fatty acids having 16 to 22 carbon atoms include sucrose caprylate, sucrose caprate, sucrose laurate, and sucrose myristine. Acid ester, sucrose palmitate, sucrose palmitoleate, sucrose oleate, sucrose linoleate, sucrose linolenate, sucrose eicosatrienoate, sucrose arachidonic ester, sucrose elca Examples thereof include acid esters and sucrose docosahexaenoic acid esters, and one or more of these can be used. Among them, sucrose laurate or sucrose oleate is preferable.
The other constituent fatty acids are saturated fatty acids other than those having 8 to 16 carbon atoms or unsaturated fatty acids other than those having 16 to 22 carbon atoms, and are not particularly limited. Specific examples of the sucrose fatty acid ester comprising the constituent fatty acid include sucrose stearate ester, sucrose arachidate ester, and sucrose behenate ester.
[0009]
The proportion of monoester in the sucrose fatty acid ester is 60% by weight or more, preferably 65% by weight or more, more preferably 70% by weight or more.
When the weight ratio of the monoester is reduced, the sucrose fatty acid ester is more likely to form a lamellar liquid crystal in an aqueous solution. In this emulsification system, the formation of lamellar liquid crystals is considered to make it difficult to emulsify a large amount of oily components.
[0010]
Sucrose fatty acid esters are sucrose containing a hydroxyl group having a high oleophobic hydrophilic group, and have a low monodisperse dissolution concentration in oily components compared to polyoxyethylene nonionic surfactants. Even when a large amount of oily component is added, the active agent component acting at the oil / water interface is not dissolved in a large amount in the oily component, and the active component amount of the active agent is not lost. Thus, a stable oil-in-water emulsion having a high oil component content can be obtained with a smaller amount of active agent.
[0011]
(water)
The water used in the present invention is not particularly limited, but it is usually preferable to use demineralized water.
(Oil component)
The oil component used in the present invention is not particularly limited, but hydrocarbons such as n-heptane, n-octane, n-decane, cyclohexane, hexadecane, squalene, squalane, liquid paraffin, ethers such as diheptyl ether, ethylene Diethers such as glycol dibutyl ether, long-chain amino alcohols such as sphingosine, long-chain aldehydes, long-chain ketones, terpenoids, steroids, carotenoids, waxes, acylglycerols, ether glycerides, ceramides, phospholipids, glycolipids, phosphoglycolipids, Examples thereof include sulfated lipids, amino acid lipids, etc., and mixtures of petrolatum, fish oil, olive oil, soybean oil, 2-ethylhexanoic acid triglyceride and the like, and natural oils and fats, mineral oils and the like can be used.
[0012]
In the present invention, particularly for hydrocarbons such as n-octane, n-decane, hexadecane, squalene, squalane, liquid paraffin, and oils such as 2-ethylhexanoic acid triglyceride and olive oil, which are used in cosmetics and foods. A stable highly oil-in-water emulsion composition can be formed.
[0013]
(composition)
The proportion of component (c) in the highly oil-in-water oil-in-water emulsion composition of the present invention is 90% by weight or more, preferably 93% by weight based on the total amount of component (a), component (b) and component (c). % Or more, more preferably 95 to 99% by weight.
The proportion of the total amount of the remaining component (a) and component (b) is 10% by weight or less, preferably 7% by weight, based on the total amount of component (a), component (b) and component (c). Hereinafter, it is more preferably 1 to 5% by weight. The combination of the component (a) and the component (b) is selected in a wide range, for example, the ratio of (a) to the total amount of (a) and (b) is in the range of 0.5 to 40% by weight. It is possible to obtain a stable composition even when the concentration of the active agent is 0.5 to 10% by weight.
[0014]
The emulsified composition of the present invention is capable of stably emulsifying a large amount of oily components with a much smaller amount of a surfactant than the conventional highly oil-containing oil-in-water emulsification system, and has extremely high safety. It can be said that. And since a continuous phase is an aqueous phase, when it applies to skin etc., the unpleasant feelings, such as stickiness by an oil-based component, can be reduced, and the refreshing feel can be given.
