KR100871050B1 - Preparation method of microcapsule comprising coenzyme Q1O - Google Patents

Abstract

The present invention relates to a method for producing a microcapsule containing coenzyme Q10, using coenzyme Q10 as a core material and a natural material as a wall material to enhance the extracorporeal storage of coenzyme Q10 in poorly soluble crystals, and to efficiently target organs. The present invention relates to a method for preparing a microcapsule which increases digestion absorption efficiency to be delivered to and improves stability in the body by providing acid resistance.

Coenzyme Q10, Microcapsules, Acid Resistance

Description

Preparation method of microcapsules containing coenzyme Q10 {Preparation method of microcapsule comprising coenzyme Q1O}

1 is an electron micrograph (x400) of Coenzyme Q10,

Figure 2a and 2b is an electron micrograph (x300) of the powder microcapsules of coenzyme Q10 in Figure 2a,

3a to 3c are electron micrographs (x400) of the microcapsules showing the results of the pH resistance test of the microcapsules of coenzyme Q10 prepared according to Example 1 (a: dH ₂ O; b: pH2 PBS; c: pH8 PBS),

4a to 4c are electron micrographs (x400) of the microcapsules showing the results of the pH resistance test of the microcapsules of coenzyme Q10 prepared according to Example 2 (a: dH ₂ O; b: pH2 PBS; c: pH8 PBS),

5a to 5c are electron micrographs (x400) of the microcapsules showing the results of the pH resistance test of the microcapsules of coenzyme Q10 prepared according to Example 3 (a: dH ₂ O; b: pH2 PBS; c: pH8 PBS),

6a to 6c are electron micrographs (x400) of the microcapsules showing the results of the pH resistance test of the microcapsules of coenzyme Q10 prepared according to Example 4 (a: dH ₂ O; b: pH2 PBS; c: pH8 PBS),

7a to 7c are electron micrographs (x400) of the liquid microcapsules (a) and the powder microcapsules (b, c) prepared according to Examples 5 to 7,

8a to 8c are electron micrographs (x400) of the liquid microcapsules (a) and the powder microcapsules (b, c) prepared according to Examples 8 to 10.

The present invention relates to a method for producing a microcapsule which increases the digestive absorption efficiency so as to be efficiently delivered to a target organ and gives acid resistance to improve the stability in the body.

Coenzyme Q10 (Coenzyme Q10, C ₅₉ H ₉₀ O ₄ ) is a fat-soluble vitamin compound synthesized in the body, is known to be involved in the metabolism of nutrients and excellent antioxidant power.

It is also found in blue fish such as mackerel, saury and sardines, as well as nuts such as brown rice, eggs, beans, spinach and peanuts. Coenzyme Q10 can be obtained in small amounts through foods such as meat, but most are made in the body.

Coenzyme Q10 reduces blood sugar by converting sugar into energy, and acts as an antioxidant like vitamin E to prevent oxidation of cell membranes and increase oxygen utilization.

In addition, it activates sperm and enhances the function of immune cells and leukocytes. It also has excellent antioxidant ability to inhibit the production of free radicals, preventing cardiovascular diseases such as arteriosclerosis and hypertension, cancer, cerebral hemorrhage, Alzheimer's disease and diabetes. Giving effect is also.

As coenzyme Q10 is in the 20s, the synthesis gradually decreases, and the cellular function is weakened and cannot be reproduced as fast as before, which causes aging.

Coenzyme Q10, which is related to ATP synthesis, a source of energy, has been recognized as a health food in addition to medicines since the 1980s in Gumi, and is generally known as a health food rather than a medicine.

It has been used as a myocardial function improver since 1974 in Japan, but the Ministry of Health, Labor and Welfare approved it as a food in 2001. Since the US has been used as a medicine for a long time since 2001 began to be used as a functional food material has been increasing in popularity even now.

Coenzyme Q10, which is used as a medicine and food because of its excellent antioxidant function, is a yellow-red powder that is hydrophobic and has a problem of using a large amount of carrier to dissolve a small amount in oil.

In addition, because coenzyme Q10 has a high physiological activity, the activity tends to decrease rapidly when exposed to air and light or exposed to acid.

Therefore, the development of a technology that can protect the physiological activity of coenzyme Q10 and further increase the digestive absorption efficiency is urgent.

The present invention was created in order to solve the problems of the prior art as described above, in order to increase the digestion and absorption efficiency of coenzyme Q10 of poorly soluble crystals in solution form and further reduce the production cost and inventory stability of the natural foods This was accomplished by developing a microcapsule using the material as a wall material.

Accordingly, an object of the present invention is to provide a method for producing a microcapsule that can protect the physiological activity of coenzyme Q10 and further increase the digestive absorption efficiency.

In order to achieve the above object, the present invention

Dissolving coenzyme quene in at least one or more edible oils selected from the group consisting of soybean oil, perilla oil, pine oil and olive oil to prepare a coenzyme quene solution; Mixing the sugar and the protein to prepare a wall material; And it provides a method for producing a liquid microcapsule comprising the step of mixing the coenzyme Q10 solution and the wall material and stirring or sonicating to precipitate the microcapsules.

In addition, the present invention comprises the steps of dissolving the coenzyme Q10 in one or more edible oils selected from the group consisting of soybean oil, perilla oil, pine oil and olive oil to prepare a coenzyme Q10 solution; Mixing the sugar and the protein to prepare a wall material; Mixing the coenzyme quene solution with the wall material and stirring or sonicating to precipitate liquid microcapsules; And spray drying the liquid microcapsules to produce a microcapsule powder.

