KR100991677B1 - Viscous salt containing spices and manufacturing method thereof - Google Patents

Abstract

The present invention uses viscous salt containing spices as a viscous agent, and can add spices and salt to the food at the same time by emulsifying the spice component, easily control the amount of salt intake and stability of the spice component By increasing the absorption rate, it is possible to control the intake amount and provide convenience when ingesting solid salt alone, and at the same time, it can be applied to foods that can take spices together, and viscous salt containing spices and these It provides a method of manufacturing.

Spices, raw polymers, nanoemulsions, viscous salts

Description

Viscosity salt containing spices and its manufacturing method {VISCOUS SALT CONTAINING SPICES AND MANUFACTURING METHOD THEREOF}

The present invention relates to a viscous salt containing a spice and a method for producing the same, and more particularly, to a spice providing a physiologically active function by nanoemulsification using an emulsifier and a water-soluble biopolymer, and then adding salt to the nanoemulsion. By adding viscosity to the salt to increase the stability of the functional ingredient and the availability of the body at the same time, it is to be able to easily control the amount used when cooking using solid salt.

Recently, the use of nanoemulsions in the food and cosmetics industry is actively increasing, especially in the food industry, the reason for the increase is because it provides the following advantages. First, O / W food nanoemulsions have functional properties of various electrical properties such as polarity, nonpolarity, and amphotericity due to their nonpolar (oil), polar (water) and amphoteric (boundary) regions. It can be included in the carrier of. Second, the food nanoemulsion having a heterogeneous structure can be used as a method of controlling the chemical stability of the encapsulated internal component material, by controlling the physical position and emulsion interface of the material having different reactivity. Third, by adjusting the composition and microstructure constituting the food nanoemulsion, it is possible to produce an emulsion with different rheological properties (viscosity liquid, paste, viscoelastic solid), thereby enabling product application suitable for each characteristic. Fourth, the food nanoemulsion is prepared in accordance with the purpose of use as a liquid as well as a solid phase to increase the convenience and usability of transportation. Fifth, food nanoemulsions can produce functional food materials that provide high quality by simple processes (mixing and stirring, high pressure homogenization, ultrasonic wave) using food raw materials (water, oil, surfactants, phospholipids, proteins, polysaccharides, etc.). Can be. Sixth, the food nanoemulsion can prevent the creaming or sedimentation during storage of the product by the nano-level small emulsion particles provide the gravity reduction effect during the Brownian movement, and the nano liquid particles prevent the flocculation of the liquid. Because of this, separation does not occur and maintains dispersion. Finally, nanoemulsion particles do not deform and thus prevent surface agglomeration, so no coalescence occurs, and the thickness of the surfactant film used (diameter of the liquid spheres) significantly reduces thinning or breakage of the liquid membranes in the liquid compartment. To interfere.

Due to these advantages, many researches are being made to prepare food functional ingredients with nanoemulsions to provide food additives or as food additives.As a demand for food carriers, ① food grade approved raw materials and ② economic production processes -Extended shelf life, marketability, superior functionality, increased bioavailability, etc. ③ Protection against chemical decay-Oxidation and hydrolysis, ④ Dosage load and activity maintenance-Maintain and deliver the maximum loading of bioactive components to unit mass of food functional ingredient carrier Carrier up to the final point, ⑤ Delivery mechanism-Active site of the carrier, release control, surrounding environment (pH, ionic strength, enzyme activity, temperature), etc. ⑥ Compatibility with food-appearance, texture, flavor, stability of final product, etc. And ⑦ bioavailability / biological activity.

Experts agree that the range of nanosizes suitable for food nanoemulsions that meet these requirements is suitable for nanomaterials on the order of 100 nm. This is based on research reports that the nano-species remain outside the cell when the size of 300 nm or more, to penetrate into the cell when 70-300 nm, and to the cell nucleus below 70 nm (Chen M. Kikecz A. Formation of nucleoplasmic protein aggregates impairs nuclear function in response to SiO2 nanoparticles.Exper.Cell Res. 305: 51-62 (2005).

The present invention is to provide a viscous salt containing spices that meet the characteristics required as a food functional ingredient carrier, while having the advantages of the nano-emulsion as described above, in particular, the production of food nano-emulsion having a nano-body size of 100nm or less And a method for producing the same.

A spice is a material that is generally used to give taste to foods by physically separating them from fragrant plants. These spices are prepared from plant essential oils extracted and separated from plants containing spices. The most commonly used method of separating plant essential oils is steam distillation. The steam distillation method refers to a method of obtaining fractions having different molecular weights according to boiling point differences while heating and refluxing raw materials containing plant essential oils using water or an organic solvent to a temperature higher than the boiling point of the solvent.