[0015]
(Additive ingredients)
About the highly oil-containing oil-in-water type emulsion composition of this invention, you may add salts, an amphiphilic substance, etc. as needed other than sucrose fatty acid ester, water, and an oil-based component. In the aqueous phase, monohydric alcohols having 1 to 3 carbon atoms, sugars such as glucose and oligosaccharides, linear polyols such as glycerol, sorbitol and ethylene glycol, sugar alcohols such as maltitol and reducing oligosaccharides, proteins, peptides, Amino acids, mucopolysaccharides such as chondroitin sulfate and hyaluronic acid, and glycosides such as saponins may be added as necessary.
[0016]
Moreover, a fragrance | flavor, a pigment | dye, an antiseptic | preservative, a chemical | medical agent, a thickener, a chelating agent etc. are suitably added to the product to which the highly oil-containing oil-in-water emulsion composition of this invention was applied.
Specifically, the protein includes milk casein, sodium caseinate, soy protein, ovalbumin, serum albumin, milk globulin, gelatin, collagen, glutelin, and the like, and the dye includes β-carotene, anato dye, turmeric dye, and publica dye. , Safrole yellow, riboflavin, lac pigment, curcumin, chlorophyll, etc. As flavoring amounts, cinnamon oil, pepper oil, peppermint oil, peppermint oil, lemongrass oil, spare mint oil, ginger oil, parsley oil, celery oil, carrot Oils, etc., as preservatives, dihydroacetic acid, benzoic acid, salicylic acid, thimerosal, benzalkonium chloride, phenylmercuric nitrate, benzyl alcohol, etc., as drugs, indomethacin, adriamycin, etc., as thickeners, gum arabic, tragacanth Beam, xanthan gum and the like, as the chelating agent, ethylenediaminetetraacetic acid, nitrilotriacetic acid, ethylene glycol bis (2-aminoethyl ether) tetraacetic acid, and the like.
[0017]
2. Method for Producing Composition The emulsified composition of the present invention can be easily obtained by vigorously stirring a predetermined amount of a mixture of the three components (a), (b) and (c). At this time, the component (a) must be completely dissolved in the system, and those solid at room temperature are heated as necessary, or mixed after being dissolved in the component (b). However, an emulsion is a so-called metastable composition, and the success or failure of production is often influenced by the production method. Such a highly oil-containing oil-in-water emulsion composition can be obtained more easily by a method in which a small amount of insoluble solid material is added to the ternary mixture system of (a), (b), and (c) and stirred.
[0018]
The insoluble solid material used in the present invention is a solid material having a fine structure and a large surface area that does not chemically interact with the mixed system of the components (a), (b), and (c). Includes small spherical or fibrous glass, cotton and the like. The size and shape of the solid material is not particularly limited as long as it is easy to remove by filtration or the like and does not interfere with stirring. For example, in the case of a small sphere, the diameter is in the range of about 0.1 to 10 mm. Things are easy and easy to handle. The addition amount of the solid is 0.01 to 10% by volume with respect to the total amount of the components (a), (b) and (c), and a more appropriate amount can be arbitrarily selected within the range. it can. These solid materials can be easily removed from the emulsified composition by filtration or centrifugation after emulsification.
[0019]
By the above method, for example, a target stable emulsion composition can be obtained more easily than when the entire system is uniformly vigorously stirred at once by applying a considerably large mechanical shearing force to the entire system.
In the case of agitation, hand shaking may be used if the amount is small, and in the case of a large amount, it is not necessary to use a special emulsifier, and it can be easily prepared if a simple agitator is used. The agitator may be, for example, a motor-driven shaft agitator having a short rotating blade, a magnetic stirrer, or the like.
[0020]
For example, using a magnetic stirrer, 1000 to 2000 r. p. m. Even if a stable emulsified composition cannot be obtained by stirring at, a stable emulsion composition can be easily obtained at the same stirring speed if an insoluble solid material is added.
