KR100504379B1 - Microencapsulation of water-soluble isoflavone, production method thereof and application - Google Patents

Abstract

The present invention relates to a microcapsule containing a water-soluble isoflavone, a preparation method and an application thereof.

An object of the present invention is to provide a functional capsule containing a water-soluble isoflavone-containing microcapsules, a preparation method thereof and a water-soluble isoflavone microcapsules as an active ingredient.

The method for producing microcapsules containing water-soluble isoflavones of the present invention

(1) adding water-soluble isoflavones to the coating material solution,

(2) stirring the solution mixed with the coating material and the water-soluble isoflavone and spraying the dispersion in the form of an aqueous solution containing a surfactant;

(3) separating the dispersion sprayed with the coating material and the water-soluble isoflavone into an encapsulated portion and an unencapsulated portion by centrifuging;

(4) spraying and encapsulating the part encapsulated by step (3) of the former in the emulsifier of step (2).

Description

Microcapsules containing water-soluble isoflavones, preparation method and application thereof {Microencapsulation of water-soluble isoflavone, production method approximately and application}

The present invention relates to a microcapsule containing a water-soluble isoflavone, a preparation method and an application thereof.

Isoflavone is a glycoside of phenolic compound, which is a kind of pigment (anthocyanin) contained in plants, and contains about 0.1-0.3mg / g of soybean, and it has anticancer activity against breast cancer and prostate cancer and arteriosclerosis. It has been found to be effective in preventing, preventing osteoporosis, and controlling blood alcohol concentration.

Isoflavones present in natural products include genistein, daidzein, formononetin, biochanin A, genistin, daidzin, and all have weak estrogen activity depending on the degree. Soybeans and soybeans are known to be rich in genistin and daidzin, the glycosides of genistein and daidzein. The anticancer activity of soybeans has recently received a lot of attention, which is believed to be due to isoflavones, protease inhibitors, phytate, dietary fiber, saponins, vegetable sterols, and phenolic substances in soybeans. Among the cancers of breast cancer or prostate cancer, isoflavones are known to be mainly caused by genistein. It has also been reported that genistein interferes with the action of protein kinase and DNA topoisomerase II and weakly binds to estrogen receptors.

Women go through menopause with a rapid physiological change around age 50. The resulting female hormone deficiency increases the risk of developing atherosclerosis, genitourinary diseases, depression, and osteoporosis. In particular, about 30% of women after menopause have been reported to experience at least one osteoporosis fracture.

Menopausal disease, especially osteoporosis, which occurs in most women after menopause, is of great importance for early diagnosis and prevention, and it is necessary to develop long-term osteoporosis prevention and treatment without side effects.

Milk is also called a complete food because it contains all of the nutrients essential to humans, including proteins, lipids, sugars, vitamins and minerals. Milk plays a particularly important role in the growth and development of infancy. In addition, it is classified as an excellent food in terms of balanced distribution of adolescents and adults in the growing season, and is very effective as a source of calcium for the elderly. Korea's milk production started in 1960 and exceeded 1.75 million tons in 1990, and the per capita milk consumption in Korea is continuously increasing to 59.2kg in 2000. In addition, 75% of the whole milk is consumed as market milk, and the consumption rate of processed dairy products such as fermented milk, cheese, and ice cream is lower than that of dairy countries. In recent years, the increase in white milk is weak, but the consumption of ingredient-modified and functional fortified milk is steadily increasing. Therefore, there is an urgent need for technology development and commercialization to diversify functional milk quality.

In order to prevent and cure osteoporosis in postmenopausal women, it is effective to add isoflavones, which are phytoestrogens, without side effects, to calcium-rich milk. It has not been added to milk yet.

The present invention is a functional food containing excellent functional isoflavones by containing microcapsules of water-soluble isoflavones, which contain excellent functionality but have a problem of unique functionalities, which are inconvenient to be consumed directly, and adding them to functional foods such as milk, beverage, and yogurt. Can be provided.

That is, an object of the present invention is to provide a functional capsule containing a water-soluble isoflavone-containing microcapsules, a preparation method thereof and a water-soluble isoflavone microcapsules as an active ingredient.

The present invention includes a functional capsule containing a microcapsule containing a water-soluble isoflavone, a microcapsules containing a water-soluble microflavone as a preparation method and application thereof.