These plant essential oils have a variety of uses and are used for various purposes, including compositions that utilize their antibacterial and antifungal properties, use in pest control agents, and aroma therapy (Wang L., Li X., Zhang G). Dong J. and Eastoe J. (2007) Oil-in-water nonoemulsions for pesticide formations.J. Colloid Interface Sci. 314 (1): 230-235).

Recently, various functional foods have attracted attention, and functional food refers to a group of foods that emphasize biological functions in addition to the nutritional and palatal functions of foods. In general, functional foods are effective for human health, physical exercise ability, mental state and nutrition when ingested. It can be defined as a food group that can fully express the bioregulatory function on the living body, such as disease prevention and treatment. In particular, the essential oil component of the spice has attracted much attention recently. The most widely used spices in Korea are Capsicum annuum (L.), Garlic (Alliul sativum L.), Ginger (Zingiber officinale) and Onion (Allium capa). Scientifically proven (Srinivasan, K. (2005) Spices as influencers of body metabolism: an overview of three decades of research.Food Research International 38: 77-86) Excavation is one of the biggest concerns in the functional food materials industry. Among the essential oils of these spices, capsaicin, allyl sulfide, diallyl sulfide and diallyl disulfide are known to provide effective physiological activity (Srinivasan K. (2005). Spices as influencers of body metabolism: an overview of three decades of research.Food Research International 38: 77-86). Capsaicin contains about 0.5% in the form of capsaicin homologue in red pepper, which is the most widely used spice in Korea, to control the pungent taste. It has energy metabolism, antioxidant activity, blood lipid improvement, immune regulation, anticancer activity, gene expression control. Action, appetite boosting, saliva secretion, intestinal peristalsis, lowering salt intake, vasodilating by Ca ²⁺ , gastric acid secretion, increasing calcium absorption, lowering cholesterol and lowering blood pressure (Surh YJ, Lee RC, Park KK, Mayne ST, Liem A. & Miller JA (1995) Chemoprotective effects of capsaicin and diallyl sulfide against mutagenesis or tumorigenesis by vinyl carbomate and N-nitrosodimethylamine.Carcinogenesis 16: 2467-2471; Yu R., Choi MA, Kawada T., Kim BS, Han IS & Yoo H. (2002) Inhibitory effect of capsaicin against carcinogen-induce d oxidative damage in rats.Journal of Food Science Nutrition 7: 67-71, etc.).

Also, in the late 1940s, it was found that capsaicin was initially a strong stimulus but analgesic over time, and since then, research has been conducted to develop new analgesics by synthesizing capsaicin derivatives. Allylsulfide is a colorless liquid with a pungent odor, insoluble in water, while being mixed with organic solvents such as alcohols or ethers. It is known that diallyl disulfide has an excellent effect on sterilization, antibacterial and blood circulation and prevents adult diseases (Marti＇nez MC, Corzo N., and Villamiel M. (2007) Biological properties of onions and garlic. Food Science & Technology 18: 609-625. Allicin is the main ingredient of garlic's unique odor and medicinal effect.It does not exist in natural garlic, but when garlic is damaged, allin is converted to allicin by an enzyme called allinase. In particular, they are attracting more attention as their role as antioxidants (Marti＇nez MC, Corzo N., & Villamiel M. (2007) Biological properties of onions and garlic. Trends in Food Science & Technology 18: 609-625) .

However, they are not soluble in water, making it easy to prepare a product that is easy to consume, has a strong intestinal irritation effect, has a unique and strong flavor, there is a problem to apply to food in a general way. One way to increase the absorption rate while stabilizing insoluble substances is to make them into emulsions. Emulsion refers to a system in which one liquid becomes fine particles and is dispersed in another liquid. When an emulsion is formed from water and oil, an oil-in-water type (O / W) in which oil is dispersed in water and oil in water is dispersed in oil. It is divided into water (W / O). Emulsions of water and oil are formed by shaking a mixture of water and oil vigorously, which is unstable. There are three main types of instability in emulsions: flocculation, in which particles form agglomerates, and mixtures that remain separated and in which the particles concentrate toward the surface or bottom depending on the relative density of the two systems. creaming and particle coalescing.