Further, the emulsified composition of the present invention can be obtained by stirring using a stirring blade or stirring tank having a fine structure and a large surface area instead of using an insoluble solid material. For example, a stirring blade having a mesh-like void, a stirring blade having a large number of fine protrusions on the surface, a stirring vessel having a baffle plate having a void in the mesh shape, a stirring vessel having a large number of baffle plates, etc. These may be used in combination.
When obtaining a highly oil-in-water emulsified composition, particularly a composition in which the oily component exceeds 90% by weight, a composition in which the oily component is about 90% by weight of the total amount is used first, rather than measuring and emulsifying a desired composition at a time. It is easier to take a method of emulsifying the product and gradually adding the oil component to a predetermined amount thereafter.
[0021]
As described above, according to the present method, an easily and more stable system can be obtained regardless of the mechanical shearing force, and at the same time, labor saving of the manufacturing process can be achieved.
The highly oil-in-water-in-water emulsion composition obtained as described above can be used for products such as foods, cosmetics, and pharmaceuticals. Specifically, as food, dressing, coffee whitener, mayonnaise, margarine, etc., as cosmetics, emollient cream, massage cream, cleansing cream, makeup cream, base cream, pre-makeup cream, etc., as pharmaceuticals, oil-soluble It can be used for cream preparations in which drugs are dissolved.
[0022]
【Example】
EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples unless it exceeds the gist.
Confirmation that the emulsification system is an oil-in-water type is made by microscopic observation (volume ratio of oil / water phase, Beckline method (H. Kunieda et al., Colloids and Surfaces, 24, 225 (1987))). And a diffusion test of the composition in water.
Moreover, the compounding quantity ratio of each component used by the Example and the comparative example is as showing in Table 1, and the constituent fatty acid composition and monoester fraction of each active agent are as shown in Table 2.
[0023]
Example 1
A solution in which sucrose lauric acid monoester (SM-1200, Mitsubishi Chemical Foods Co., Ltd.) is uniformly dissolved in distilled water and n-decane (special grade, Tokyo Chemical Industry Co., Ltd.) are weighed into a screw test tube, Absorbent cotton (Japanese Pharmacopoeia absorbent cotton: Toei Co., Ltd.) was added in an amount of 0.5% by volume and emulsified by shaking at 25 ° C., and the absorbent cotton was taken out to obtain an oil-in-water emulsion composition.
The prepared oil-in-water emulsion composition was stable without separation at 25 ° C. for 6 months, and stable even at 40 ° C. for 4 weeks.
[0024]
Example 2
A solution in which sucrose lauric acid monoester (SM-1200, Mitsubishi Chemical Foods Co., Ltd.) is uniformly dissolved in distilled water, and n-decane (special grade, Tokyo Kasei Kogyo Co., Ltd.) as an oil component are used as screw bottles. After adding 0.03% by volume of glass wool (Quality Glass Wools Grade A Toshiba Ceramics Co., Ltd.), the mixture was stirred and emulsified at 1500 ° C. with a magnetic stirrer at 25 ° C. to obtain an oil-in-water emulsion composition. .
The prepared oil-in-water emulsion composition was stable without separation at 25 ° C. for 6 months.
[0025]
Example 3
An oil-in-water emulsion composition was obtained in the same manner as in Example 1 except that n-hexadecane (special grade, Tokyo Chemical Industry Co., Ltd.) was used and the formulation shown in Table 1 was used.
The prepared oil-in-water emulsion composition was stable without separation at 25 ° C. for 6 months.
[0026]
Examples 4 and 5
An oil-in-water emulsion composition was obtained in the same manner as in Example 2 except that squalane (special grade, Tokyo Chemical Industry Co., Ltd.) was used and the composition shown in Table 1 was used.
The prepared oil-in-water emulsion composition was stable without separation for 1 month at 25 ° C. The composition of Example 5 was stable without separation for 4 weeks even at 40 ° C.
[0027]
Example 6
An oil-in-water emulsion composition was obtained in the same manner as in Example 1 except that sucrose palmitic acid monoester was used and the formulation shown in Table 1 was used.