The microcapsules containing the water-soluble isoflavones of the present invention are composed of 10 to 40% by weight of water-soluble isoflavones based on the weight of the microcapsules, and 60 to 90% by weight of the coating material for coating the core material. In the microcapsules of the present invention, if the water-soluble isoflavone is less than 10% by weight, it is not meaningful to microencapsulate the isoflavone. If the isoflavone exceeds 40% by weight, the content of the coating material decreases, so that sufficient coating of isoflavone is achieved. Since it is not made in the present invention, the water-soluble isoflavone preferably contains 10 to 40% by weight based on the weight of the microcapsules.

In the present invention, the coating material of the microcapsules may use an emulsifier, and in the present invention, polyglycerol monostearate (PGMS) or medium-chain triacylglycerol (MCT) may be used as an example of such an emulsifier.

The size of the microcapsules containing the water-soluble isoflavone of the present invention can be adjusted according to the amount of the core material and the coating material, and more preferably, the microcapsules having a size of 2 to 5 μm in diameter are preferable. In the present invention, if the size of the microcapsules is less than 2㎛, the amount of water-soluble isoflavones contained in the capsule is reduced, and if the size of the microcapsules exceeds 5㎛, the functionality of the functional food when the microcapsules are added to the functional food Since the microcapsules containing water-soluble isoflavones in the present invention can be reduced, it is preferable that the microcapsules have a size of 2 to 5 μm in diameter.

The method for producing microcapsules containing water-soluble isoflavones of the present invention

(1) adding water-soluble isoflavones to the coating material solution,

(2) stirring the solution mixed with the coating material and the water-soluble isoflavone and spraying the dispersion in the form of an aqueous solution containing a surfactant;

(3) separating the dispersion sprayed with the coating material and the water-soluble isoflavone into an encapsulated portion and an unencapsulated portion by centrifuging;

(4) The microcapsules containing water-soluble isoflavones can be obtained by spraying the part encapsulated by step (3) above into the dispersion of step (2) and centrifuging.

In preparing the water-soluble isoflavone in the present invention, 1 to 2 g of water-soluble isoflavone is added to 3 to 20 g of the coating material. At this time, if the coating material is a solid at room temperature, first dissolve the coating material 3 to 20g in 30 ~ 70ml of distilled water and then add the water-soluble isoflavones. Medium-chain triglycerol used as a coating material in the present invention can be added immediately isoflavones in the liquid state at room temperature, but polyglycerol monostearate is a solid at room temperature, so when used as a coating material as mentioned above Polyglycerol monostearate is first dissolved in distilled water and then water-soluble isoflavones are added.

The solution mixed with the coating material and the water-soluble isoflavone is stirred in a predetermined stirring condition, preferably at a speed of 1200 to 2000 rpm, within 5 minutes so as to be suitable for spraying. After stirring, the solution mixed with the coating material and the water-soluble isoflavone is sprayed into an aqueous solution containing a low temperature surfactant by using a nebulizer. As the surfactant, food grade surfactant may be used. In the present invention, as an example of the surfactant, tween-60 is used to disperse the coating material coating the water-soluble isoflavone, so that the water-soluble isoflavone microcapsules have a compact structure. Can be prepared. In addition, the dispersion containing the surfactant used in the present invention is used by adjusting the concentration of the surfactant to 0.05 to 1.0%, the temperature of the dispersion for the production of water-soluble isoflavone microcapsules 5 ℃ or less, more preferably 0 ~ It is preferable to keep it at 5 degreeC.

Spraying the mixed solution of the coating material and the water-soluble isoflavone to the dispersion in the form of an aqueous solution containing a surfactant, the water-soluble isoflavone is coated by the coating material in the dispersion to be microencapsulated. Thereafter, the dispersion is centrifuged to separate the encapsulated and non-encapsulated portions to obtain microcapsules containing water-soluble isoflavones. Then, the microencapsulated portion is sprayed onto the dispersion containing the above-mentioned surfactant and centrifuged again to obtain microcapsules containing water-soluble isoflavones.

The present invention includes a functional food comprising the above-mentioned microcapsules containing water-soluble isoflavones as an active ingredient.