Salt is a salty seasoning that contains sodium chloride as the main ingredient. It is also called salt. Salt is present in body fluids and is important for humans and animals because it plays an important role in maintaining osmotic pressure. In addition, it keeps the body fluid alkaline and keeps the acid and alkali parallel to the buffer material. About 3% of seawater is made up of salt, which can be obtained from seawater, but can also be produced artificially. Without salt, many living things on Earth are essential because they cannot survive. However, too much salt in the body can cause high blood pressure, kidney disease, heart disease. However, there are now people who are afraid of excessive salt intake and who go to the hospital because they are in a coma because they do not consume too much salt. In this case, if the salt is chronically insufficient, even though the life is saved, the body changes to maintain a certain range of low levels of sodium ions. Therefore, a treatment for ingesting a large amount of salt for a long time should be performed due to the rapid discharge of salt. . Except in these cases, when you exercise or sweat in hot weather, not only water but also salts are released. The body releases sweat or urine to maintain a certain concentration of sodium ions in the blood. Rather, it can lead to heat stroke or cramps. Therefore, where working in high temperature environments, salt is often used to replenish salt.

Although salt is an indispensable seasoning for living organisms, ingesting too much of it may cause the above-mentioned diseases. Currently, in most homes and restaurants, the salt is added to foods or the salt is added to a solid state when cooking. have. Since the salt is in a solid state, it is not easy to add an appropriate amount, and since an excessive amount may be added, an excess amount may be included in the food, so a method for ingesting an appropriate amount is needed. In addition, since salt and spices are often added at the same time, there is a need to add salt with an appropriate amount of spices.

Emulsifiers are used to stabilize emulsions and most emulsifiers are surfactants. Food emulsions can generally be prepared by applying mechanical or ultrasonic energy to mixtures of oil, water and emulsifiers. These emulsions are opaque and stable over a period of time, but have thermodynamically unstable characteristics to show long-term stability. It is a well-known fact. Another problem that arises in the preparation of emulsions in the food industry is the limitation of emulsifiers that can be used, that is, many emulsifiers are not allowed for food and some of them are only available at very low concentrations. Moreover, in the case of soybean oil, which is widely used as an emulsifier for preparing emulsions in the food industry, long-chain fatty acid glycerides contained in soybean oil are more difficult to dissolve than short-chain or medium-chain fatty acid glycerides.

Ingredients involved in preparing food nanoemulsions can be broadly classified into surfactants, auxiliary surfactants, fats, and the like. Double surfactants are also referred to as emulsifiers or amphiphiles, and are important for reducing interface tension in nanoemulsion preparations. Play a role. Current licensed uses include glycerin fatty acid esters, sucrose fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters, soybean phospholipids, and calcium stearyl lactate. Phospholipid lecithin is a natural emulsifier. The auxiliary surfactant further serves to reduce the interface tension, thereby increasing the fluidity of the interface and thus increasing the entropy of the emulsion system.

On the other hand, biopolymers such as proteins or polysaccharides can be used to prepare food nanobodies containing bioactive materials, which can promote self-association, agglomeration of single biopolymers, In biopolymer mixture systems, this is possible by inducing phase separation such as manipulation of interaggregation or interaction. Biopolymer-based nanobodies provide a function of a physiologically active delivery system, and thus, widespread use has been attempted to increase the palatability of lipophilic physiologically active substances, body absorption, and stability of physiologically active ingredients. Biopolymers are being used as a material for the production of efficient delivery systems in the food and pharmaceutical fields because they offer advantages such as safety, biocompatibility, and biodegradability. Chitosan, alginic acid, gelatin, etc. It is recognized as this rich material.

In order to use these food functional ingredients as food additives, nano-emulsions using plant essential oils, emulsifiers, and water-soluble biopolymers that can be used as spices can be used to stabilize functional ingredients in foods based on materials suitable for use in foods. Nano to maximize the absorption in the body, reduce the strong intestinal irritation effect and flavor of the functional ingredients in the food, and further increase the stability of the functional ingredients in the food for long-term preservation and easier to apply to other foods It can also provide particles. In particular, it is possible to give viscosity to the salt contained in the nanoemulsion by using the viscosity improvement effect of the raw polymer.

On the other hand, due to the salting-in effect, nanoemulsions containing a certain concentration of electrolytes are known to be highly stable (Eleousa A Makri, Georgios I Doxastakis (2006) .Journal of the Science of Food and Agriculture 86: 1863-1870). Therefore, by adding salt to the food nanoemulsion, it is possible to give higher stability to the nanoemulsion containing spices.

Accordingly, it is an object of the present invention to provide a nanoemulsion which can be used as a viscous salt and a method for preparing the same, based on a substance suitable for use in foods to stabilize the functional ingredients in the food and maximize absorption in the body. .

It is another object of the present invention to provide a nanoparticle comprising a spice that can reduce the strong intestinal irritation effect and flavor of a functional ingredient in a food and can be used as a viscous salt and a method for producing the same.