The prepared oil-in-water emulsion composition was stable without separation for 1 month at 25 ° C.
[0028]
Example 7
An oil-in-water emulsion composition was obtained in the same manner as in Example 1 except that sucrose oleic acid monoester was used and the formulation shown in Table 1 was used.
The prepared oil-in-water emulsion composition was stable without separation for 1 month at 25 ° C.
[0029]
Example 8
Example 1 was used except that sucrose laurate (L-1695, Mitsubishi Chemical Foods Co., Ltd.) and 2-ethylhexanoic acid triglyceride (TEH, Nisshin Oil Co., Ltd.) were used. Thus, an oil-in-water emulsion composition was obtained.
The prepared oil-in-water emulsion composition was stable without separation for 1 month at 25 ° C.
[0030]
Example 9
An oil-in-water emulsion composition was obtained in the same manner as in Example 1 except that sucrose stearate ester (S-1670, Mitsubishi Chemical Foods Co., Ltd.) was used and the formulation shown in Table 1 was used.
The prepared oil-in-water emulsion composition was stable without separation for 1 month at 25 ° C.
[0031]
Comparative Example 1
Emulsification was carried out in the same manner as in Example 1 except that sucrose monostearate was used and blended as shown in Table 1.
Immediately after the preparation, the oil / water phase was separated, and a stable oil-in-water emulsion composition could not be obtained.
[0032]
Comparative Example 2
Emulsification was carried out in the same manner as in Example 1 except that sucrose stearate (S-1170A, Mitsubishi Chemical Foods, Inc., monoester of about 55% by weight) was prepared as shown in Table 1.
The oil / water phase separated immediately after preparation.
[0033]
Comparative Example 3
Emulsification was carried out in the same manner as in Example 1 except that sucrose stearate ester (S-770, Mitsubishi Chemical Foods, Inc., about 40% by weight monoester) was used and the formulation shown in Table 1 was used.
The oil / water phase separated immediately after preparation.
[0034]
[Table 1]

[0035]
[Table 2]

[0036]
【The invention's effect】
The oily component, which has been considered difficult in conventional oil-in-water emulsion compositions, is stable under a high oil content condition of 90% by weight or more, and only with surfactants widely used as food additives, Since the oil component can be stably blended even when used in an extremely small amount of 0.5 to 40% by weight with respect to the water phase, it can be said that it is highly practical in terms of safety and mechanical aspects.
In the industrial field, in particular, it can be used in products such as cleansing creams, massage creams, emollient creams, hair creams, and other foods such as foods and pharmaceuticals. Since it is an aqueous component, even when a large amount of an oil component is blended, there is no stickiness when applied to the skin, and a moist feeling after application is obtained.

Claims (4)

In the emulsion composition comprising (a) sucrose fatty acid ester, (b) water and (c) oil component as essential components,
(1) The component (c) is 90% by weight or more based on the total amount of the component (a), the component (b) and the component (c).
(2) At least 20% by weight of the constituent fatty acid of component (a) is a saturated fatty acid having 8 to 16 carbon atoms or an unsaturated fatty acid having 16 to 22 carbon atoms, and monoester in component (a) is 60% by weight. That's it,
An oil-in-water emulsified composition having a high oil content. The highly oil-in-water-in-water emulsified composition according to claim 1, wherein at least 20% by weight of the constituent fatty acid of component (a) is lauric acid or oleic acid, and the monoester in component (a) is 60% by weight or more. object. The highly oil-in-water oil-in-water emulsion composition according to claim 1 or 2, wherein the component (a) is 0.5 to 40% by weight relative to the total amount of the component (a) and the component (b). A solid material insoluble in 0.01 to 10% by volume of the mixture based on the total amount of the three components is added to a mixture system containing the component (a), the component (b) and the component (c). The method for producing a highly oil-in-water oil-in-water emulsion composition according to any one of claims 1 to 3, wherein a solid substance is removed.