In the present invention, the microcapsules containing water-soluble isoflavones may be added to any one functional food selected from milk, yogurt, and beverages. In this case, the amount of the microcapsules may vary slightly depending on the type of functional food, but is generally added in an amount of 0.01 to 5 parts by weight based on 100 parts by weight of the functional food. If it is added less than 0.01 parts by weight, it does not mean adding the microcapsules containing water-soluble isoflavones, and when added by more than 5 parts by weight, there is no significant effect of the addition of microcapsules, so the microcapsules containing water-soluble isoflavones are not added. It is good to add 0.01-5 weight part with respect to 100 weight part of silver functional foods.

Hereinafter, the present invention will be described by the following examples and test examples. However, these are only examples of the present invention, and the scope of the present invention is not limited thereto.

Example 1 Microcapsules of Water-Soluble Isoflavones Using PGMS

5 g, 10 g, 15 g, and 20 g of polyglycerol monostearate (polyglycerol monostearate, PGMS, Ilshin Emulsification) were respectively mixed with 50 ml of distilled water. After mixing, the mixture was allowed to stand at 55 ° C. for 20 minutes and stirred for 1 minute at a speed of 1200 rpm to sufficiently dissolve PGMS to enable spraying.

To each PGMS solution was added 1 g of 30% water-soluble isoflavone (available from Pacific), and then stirred at 1200 rpm for 1 minute.

After stirring, the PGMS solution to which the water-soluble isoflavone was added was sprayed (W-300, Wagner Spray Tech. Co. Markdorf. Germany) into an aqueous solution at 5 ° C containing 0.05% of Tween-60 (Ishinshin Oil Products) as a surfactant. Sprayed to disperse.

The water-soluble isoflavones and PGMS sprayed emulsifier were centrifuged at 24900 × g for 10 minutes to separate the unencapsulated supernatant and the encapsulated filtrate. The encapsulated filtrate was sprayed into an aqueous solution at 5 ° C. in which 0.05% of Tween-60 was dissolved and centrifuged at 24900 × g for 10 minutes to prepare microcapsules containing water-soluble isoflavones.

Example 2 Microcapsules of Water-Soluble Isoflavones Using MCT

2000rpm speed by mixing 1g of 30% water-soluble isoflavone (Pacific Co., Ltd.) in 5g, 10g, 15g, 20g of liquid medium-chain triglycerol (MCT) Stirred for 1 minute. Each mixed solution was sprayed with an atomizer (W-300) into an aqueous solution at 5 ° C. containing 0.05% of Tween-60 (produced by Ilshin Emulsifier) as a surfactant.

It was then centrifuged at 4520 × g for 10 minutes to separate the encapsulated upper layer and the unencapsulated filtrate. The encapsulated upper layer was sprayed into an aqueous solution at 5 ° C. in which 0.05% of Tween-60 (Ilshin Emulsification) was dissolved and centrifuged at 4520 × g for 10 minutes to prepare microcapsules containing water-soluble isoflavones.

Test Example 1 Yield of Microcapsules

The yields of the microcapsules containing water-soluble isoflavones obtained in Examples 1 and 2 were measured and shown in Tables 1 and 2 below. Yield of isoflavone-containing microcapsules is calculated by measuring the amount of water-soluble isoflavones present in the external solution of microcapsules in an aqueous solution sprayed with water-soluble isoflavones. It was.

First, an appropriate amount of the solution except the microcapsules after centrifugation was taken and used as a sample of HPLC. As a result of HPLC, the area of each peak of the sample was compared with the standard to measure the encapsulation yield of the water-soluble isoflavones.

HPLC analysis of water-soluble isoflavones was a modified and supplemented method of Yi et al. (36) (Kwak HS, Ihm M R. β-D-galactosidase microencapsulated with fatty acid ester and milk containing the same.US patent No: 6,491,955). Analysis was performed with a gradient solvent system. The column used for the analysis was a μ-Bondapak C18 column of Waters (U.S.A.), a detector was used with a 254nm UV detector (Shimazu, Japan), and the injection volume was 20 μl. Mobile phases A and B used 20% methanol and 60% methanol, respectively. After the sample injection, the solvent gradient started from mobile phase A to 100, and then mobile phase B was linearly increased to 100 by 50 minutes, then mobile phase A was 100% by 60 minutes, and then mobile phase A was 100% by 65 minutes. Stabilizer and the column was stabilized by maintaining.