In order to achieve the above object, the present invention nano-emulsifies the food functional ingredient using an emulsifier and hydrophilic raw polymer and add salt to it to increase the stability and absorption of the food functional ingredient and at the same time stimulate the intestines by the hydrophilic biopolymer. The present invention provides a nanoparticle and a method for preparing the same, which can reduce the effects, further increase stability by solvent precipitation or vacuum freeze-drying, and to be easily applied to other foods in the form of powder from the nanoemulsion. Since the raw polymer improves the viscosity as is known to those skilled in the art, it is possible to make the salt viscous.

Hereinafter, the present invention will be described in detail.

A method for stabilizing functional components that are insoluble in water or increasing absorption efficiency is to prepare nanoemulsions. Nanoemulsions have various advantages over emulsions or microemulsions. While emulsions are opaque and have particle sizes ranging from 0.2 to 50 µm, they are stable for a certain period of time and are thermodynamically unstable, while nanoemulsions are thermodynamically stable compared to common emulsions and exhibit a transparent solution state due to their low light dispersion. The particle size is maintained at the nanometer level. It is also possible to maintain a more stable emulsion state by continuous self-assembly with the hydrophilic or lipophilic portion of the emulsifier.

Since the nanoemulsion has very small particles, gravity acceleration and Brownian motion are significantly reduced, so that no creaming or sedimentation occurs during storage, and no aggregation occurs in the dispersed state. Since the small particles forming the nanoemulsion have a property that the particles themselves are not deformed, the occurrence of coalescence phenomenon is suppressed and thus surface aggregation is also prevented. Nanoemulsion can provide the effect of increasing the availability of the body because the stability of the higher active material than the conventional microemulsion is greater.

Methods of making nanoemulsions are known to those skilled in the art. Such methods include agitation, high pressure homogenization, ultrahigh pressure, ultrasound, and micro-flow. The stirring method can produce nanoemulsion with low energy, and in the high pressure homogenization method, the high pressure fluid generated by the operation of the plunger passes through a small gap in the valve at high speed, which causes cavitation, turbulence and Shear forces break down into nano-sized microparticles, resulting in a completely uniform component of the liquid.

Emulsifiers are used in the preparation of nanoemulsions, but the types of emulsifiers that can be used in foods are limited, so that soybean phospholipid (lecithin), sucrose fatty acid ester, glycerin fatty acid ester, sorbitan fatty acid ester, polyglycerol fatty acid ester, stearyl Calcium lactate, and the like. In the food sector, the use of emulsifiers is often possible only at low concentrations. For example, propylene glycol cannot use more than 1 g per 1 kg of food. In this invention, use of sorbitan fatty acid ester is preferable as an emulsifier.

Sorbitan fatty acid esters are nonionic surfactants, which have different properties and uses depending on the type and number of fatty acids bound to sorbitan and the degree of esterification. Commercially available sorbitan monoesters include lauric acid (Tween 20), palmitic acid (Tween 40), stearic acid (Tween 60) and oleic acid (Tween 80). In the present invention, Tween 60 or Tween 80 is particularly preferable as an emulsifier. In the case of Tween 20 or Tween 40, the chemical structure is more suitable for the preparation of water-in-oil (W / O) emulsions, which is not suitable for the preparation of oil-in-water (O / W) emulsions provided by the present invention, and plant essential oils are water-soluble biopolymers. This is because it does not dissolve well in and easily separates the emulsion.

One of the advantages of the nanoemulsion according to the present invention is not only to increase the stability of food functional ingredients and to increase the absorption efficiency in the body, but also to use raw polymers to maintain the activity of the functional ingredients in foods to the human organs targeted for delivery. By controlling the particle size of the nanoemulsion can be used as a new functional food functional carrier. It is preferable that the biopolymer is water-soluble. By using the water-soluble biopolymer, the absorption of the food functional ingredient in the body can be increased and it is easier to prepare a product which is easy to consume. When water-soluble raw polymers are used, vegetable oils are highly irritating, and the high-molecular weights of the essential oils are gradually released due to the coating, and the masking effect is not applied to the human throat. The intestinal stimulation effect of the functional ingredients can be reduced, and the strong flavor that appears when they are present alone has the advantage of solving the rejection of ingestion. Water-soluble raw polymers that can be used in the present invention include chitosan, alginic acid, cellulose, carrageenan, gelatin, gum arabic, pectin and guar gum, and cellulose is particularly preferred.

