KR20040048749A - Microencapsulation of vitamin C and iron fortified milk with Microencapsulation of vitamin C - Google Patents

Abstract

PURPOSE: Provided is iron fortified milk which contains vitamin C, micro-encapsulated by polyglycerol monostearate(PGMS), preventing oxidation of iron in the milk. The PGMS capsule is stable in an artificial gastric and small intestine fluid. CONSTITUTION: The milk comprises 10mg of iron and 10-40mg of vitamin C, micro-encapsulated by PGMS or middle sized triacylglycerol(MCT) in 100ml of milk in which the ratio of vitamin C and the coating material is 87-97wt.% : 3-13wt.% and the diameter of the capsule is 2-5micrometer. The specific gravity of the capsule and the milk is identical.

Description

Microcapsule containing vitamin C and iron fortified milk containing same {Microencapsulation of vitamin C and iron fortified milk with Microencapsulation of vitamin C}

The present invention relates to microcapsules containing vitamin C and iron fortified milk containing the same, and more specifically, to polyglycerol mono stearate (PGMS) or medium-chain triacylglycerol (MCT) as a coating material The present invention relates to a microcapsule containing vitamin C encapsulating vitamin C and iron fortified milk which can inhibit oxidation of iron in milk by adding it to milk containing iron.

Milk is an almost complete nutritious food that contains all the nutrients necessary for human health, such as proteins, fats, carbohydrates, vitamins and calcium. come. In Korea, the dairy industry started in 1960, and in 1990, milk production exceeded 1.75 million tons. In 2000, more than 2.25 million tons of milk was consumed. It 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 developed countries.

Recently, the increase in white milk is weak, but the consumption of processed milk containing nutrients or other flavor-rich substances has been steadily increasing.Therefore, there is an urgent need for technology development and commercialization to diversify the quality of processed milk. It's happening. Among them, vitamin-enriched milk, which is fortified with insufficient vitamins in milk, to make milk more complete foods, is emerging in the market one after another.

Milk must be heat sterilized to kill pathogenic microorganisms and inactivate harmful elements. The ultra high temperature sterilization process, which is most widely used in Korea, is an essential process to sterilize harmful microorganisms.However, in the process of heating and sterilization, major nutrients in milk, especially protein and calcium, occur, and micronutrients such as vitamin B1, B6, It is known that B12, folic acid and vitamin C are lost by heat treatment.

In order to make up for this drawback, milk is subjected to long time low temperature (LTLT), but the loss of vitamin C and other vitamins is inevitable.

Vitamin C is a water-soluble vitamin. It is an essential vitamin that is not produced by the body. Its chemical structure is similar to glucose and its active form in the body, L-ascorbic acid and its oxidized L-dehydroasco It can be divided into L-dehydroascorbic acid. They are interconverted in living cells, and L-ascorbic acid is called reduced vitamin C and L-dehydroascorbic acid is called oxidized vitamin C.

Vitamin C has several important functions in the body, which are antioxidants. Since vitamin C is easily oxidized, it can act as an antioxidant that inhibits oxidation of other substances by first oxidizing under conditions that can be oxidized, and is actually used for preventing rancidity in food processing. In addition, vitamin C is known to prevent oxidation of linoleic acid, polyunsaturated fatty acids, vitamin E, vitamin A and the like in the body.

Secondly vitamin C is indirectly by increasing the absorption of inorganic iron maintain the polar active form of God-tetrahydro-polar new (THFA) involved in the formation of red blood cells with vitamin in relation to the iron absorption C is the Fe ³ oxidation ⁺ (ferric iron) helps the absorption because it helps the conversion to reduced form of Fe ²⁺ (ferrous iron). In addition, vitamin C is an essential ingredient for collagen synthesis and is required for the amino acid metabolism.

Currently, the recommended daily dose of vitamin C is 60 mg in the US and 50 mg in Japan. In our country, infants (0-11 months) 35mg, children (1-9 years) 40mg, 50mg from 10 to 15 years old, 55mg from 16 years of age or older. However, the recommended amount of vitamin C varies depending on the individual's condition. For pregnant women, 70 mg is considered to be the loss from the fetus, and for lactating women, it is 90 mg for the loss from breast milk.

The present invention aims to provide an iron-enriched milk that can inhibit the oxidation of iron by containing a microcapsules containing vitamin C encapsulating vitamin C having antioxidant properties and iron-enriched milk.