Table 1. Yield of microcapsules containing water-soluble isoflavones prepared in Example 1

Coating material (g) Core substance (g) yield(%) 5 One 43.4 10 One 61.8 15 One 67.2 20 One 50

Table 2. Yield of microcapsules containing water-soluble isoflavones prepared in Example 2

Coating material (g) Core substance (g) yield(%) 5 One 60.3 10 One 67.1 15 One 74.5 20 One 71.6

Test Example 2 Stability of Microcapsules in Artificial Gastric Fluids

The stability of the water-soluble isoflavone microcapsules was carried out using a method of measuring the release amount of the water-soluble isoflavone from the microcapsules according to the pH of the gastric juice and the incubation time, and the results are shown in FIG. 1.

After adding 20 mg of water-soluble isoflavone microcapsules prepared in Example 1 and 4 ml of pepsin solution (pH 1.2, 1 mg / ml) to 2 ml of distilled water, the pH of the solution in which the water-soluble isoflavone microcapsules was dissolved in 1N HCl was 2 , 3, 4, and 5 were adjusted. The above solution was incubated at 37 ° C in a constant temperature water bath each time (0, 20, 40, 60 minutes) (quality change during storage of yogurt containing micro-coated iron. Yun-ji Kim, Chil-seok Yoon. 1999. J. Korean Soc. Water soluble isoflavones released in the solution under Food Sci.Nutr. 28 (3): 542-546.) Were quantified by the HPLC method mentioned in Test Example 1.

Test Example 3 Stability of Microcapsules in Artificial Small Intestine

Stability in the artificial intestine of the microcapsules containing water-soluble isoflavones is measured as shown in Figure 2 as shown.

In Test Example 2, 0.02M cholic acid, 0.02M deoxycholic acid (bile salt), 5mg lipase, and pancreatin (pancreatin) were added to the solution incubated at different pH and time with artificial gastric juice. ) Solution (1 mg / ml phosphate buffer, pH 7.4) was added. The pH of this solution was adjusted to 6, 7, 8 with 1N hydrochloric acid and 1N sodium hydroxide, followed by incubation at 37 ° C. for each hour (0, 20, 40, 60 minutes) to quantify the water-soluble isoflavones by HPLC.

<Test Example 4>

Microcapsules containing water-soluble isoflavones prepared in Example 1 Water-soluble isoflavone according to the storage period while storing for 1 day, 3 days, 5 days, 8 days, 12 days at temperature conditions of 4 ℃, 20 ℃ and 30 ℃ The amount of flavone was grasped and the sensory effect was investigated. The results are shown in FIG. 3.

As shown in Figure 3 it can be seen that the optimum temperature for the storage of the water-soluble isoflavone microcapsules is 4 ℃.

<Test Example 5>

Nothing was added to 100 parts by weight of milk as a control, and 1 part by weight of water-soluble isoflavone microcapsules prepared in Example 1 was added to 100 parts by weight of milk. Experiment 1 and 1 g of isoflavones were added to 100 parts by weight of milk. What was done was experimental group 2. The control group, experimental group 1 and experimental group 2 were measured at 4 ° C. for 1 day, 3 days, 5 days, 8 days, and 12 days, and sensory characteristics such as degree of odor and taste were measured. Table 3 shows.

Sensory test personnel were selected 20 people (10 men and women each) who can distinguish the taste of milk, and trained for 10 days to conduct a sensory test. Sensory characteristics were evaluated by 9-point scoring method, and the results of sensory evaluation were analyzed statistically by analysis of variance and least significant difference test using SAS.

Table 3. Sensory test results of milk containing water-soluble isoflavone microcapsules

Sensory characteristics Experimental group storage duration 1 day 3 days 6 days 9th 12 days Bean fishy Control 1.0 * 1.0 1.0 1.0 1.0 Experimental group 1 1.7 2.0 2.1 2.4 2.7 Experiment group 2 4.3 3.9 4.7 5.4 5.5 bitter Control 1.0 1.0 1.0 1.0 1.0 Experimental group 1 1.17 1.3 1.5 1.7 2.1 Experiment group 2 1.5 1.4 2.2 2.6 2.7 color Control 1.0 1.0 1.0 1.0 1.0 Experimental group 1 1.4 1.6 2.1 2.5 2.7 Experiment group 2 4.9 5.3 5.6 5.45 5.9

* 1: No change, 3: Slightly present, 5: Medium, 7: Strong. 9: Very strong.