In addition, by providing a nanoemulsion containing raw polymer that can improve the viscosity, it is possible to give viscosity to the salt contained in the nanoemulsion, functional properties such as antimicrobial activity, antioxidant, dietary fiber intake provided by the raw polymer itself It is also possible to provide at the same time. In the present invention, the water-soluble raw polymers are based on the weight of the whole nanoemulsion prepared. It is used as a solution of 0.1 to 5.0% by weight, prepared by dissolving water-soluble raw polymers in distilled water. When the water-soluble raw polymers are added at less than 0.1% by weight, not only are they less effective in reducing the intestinal irritation effect, the stronger flavor of the spice essential oils, but also the viscosity of the salts contained in the nanoemulsion is less than 5.0% by weight. When added, the particle size of the emulsion becomes too large to form a nonuniform emulsion in micro units. In preparing a nanoemulsion using water-soluble raw polymer as a base material, three conditions of a water base, an oil base, and an emulsifier must be mixed in a constant ratio to form a nano-sized emulsion. This is the most important factor in the production of nanoemulsion. In the present invention, the water base becomes a water-soluble raw polymer solution and salt, the oil base becomes a plant essential oil, and the emulsifier becomes a sorbitan fatty acid ester.

In the present invention, the blending ratio of plant essential oil and emulsifier is preferably 1: 3 to 1: 5. When the mixing ratio is 1: 1 or 1: 2, secondary particles are formed, an unstable emulsion is formed, and the particle size exceeds 1000 nm, resulting in separation of the oil phase and the water phase. If the blending ratio exceeds 1: 5, the amount of functional ingredient in the plant essential oil for the emulsifier becomes too small. According to the present inventors, a nanoemulsion composed of 0.03 to 0.3% by weight of plant essential oil, 0.09 to 1.5% by weight of emulsifier, and 0.1 to 5.0% by weight of water-soluble raw polymer, 1.0% to 30.0% by weight of salt, and remaining water, It can be seen that it can have the same effect.

Nanoemulsion of the present invention can be prepared in a double layer and a triple layer in addition to a single layer. Bilayer and triple layer nanoemulsions can be prepared by preparing a single layer nanoemulsion and then treating with calcium chloride and adding other water-soluble biopolymers. Treatment with calcium chloride increases the reactivity, making bilayer nanoemulsion easier. The water-soluble biopolymers used in the preparation of the bilayer nanoemulsions preferably have different charges because of the increased efficiency of encapsulation of the bilayer on the single layer. After the bilayer nanoemulsion is prepared, the microsized particles are removed by centrifugation and taking only the supernatant. The triple layer nanoemulsion is prepared by adding another water soluble biopolymer solution after preparing the double layer nanoemulsion. Bilayer and triple layer nanoemulsions can form more stable forms of nanoemulsions compared to single layer nanoemulsions and can increase the utilization of the body by reducing the rate of absorption and degradation of plant functional components.

In order to apply the nanoemulsion of the present invention to food, it is desirable to be stable to heat treatment, since most foods are heat treated for sterilization at the end of the manufacturing process. In addition, it is particularly preferable to be stable in the range of pH 4 to 5 in order to be applied to the beverage product because it is controlled and sold in the appropriate pH range of 4 to 5 of the general beverage product. Nanoemulsion according to the present invention is stable to the heat treatment as shown in the results of the study it can be seen that the stable in the above pH range.

The nanoemulsion of the present invention can be recovered by solvent precipitation such as ethanol or acetone or dried by vacuum freeze-drying method to be prepared as nanoparticles. Nanoparticles in powder form are more stable than nanoemulsions for a long time. It has the advantage of being able to be stored and easier to apply to many foods (Galindo-Rodriguez S., Allemann E., Fessi H., & Doelker E. (2004) Physicochemical parameters associated with nonoparticle formation in the salting-out, emulsification-diffusion and nanoprecipitation methods, Pharmaceutical Research 21: 1428-1439).

The nanoemulsion prepared by the present invention may be added to a beverage and sold. According to the research results of the present inventors, the nanoemulsion prepared by the present invention exhibits a very transparent red light, and when used in a beverage industry, It suggests the possibility of using the product to satisfy satisfaction. It can also be used as a seasoning ingredient and can also be used as a food additive in various confections and foods such as gum, baking or butter. Furthermore, since the nanoparticles of the present invention are prepared from nanoemulsions based on water-soluble raw polymers, they are very easy to dissolve when the nanoparticles are dispersed in water.

The present invention can maximize the stabilization of the functional components and absorption of the body by preparing a plant essential oil having a lot of functional ingredients that provide bioactivity in the functional food in a nanoemulsion based on water-soluble biopolymer with salt By reducing the strong flavor that may occur when functional ingredients, especially essential oils of spices, are present alone, not only can they solve the objection to ingestion, but it is also possible to easily control the amount of salt added and to add salt and spices at the same time. Functional salts that provide a combined effect by providing salt intake and food bioactive functionality are provided. In addition, it is possible to reduce the intestinal irritation effect of spice essential oil by using water-soluble biopolymer as a base material in the preparation of nanoemulsion, and at the same time, it is possible to provide functions such as antimicrobial activity and antioxidant provided by the biopolymer itself. In particular, when the nanoemulsion prepared by the present invention is prepared with nanoparticles, the stability is further increased and it is easy to apply to other foods in the form of powder.