In another aspect, the present invention is to provide a vitamin C-enriched milk by adding the microcapsules containing vitamin C to the milk.

1 is a graph showing the change of vitamin C released at each temperature during the storage period of the capsule containing the PGMS coating material.

2 to 4 is a graph showing the absorbance of the milk according to the additives of milk (control) and iron fortified milk added nothing during the storage period of 15 days.

5 is a graph showing the amount of vitamin C released according to the pH of the pepsin solution capsules prepared with a weight ratio of 5: 5 to PGMS: vitamin C in Example.

FIG. 6 is a graph showing the amount of vitamin C released according to pH and incubation time in the artificial intestine containing a vitamin C capsule containing PGMS as a coating material.

The present invention includes a microcapsule containing vitamin C and iron fortified milk which can inhibit the oxidation of iron in milk by adding it to iron fortified milk containing iron.

Vitamin C in addition to the role of vitamin as a nutritional substance in the present invention serves as an antioxidant that can prevent the oxidation of iron contained in iron fortified milk.

In the present invention, the coating material in the microencapsulation of vitamin C encapsulates vitamin C using polyglycerol monostearate (PGMS) or medium-chain triacylglycerol (MCT).

In the microcapsules containing vitamin C in the present invention, the vitamin C as the main substance is to contain 87 to 97% by weight based on the capsule weight, the coating material is to contain 3 to 13% by weight based on the capsule weight capsule Specific gravity equals to milk. In the present invention, if the specific gravity of the capsule is added to the milk in comparison with the specific gravity of the milk, the capsules are gathered at the upper part of the milk, and if the specific gravity of the capsule is large, it is mainly distributed in the lower part of the milk to effectively inhibit the oxidation of iron contained in the milk. Not preferred below. Therefore, in the present invention, it is preferable to make the specific gravity of the capsule equal to that of milk, and to distribute the milk evenly.

In the present invention, the capsule containing vitamin C has a diameter of 2 to 5 µm and has a spherical shape. If the capsule diameter is less than 2㎛ the amount of vitamin C that can inhibit the oxidation of iron contained in the milk is insufficient, if the diameter of the capsule exceeds 5㎛ the capsule material rises up when storing the milk containing the capsule For this reason, in the present invention, the diameter of the capsule is preferably maintained at 2 to 5 μm.

Meanwhile, the present invention comprises 10 to 40 mg of microcapsules containing vitamin C with respect to 100 ml of iron fortified milk containing 10 mg of iron. If the amount of the microcapsules containing vitamin C was less than 10 mg to 100 ml of iron fortified milk containing 10 mg of iron, it was insufficient to inhibit the oxidation of iron, and the amount of the microcapsules containing vitamin C exceeded 40 mg. When the milk is ingested by the addition of an excess capsule without a noticeable effect of inhibiting the oxidation of iron, in the present invention, vitamin C is contained in 100 ml of iron fortified milk containing 10 mg of iron. It is preferable to contain 10-40 mg of the prepared microcapsules.

In the present invention, iron-enriched milk containing iron includes processed milk such as strawberry milk, chocolate milk, vanillau oil, as well as ordinary white milk.

Meanwhile, the iron-enriched milk containing the microcapsules containing vitamin C of the present invention is sufficient to add a process of adding a capsule containing vitamin C to known iron-enriched milk. The addition of capsules may include (1) adding only capsules containing vitamin C, for example, iron powder containing microcapsules containing vitamin C by adding and mixing microcapsules containing vitamin C to sterilized iron fortified milk. Fortified milk can be prepared. (2) Iron capsules containing vitamin C may be mixed with iron-enriched milk and mixed with sterilized milk to produce iron-enriched milk containing microcapsules containing vitamin C.

The microcapsules containing vitamin C of the present invention may be added in iron-enriched milk by varying the size, weight and blending ratio of the capsules according to the iron content.

The present invention can be microencapsulated containing vitamin C by PGMS or MCT as a coating material by the following process. For example, PGMS may be used as a coating material to microencapsulate vitamin C by the following steps.

(1) At room temperature, liquid PGMS having a high viscosity is mixed with distilled water, and the mixture is allowed to stand at 55 to 60 ° C. for 20 to 30 minutes, followed by stirring at 1200 to 1400 rpm for 1 to 3 minutes to sufficiently dissolve the PGMS.