In the case of bitterness (bitterness) as shown in Table 3 there was little change with increasing storage period in all experimental groups. Differences between experimental groups were also not significant for 12 days of storage. This means that the water-soluble isoflavones do not produce other off-flavors even after breakdown of the coating over time, and there is no sensory change in the bitter taste of the milk's inherent flavor.

In the case of color, isoflavones have inherent brown color, so the change of color with increasing storage period is important. Experimental group 2 with isoflavones was evaluated to have a brown color gradually with increasing storage period. In particular, after 6 days of storage, the color changed to brown compared to the control, which showed a significant difference in the sensory properties of milk. Experimental group 1 with water-soluble isoflavone microcapsules showed a subtle difference that was difficult to judge with the naked eye and showed a slight sensory difference after 9 days. This is because isoflavones leak into the milk with the destruction of the coating material as the storage period becomes longer.

In case of beany flavor, experimental group 2 showed significant difference compared to the control group from day 1, and soybean odor increased as storage period increased. On the other hand, the experimental group 1 showed a slight difference compared to the control, but as the storage period increased, soybean odor also increased slowly. There was little change until 3 days after storage, and it showed a tendency to increase gradually after 6 days, but it did not change the state of the product significantly.

The results of sensory evaluation showed that the encapsulated isoflavones had little change in the bitter taste according to the storage period. It can be seen that the addition of isoflavone microcapsules is effective.

The water-soluble isoflavone microcapsules of the present invention from the results of the above examples and test examples facilitate the ingestion of isoflavones without reducing the sensory properties of milk when added to functional foods, especially milk. Therefore, there is an advantage that can easily consume conventionally useful isoflavones.

1 is a graph showing the release amount of water-soluble isoflavones from water-soluble isoflavone microcapsules according to pH and incubation time in artificial gastric juice.

Figure 2 is a graph showing the release amount of water-soluble isoflavones from water-soluble isoflavone microcapsules according to pH and incubation time in artificial intestine.

3 is a graph showing the free amount of water-soluble isoflavones from water-soluble isoflavone microcapsules according to temperature and storage period.

Claims (9)

A microcapsule containing a water-soluble isoflavone encapsulated with polyglycerol monostearate (PGMS) or medium-chain triacylglycerol (MCT) as a coating material coating the core material with a water-soluble isoflavone as a core material. According to claim 1, wherein the coating material is a microcapsules containing water-soluble isoflavones, characterized in that 60 to 90% by weight based on the weight of the capsule. The microcapsule containing water-soluble isoflavones according to claim 1, wherein the water-soluble isoflavone is 10 to 40% by weight based on the weight of the capsule. The microcapsule containing water-soluble isoflavones according to claim 1, wherein the capsule has a diameter of 2 to 5 μm. In the preparation of microcapsules containing water-soluble isoflavones, (1) adding water-soluble isoflavones to a coating material solution of polyglycerol monostearate (PGMS) or medium-chain triacylglycerol (MCT), (2) stirring the solution mixed with the coating material and the water-soluble isoflavone and spraying the dispersion in the form of an aqueous solution containing a surfactant; (3) centrifuging the emulsifier sprayed with the coating material and the water-soluble isoflavone to separate the encapsulated portion and the non-encapsulated portion, (4) a method for producing a water-soluble isoflavone-containing microcapsule, comprising the step of spraying and centrifuging the part encapsulated by step (3) in the former step (2). The method for preparing a microcapsule containing water-soluble isoflavones according to claim 5, wherein 1 to 2 g of water-soluble isoflavones are added to 3 to 20 g of the coating material of polyglycerol monostearate or medium chain triglycerides. The method of claim 5, wherein the coating material solution is a solution obtained by adding 3 to 20 g of polyglycerol monostearate to 30 to 70 ml of distilled water or 3 to 20 g of medium chain triglyceride. . Functional food comprising a microcapsule containing the water-soluble isoflavone of any one of claims 1 to 4. The functional food according to claim 8, wherein the functional food comprises microcapsules containing water-soluble isoflavones, wherein the functional food is any one selected from milk, yogurt and milk.