Hereinafter, the present invention will be described in detail by way of examples. However, the examples are provided to illustrate the invention and are not intended to limit the scope of the invention.

Example 1-1 Preparation of Self-Adhesive Viscosity Salt Containing Capsaicin Nanoemulsion

Oleoresin capsicum and Tween 80 were mixed at a ratio of 1: 4 and stirred at 150 rpm for 3 minutes. The mixed solution was added to 100 ml of cellulose solution having different concentrations (2 wt%, 3 wt% and 4 wt%) at a concentration of 1 wt%, and stirred at room temperature for 60 minutes at the above speed. At different concentrations (20% by weight, 25% by weight and 30% by weight) to the prepared nanoemulsion, the salt was slowly added and stirred at the above speed for 1 hour, followed by stabilization at room temperature for 24 hours. The nanoemulsion thus prepared was found to be stable to freezing and thawing. The particle size of the prepared nanoemulsion was confirmed to be 100nm or less as shown in [Table 1].

TABLE 1

number Brine concentration Cellulose concentration Nanoemulsion Particles (nm) 1-1-1 20 wt% 2 wt% 6.65 1-1-2 25% by weight 3 wt% 6.95 1-1-3 30 wt% 4 wt% 9.27

[Example 1-2] Manufacturing method of viscous salt containing capsaicin nanoemulsion-ultrasonic method

A premixed liquid was prepared by mixing oleoresin capsicum and Tween 80 in a ratio of 1: 4 and stirring at 150 rpm for 3 minutes. Water was added to this mixed solution three times the total volume of the mixed solution, followed by stirring, followed by reaction for 1 minute in a 50 ° C. water bath to prepare a mixed solution. This mixed solution was sonicated for 5 minutes using an ultrasonic device (Sonic dismembrator Model 500, Fisher scientific, USA) under conditions of 30% by weight, 30W, 18 ° C. The treated sample was added to 100 ml of cellulose solution having different concentrations (2 wt%, 3 wt% and 4 wt%) prepared in advance, and stirred at room temperature for 1 hour at the above rate at 4 wt%. Stirring at this rate for 1 hour with varying concentrations (20% by weight, 25% by weight and 30% by weight) of brine was slowly added to the prepared nonoemulsion and then stabilized at room temperature for 24 hours. The nanoemulsion thus prepared was found to be stable to freezing and thawing. The particle size of the prepared nanoemulsion was confirmed to be 100nm or less as shown in Table 2.

TABLE 2

number Brine concentration Cellulose concentration Nanoemulsion Particles (nm) 1-2-1 20 wt% 2 wt% 10.4 1-2-2 25% by weight 3 wt% 10.6 1-2-3 30 wt% 4 wt% 11.2

[ Example  2] Capsaicin  Contains nanoemulsion Viscous salt  stability

Stability was measured while varying the salt content and the cellulose content by the method according to Example 1-1 (self-bonding method) as shown in Table 3 below. The nanoemulsion prepared as described above can be seen that the nanoemulsion prepared by the method as shown in the number 2-1 to 2-8 of the table was stable at 50 ℃, and also stable in freezing / thawing. In the experiments of 2-9 to 2-11 containing no cellulose, the stability is greatly reduced. According to the results of Experiment 2-12 according to the present invention, the stability is slightly decreased at a high temperature of 50 ° C., but the stability according to freezing / thawing is the same. This result was confirmed to be the same as the nanoemulsion prepared by the method of Example 1-2 (ultrasonic method).

[Table 3]

number sample Zhejiang 50 ℃ Freeze / Thaw 2-1 20 wt% salt, 1 wt% cellulose Stable, 28 days Stable, 28 days 2-2 20 wt% salt, 2 wt% cellulose Stable, 28 days Stable, 28 days 2-3 20 wt% salt, 3 wt% cellulose Stable, 28 days Stable, 28 days 2-4 20 wt% salt, 4 wt% cellulose Stable, 28 days Stable, 28 days 2-5 25 wt% salt, 3 wt% cellulose Stable, 28 days Stable, 28 days 2-6 25 wt% salt, 4 wt% cellulose Stable, 28 days Stable, 28 days 2-7 30 wt% salt, 3 wt% cellulose Stable, 28 days Stable, 28 days 2-8 30 wt% salt, 4 wt% cellulose Stable, 28 days Stable, 28 days 2-9 20 wt% salt, OC: T = 1: 4, 1 wt% Stable, 28 days Stable, 28 days 2-10 25 wt% salt, OC: T = 1: 4, 1 wt% Stable, 28 days Stable, 28 days 2-11 30 wt% of salt, OC: T = 1: 4, 1 wt% Stable, 28 days Stable, 28 days 2-12 Salt 25 wt%, OC: T = 1: 4, 1 wt% cellulose 5 wt% Stable, 15 days Stable, 28 days