(2) PGMS and vitamin C are mixed at a weight ratio of 5 to 20: 1 and stirred for 1 to 3 minutes at 1200 to 1400 rpm.

(3) Spray the mixture of PGMS and vitamin C with a spray gun (W-300) to a dispersion of 5-7 ° C in which 0.05% of Tween-60 is dissolved.

(4) Centrifuge the spray liquid obtained in step (3) at 24,900 x g for 10 minutes to separate the unencapsulated supernatant from the encapsulated filtrate.

(5) Take only the encapsulated filtrate and spray it on the Tween-60 dispersion, and then perform step (4) again to prepare a microcapsule with the core material as vitamin C and the coating material as PGMS.

Hereinafter, the present invention will be described by the following examples and test examples. However, these are not limited to the scope of the present invention by them as an example of the present invention.

EXAMPLES Preparation of Vitamin C Microcapsules Using PGMS as a Coating Material

Since PGMS is solid at room temperature, it is first mixed with distilled water, and then heated at a high temperature, preferably 80 ° C. or more, to dissolve PGMS. Since it is difficult to spray even in this state, the liquid PGMS having high viscosity at room temperature was mixed with distilled water, and the mixture was allowed to stand at 55 ° C. for 20 minutes, followed by stirring at 1200 rpm for 1 minute to sufficiently dissolve the PGMS.

PGMS and vitamin C are mixed at a weight ratio of 5 to 20: 1 and stirred at 1200 rpm for 1 minute, and the PGMS and vitamin C mixture is sprayed with a spray gun (W-300) at 0.05% of Tween-60 (Ilshin Oil Products, Korea). Sprayed to this dissolved 5 ° C dispersion.

The previous dispersion is centrifuged at 24,900 x g for 10 minutes to separate the unencapsulated supernatant from the encapsulated filtrate. Then, only the encapsulated filtrate was taken and sprayed into the Tween-60 dispersion, followed by one more centrifugal separation process to remove the unencapsulated vitamin C, thereby preparing a microcapsule having a core material of vitamin C and a coating material of PGMS. .

Test Example 1 Yield of Microcapsules Containing Vitamin C

The yield of the microcapsules prepared in Example 1 was measured and the results are summarized in Table 1 below.

Yield measurement of microcapsules is a method of calculating the amount of vitamin C present in the microcapsule external solution in the dispersion sprayed with vitamin C (DNP quantitative method, Food Code) 2000. KFDA Chapter 7: 289-291).

Table 1. Yield of capsules according to the weight ratio of PGMS and vitamin C

Weight ratio (w / v) yield(%) PGMS Vitamin c 5 One 94.2 ^a 10 One 86 ^b 15 One 85 ^b 20 One 80.7 ^c

^The absence of the same letter in the column of ¹ yield means no significant difference (P <0.05).

Test Example 2 Measurement of Vitamin C Free Amount of Vitamin C Capsule

In Example 1, the weight ratio of the coating material: vitamin C was 5: 1, and the vitamin C-containing microcapsules prepared at a different temperature were stored for a predetermined period of time to measure stability.

10 ml (1 mg / ml) of capsule solution obtained by dissolving 1 mg of each capsule in 1 ml of distilled water and the same amount of distilled water were added, and the amount of free vitamin C was measured while storing at 4 ° C., 20 ° C. and 30 ° C. for 30 days. The results are shown in FIG.

The amount of free vitamin C was measured by centrifugation of 10 ml of the stored vitamin C microcapsule mixed solution to separate the free vitamin C from the microcapsules and microcapsules by DNP method.

1 is a graph showing the change of vitamin C released at each temperature during the storage period of the capsule containing the PGMS coating material.

Test Example 3 Oxidation Degree of Milk

100 ml milk was used as a control and various additives were added to 100 ml milk as experimental groups (samples 1 to 4) and stored at 4 ° C. for a period of time (5 days, 10 days, 15 days) and TBA ( thiobarbituric acid) was used to determine the oxidation of the control and experimental milk.

TBA mixed solution was prepared by mixing 15% (w / v) TCA, 0.375% (w / v) 4,6-dihydroxypyrimidine-2-thiol, 0.25N HCl well.