(OC: Oligo Resin Capsicum, T: Tween 80)

Example 3 Particle Size Change of Capsaicin Nanoemulsion in Viscous Salt

Nanoparticles containing 25% by weight of salt, OC: T = 1: 4, 1% by weight and 5% by weight of cellulose were prepared by the method of Example 1-1 to prepare a particle size to size from 3nm to 6㎛ 5 minutes at 25 ℃ using a light-scattering particle size analyzer (Nanotrac TM250, Microtrac Inc. USA) that can measure the results showed that the size immediately after the manufacture was 72.4nm, As a result of thawing, it was confirmed that it was 37.5 nm, and the freezing / thawing confirmed that the particle size was reduced to improve stability.

[Example 4] Raw polymer for preparing viscosine salt containing capsaicin nanoemulsion

Table 4 shows particle sizes of nanoemulsions prepared using various raw polymers by the method of Example 1-1. According to the results of the table, it can be seen that the particle size is 100 nm or less even after preparation, and the longer the storage, the smaller the particle size is, thereby improving stability.

[Table 4]

number Salt concentration (% by weight) Raw Polymer Concentration OC: T Particle size (nm) 28 days storage (nm) One 25 Alginate 0.5 wt% 1: 4 65 42 2 25 Xanthan gum 0.5 wt% 1: 4 76 55 3 25 Guar gum 0.5 wt% 1: 4 46 42 4 25 Chitosan 0.2% by weight 1: 4 84 61 5 25 0.5% by weight of gelatin 1: 4 72 57 6 25 0.5% by weight pectin 1: 4 53 48 7 25 Starch 0.5% by weight 1: 4 102 84 8 25 Carrageenan 0.5% by weight 1: 4 97 49

[ Example  5] Double layer  And Triple layer  Preparation of Nanoemulsions

To prepare the double layer nanoemulsion, 0.4 g of the nanoemulsion prepared in Example 1-1 was added to 100 ml of 0.05 wt% alginate solution (pH 4.9), stirred and mixed at 25 ° C. at 150 rpm for 30 minutes, followed by 18 mM CaCl. ₂ solutions of 7.6 ml were added and stirred and mixed at 150 rpm for 60 minutes. 25 ml of 0.05 wt% chitosan solution (pH 4.6) was added thereto, followed by stirring and mixing at 150 rpm for 2 hours to stabilize the bilayer emulsion. In order to remove the micro-sized emulsion was centrifuged for 40 minutes at 11,000 rpm at 4 ℃ and then only the supernatant was taken. In order to select the concentration of alginic acid and chitosan for the preparation of the triple layer nanoemulsion, the concentration of alginic acid was fixed at 0.05% by weight and the concentration of chitosan was prepared at 0.05-0.09% by weight. 0.05 wt% alginic acid solution and 0.05 wt% chitosan solution were prepared by adjusting the pH to 4.9 and 4.6, respectively. To 0.75 g of a mixture of oleoresin capsicum and Tween80, 117.5 ml of 0.05 wt% alginic acid (pH4.9) was added and stirred at 150 rpm for 30 minutes. Then, 7.5 ml of 18 mM CaCl ₂ solution was added at 150 rpm for 1 hour. Alginate primary emulsions were prepared by slow addition with stirring. 25 mL of 0.05 wt% chitosan (pH4.6) was slowly added to the prepared alginic acid primary emulsion with stirring at 150 rpm for 1 hour 30 minutes. The formed nanoemulsion was filtered through a filter by stirring at 150 rpm for 30 minutes and stabilized at room temperature for 24 hours.

A schematic manufacturing process of the bilayer and triple layer nanoemulsions is shown in FIG. 2.

The efficiency of encapsulation of the chitosan bilayer on the alginic acid monolayers of the bilayer and trilayer nanoemulsions thus prepared was the highest at 68% by weight when prepared with 0.05% by weight chitosan solution at the same concentration as the 0.05% by weight alginic acid solution. As the concentration of increased, the inclusion efficiency decreased (FIG. 3). In the particle size, the micelle structure of the nanoemulsion was increased in the chitosan solution of 0.07% by weight or more (Fig. 4). Therefore, when the hydrophilic biopolymers having different charges were used in the preparation of the double layer nanoemulsion, it was confirmed that stable nanoemulsion was possible using the same concentration.