Oxidation degree was determined by weighing 1 g of control and experimental group milk, putting it in a glass centrifuge tube, adding 9 ml of the TBA solution prepared above, mixing well, and heating in a water bath for 15 minutes. do. The reaction solution was immediately cooled to room temperature (20 ° C.), and then centrifuged at 7000 × g for 15 minutes to obtain a clear pink-yellow color supernatant, which was measured for absorbance at 535 nm. 3 and 4 (Buege, JA and Aust, SD 1984. Microsomal lipid peroxidation. In Methods in Enzymology. S. Fleischer and L. Packer, ed. Academic Press. New York, NY. P105).

In the above experimental group, Sample 1 includes 10 mg of iron (Ferric ammonium sulfate) in 100 ml of milk. Sample 2 contains 10 mg of iron capsules encapsulated in PGMS in 100 ml milk. Sample 3 contains 10 mg of iron capsules encapsulated in PGMS in 100 ml of milk and 10 mg of L-ascorbic acid. Sample 4 includes 10 mg of iron capsules encapsulated in PGMS in 100 ml milk and 10 mg to 40 mg of vitamin C capsules encapsulated in PGMS.

Vitamin C capsules encapsulated in PGMS in Sample 4, the capsules prepared in Example 1 with a weight ratio of 5: 5 PGMS: vitamin C was used.

2, 3 and 4 is a graph showing the absorbance of the milk, where Sample 4 is 10mg, 25mg, 40mg is added to the vitamin C capsule encapsulated in PGMS, respectively.

As shown in FIGS. 2 to 4, the experimental group (Sample 4) to which vitamin C capsules were added to the iron-enriched milk up to 10 days of storage period showed similar absorbance to that of the control milk to which nothing was added. It can be seen that. On the other hand, Sample 3 immediately added with vitamin C has low absorbance until the first 5 days to inhibit the oxidation of milk, but after 5 days it can be seen that the absorbance is increased dramatically, the iron oxidation in milk is increased by the initial vitamin C Oxidation of is inhibited It can be seen that the oxidation of iron in milk proceeds rapidly due to inactivation of vitamin C.

Test Example 4 Sensory Test

Add 10mg, 25mg, 40mg of vitamin C capsules to 100ml of white milk (Seoul milk products) and store it for a certain period of time (1, 3, 5, 8, 12 days), Sensory properties were measured and the results are shown in Table 2 below.

The sensory test personnel selected 30 people who could distinguish the taste of milk and performed the 5-point method.The results of the sensory test were analyzed by SAS (SAS (R) User's Guide.1986. Statistics. SAS Inst., Inc., Cary, NC, USA.) Were used for statistical analysis by analysis of variance and least significant difference test.

Table 2. Sensory test results of milk containing vitamin C capsules coated with PGMS

Coating material Capsule addition amount (mg) Sensory characteristics Storage period (day) One 3 5 8 12 PGMS 10 Sour taste 1 ^b 1.4 ^b 1.6 ^b 2.4 ^a 3 ^a Already, Off-flavor ¹ 1.2 ^c 1.4 ^c 1.6 ^c 2.4 ^b 3.2 ^a Full symbol 1 ^c 1.6 ^bc 1.8 ^b 3 ^a 3.4 ^a 25 Sour taste 1 ^c 1.2 ^c 2 ^b 2.6 ^b 3.4 ^a Already 1.4 ^c 1.4 ^c 1.8 ^bc 2.2 ^b 3.8 ^a Full symbol 1.2 ^d 1.8 ^cd 2.4 ^bc 3 ^ab 3.8 ^a 40 Sour taste 1.4 ^c 2.2 ^b 2.6 ^b 3.4 ^a 3.6 ^a Already 1.4 ^d 1.8 ^cd 2.4 ^bc 2.8 ^b 3.8 ^a Full symbol 1.2 ^d 2.4 ^c 3 ^bc 3.8 ^ab 4.6 ^a

* Sour & Already, resulting in off-flavor: 1: none, 2: slight, 3: moderate, 4: slightly strong, 5: strong.

* The higher the numerical value is, the less the preference is.

* There was no significant difference (P <0.05) in columns without subscripts of the same letter of sensory results.

* ¹ Except for sour and normal milk taste.

As shown in Table 2, the sourness of the milk to which the vitamin C capsules containing PGMS as a coating material was added was increased during storage for one day, and the change amount was small for five days when 10 mg of microcapsules were added. The milk with 25 mg added also had little change in taste. However, the strength of the sour taste increases from the 5th day of storage of the milk added 40mg.