Example 6 Stability Measurement According to pH

Oleoresin Capsicum and Tween 80 were mixed at a ratio of 1: 4 to 0.2% by weight of chitosan solution at 0.4% by weight, followed by adjusting the pH to 3, 4, 5 and 6. Sean was prepared. The prepared nanoemulsion was measured for particle size and viscosity by the method described above. The particle size of the nanoemulsion increased as the pH was increased from 3 to 6, but after 4 days of storage, the particle size decreased to a similar particle size of 15.45 nm to 22.53 nm. These results were thought to be due to the chemical decomposition of chitosan by low pH. (Figure 5)

[ Example  7] Effect of heat treatment

A nanoemulsion was prepared by mixing oleoresin capsicum and Tween 80 in a ratio of 1: 4 to 0.2% by weight of chitosan solution at an amount of 0.4% by weight, and then preparing a nanoemulsion at 15 ° C, 75 ° C, and 100 ° C. Heat treatment was performed for a minute. The nanoemulsions had a particle size of 66.30 nm, 63.40 nm, and 93.60 nm, respectively, by heat treatment at 50 ° C., 75 ° C., and 100 ° C. (Fig. 8). As a result, it was confirmed that the stability of the nanoemulsion (micelle) structure of the nanoemulsion was slightly deteriorated in the heat treatment of 50 ° C. or higher, but the possibility of forming a nanoemulsion of less than 100 nm and the possibility of using it in food was also suggested. .

1 is an overall flow chart of a method of making a nanoemulsion of the present invention.

Figure 2 illustrates an example of a method for producing a bilayer and triple layer nanoemulsion.

3 is a result of measuring the inclusion efficiency according to the concentration of chitosan solution in the preparation of the double-layer nanoemulsion.

Figure 4 is the result of measuring the change in particle size according to the concentration of chitosan solution in the preparation of the double-layer nanoemulsion.

5 is a result of measuring the change in particle size of the nanoemulsion prepared by the present invention according to pH.

Claims (9)

Nanoemulsion consisting of 0.03 to 0.3% by weight plant essential oil, 0.09 to 1.5% by weight emulsifier, and 0.1 to 5.0% by weight water soluble raw polymer, 1.0% to 30.0% salt and residual amount of water relative to the total nanoemulsion. The method of claim 1, The plant essential oil nanoemulsion, characterized in that at least one selected from the group consisting of pepper essential oil, garlic essential oil, ginger essential oil and onion essential oil. The method of claim 1, The water-soluble biopolymer is a nanoemulsion comprising at least one selected from the group consisting of chitosan, alginic acid, cellulose, carrageenan, gelatin, gum arabic, pectin and guar gum. The method of claim 1, The emulsifier is Tween 60 or Tween 80, characterized in that the nanoemulsion. The method according to any one of claims 1 to 4, Nanoparticles are prepared by solvent precipitation or vacuum freezing and drying the nanoemulsion. Adding 0.03% to 0.3% by weight of plant essential oil and 0.09% to 1.5% by weight of sorbitan fatty acid ester to 0.05% to 1.0% by weight of water-soluble raw polymer; Adding brine; Adding a balance of water to produce a mixture; And Nanoemulsifying the mixture comprising the steps of preparing a single layer nanoemulsion. Adding from 0.03% to 0.3% of plant essential oil and from 0.09% to 1.5% by weight of sorbitan fatty acid ester to 0.05% to 1.0% by weight of one water soluble raw polymer; Adding brine; Adding a balance of water to produce a mixture; Adding calcium chloride to the mixture; Nanoemulsifying the mixture with calcium chloride; Adding 0.05% to 1.0% by weight of other water soluble biopolymer to the nanoemulsion followed by nanoemulsion; And Method for producing a double-layer nanoemulsion comprising the step of separating the emulsion of nanoscale by centrifugation. Adding from 0.03% to 0.3% of plant essential oil and from 0.09% to 1.5% by weight of sorbitan fatty acid ester to 0.05% to 1.0% by weight of one water soluble raw polymer; Adding brine; Adding a balance of water to produce a mixture; Adding calcium chloride to the mixture; Nanoemulsifying the mixture with calcium chloride; Adding 0.05% to 1.0% by weight of other water soluble biopolymer to the nanoemulsion followed by nanoemulsion; Adding another 0.05 wt% to 1.0 wt% of the water-soluble biopolymer solution to the nanoemulsion followed by nanoemulsion; And Method for producing a triple-layer nanoemulsion comprising the step of separating the nano-sized emulsion by centrifugation. 9. The method according to any one of claims 6 to 8, Method of producing a nanoparticles, characterized in that further comprising the step of solvent precipitation or vacuum freeze-drying the nanoemulsion.

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