In the case of off-taste, milk with 10 mg and 25 mg added showed similar scores up to 5 days, and off-taste felt off-taste from day 1 and strongly after 8 days. . The milk added 10mg and 25mg also felt off-taste after 8 days, which may be due to the capsule off-taste, but the production of off-taste with the expiration date of milk is one of the causes.

In the case of total palatability, which is a comprehensive sensory test, all the milk containing 10 mg, 25 mg, and 40 mg of vitamin C capsules decreased as the storage period increased.

Test Example 5 Stability of Vitamin C Capsules

(1) Stability of vitamin C capsule in artificial gastric juice

The stability of the vitamin C capsule was measured by measuring the amount of vitamin C released from the capsule according to the pH and incubation time of the gastric juice.

First, 20 mg of microcapsules containing vitamin C were added to 2 ml of distilled water, and 4 ml of pepsin solution (pH 1.2 1 mg / ml) was added, and then the pH of the pepsin solution was adjusted to 2, 3, 4, and 5 with 1N HCl. . The pepsin solution was then incubated in a 37 ° C. constant temperature water bath (0, 20, 40, 60 minutes) (Rao DR, Chawan CB, Veeramachaneni R. 1995. Liposomal encapsulation of β-galactosidase: Comparison of two methods of encapsulation and in In vitro lactose digestibility. J. Food Biochem. 18: 239-251.) The vitamin C released in the pepsin solution was quantified by the DNP method, and the results are shown in FIG. 5.

In the capsule containing vitamin C, a vitamin C capsule prepared in Example 1 with a weight ratio of PGMS: vitamin C 5: 1 was used.

FIG. 5 is a graph showing the amount of vitamin C released according to the pH of pepsin solution of the capsule prepared in Example 2 with a weight ratio of PGMS: vitamin C 5: 1. At pH 5 of FIG. 5, the release amount of vitamin C was increased until the initial 20 minutes, after which the release amount was decreased.

(2) Stability of vitamin C capsule in artificial intestine

After measuring the amount of vitamin C released from the artificial gastric juice of (1), the amount of vitamin C released from the capsule was measured while adding artificial small intestine and adjusting the pH to 6, 7, and 8.

After the above step (1), 0.02M cholic acid, 0.02M dioxycholic acid (bile salt), 5mg lipase was added to pepsin solution as an artificial small intestine solution and pancreatin solution (1mg / ml phosphate buffer, pH7). .4) was added.

After adjusting the pH of the solution with 1N HCl and 1N NaOH to 6, 7, 8, the solution containing pancreatin was incubated for 1 hour at 37 ° C for 20 minutes and quantified by the DNP method. The results are shown in FIG.

FIG. 6 is a graph showing the amount of vitamin C released according to pH and incubation time in the artificial intestine containing a vitamin C capsule containing PGMS as a coating material.

As shown in the results of the test example, vitamin C capsules using PGMS as a coating material are not only stable in gastric juice and intestinal fluid but also excellent in sensory test in milk containing vitamin C capsules. On the other hand, iron-enriched milk containing microcapsules containing vitamin C, which is made from vitamin C as a main substance and coated with a coating material that coats the core substance, inhibits the oxidation of iron in milk and is easily consumed by drinking it. Do.

Claims (7)

A microcapsule containing vitamin C as the main substance and vitamin C encapsulated in a coating material coating the core substance. The microcapsule containing vitamin C according to claim 1, wherein the coating material is polyglycerol monostearate (PGMS) or medium-chain triacylglycerol (MCT). According to claim 1, Vitamin C is a microcapsules containing vitamin C, characterized in that 87 to 97% by weight based on the weight of the capsule. According to claim 1, wherein the coating material is a microcapsules containing vitamin C, characterized in that 3 to 13% by weight based on the weight of the capsule. The microcapsules containing vitamin C according to claim 1, wherein the capsule has a diameter of 2 to 5 μm. Iron-enriched milk comprising a microcapsules containing vitamin C, characterized in that 10 to 40mg of the microcapsules containing vitamin C of claim 1 for milk 100ml containing iron 10mg. 8. The iron fortified milk of claim 7, wherein the specific gravity of the capsule is the same as that of milk.