Hereinafter, the present invention will be described in more detail.

Coenzyme Q10 used as the active ingredient in the present invention is a crystalline phase, as shown in Figure 1 shows a poor solubility insoluble in water or edible oils and fats.

First, one or more edible oils and fats selected from the group consisting of soybean oil, perilla oil, pine oil and olive oil are used as a substrate for dissolving poorly soluble coenzyme Q10.

At this time, the edible oil is preferably used in 50 to 100 parts by weight with respect to 1 part by weight of coenzyme Q10. If edible oil is used in less than 50 parts by weight of coenzyme Q10 is not dissolved as desired, if used in excess of 100 parts by weight of saturation of the coenzyme Q10 is edible edible oil and waste is not economical.

In addition, in the present invention, the wall material used to manufacture the capsule around the coenzyme Q10 is made of a natural material, prepared by mixing maltodextrin, wheat flour extract, milk protein, and gum, preferably maltodextrin 80-98 It is prepared by mixing weight%, wheat flour extract 0.1-10% by weight, milk protein 0.1-5% by weight and galvanic 0.1-5% by weight.

At this time, the content of the wall material with respect to 1 part by weight of the coenzyme qten solution, which is the main substance, is 1 to 10 parts by weight, and preferably mixed in the same amount with the coenzyme qten solution, but can be determined in consideration of the coenzyme qten concentration of the final product. have.

However, when the content of the wall material solution is less than 1 part by weight, microcapsules may be unstable to cause liposomes to leak, and when the content of the wall material is more than 10 parts by weight, the production cost may increase due to excessive use of the wall material. Can be.

On the other hand, the maltodextrin can be used by replacing with cyclodextrin, modified starch or polysaccharides.

The agitation is performed for 30 seconds to 30 minutes, and the stirring device used can be used for everything from a high speed stirrer of 10,000 rpm to a general mixer for home use.

In this case, when the stirring time is less than 30 seconds, microcapsulation may be incomplete, causing a problem of layer separation, and when the stirring time exceeds 30 minutes, a high temperature may occur to cause degeneration of the membrane and increase a manufacturing cost. have.

The ultrasonic wave is processed for 30 seconds to 3 minutes, and any ultrasonic wave device capable of stirring the solution while radiating the ultrasonic wave in a predetermined direction may be used.

In this case, if the ultrasonic treatment time is less than 30 seconds, the production of microcapsules may be incomplete, causing problems such as liposomes leaking or the shape of the capsules being uneven, and if exceeding 3 minutes, the wall component of the capsule may be affected by high heat. This can lead to denaturation which can lead to the problem of capsule instability.

The liquid microcapsules prepared by including the above steps induce the microencapsulation of coenzyme Q10, facilitate digestion and absorption of coenzyme Q10, which is a poorly soluble crystal phase, and have the advantage of improving acid stability by providing acid resistance.

On the other hand, unlike the liquid microcapsules in order to prepare a powder microcapsules spray-dried them, the prepared liquid microcapsules are spray-dried.

The spray drying is determined at a level at which the inlet temperature does not cause browning of the wall material, and is suitably 120 to 170 ° C., and the outlet temperature is controlled to be 60 to 100 ° C. by adjusting the flow rate of the inflowing air.

In addition, the powder microcapsules prepared according to the present invention may further comprise the step of treating the polyvinylpyrrolidone after the spray drying.

At this time, the polyvinylpyrrolidone used is preferably 0.5 to 1 parts by weight based on 1 part by weight of the powder microcapsules, and the treatment of the polyvinylpyrrolidone improves the stability of the microcapsules.

Meanwhile, in order to increase the solubility of the powder product, CMC (carboxymethyl cellulose) may be used in an amount of 0.5 to 1 parts by weight.

The content of coenzyme Q10 in the microcapsules prepared according to the present invention may be included up to 50% by weight.

In addition, the microcapsules may further include a flavoring agent, and the flavoring agent may be used as 0.1 to 1% by weight of persimmon oil or herb aroma, based on 100% by weight of the powder microcapsules, in addition to providing functionality Vitamins and natural antioxidants may be added in an amount of 1 to 10% by weight based on 100% by weight of powder microcapsules, and natural sweeteners including stevia may be added in an amount of 0.1 to 1% by weight based on 100% by weight of powder microcapsules. have.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the present invention is not limited by these examples.

<Examples 1 to 2> Preparation of liquid microcapsules

Coenzyme Q-tenen was prepared by mixing soybean oil such that the concentration of coenzyme Q-tenen, a poorly soluble crystal phase, was 10% by weight and then mixed with the same amount of wall material solution.

At this time, the solution containing the wall material was prepared by dissolving 25% by weight maltodextrin, 0.1% by weight wheat flour extract, 0.1% by weight milk protein and 0.1% by weight distilled water as a solvent.

The coenzyme Q10 solution was stirred for 3 minutes to prepare a liquid microcapsule of Example 1.

In addition, the coenzyme Q10 solution was sonicated for 30 seconds to prepare a liquid microcapsules of Example 2.

Example 3 Preparation of Powder Microcapsules

Powder microcapsules were prepared by heating the liquid microcapsules prepared by the ultrasonic treatment in Example 2 using a spray dryer.

The spray drying was carried out by adjusting the inlet temperature to 150 ± 10 ℃ and the outlet temperature to be 80 ± 10 ℃ by adjusting the flow rate of the air introduced.

As a result, as shown in FIG. 2A, microcapsules having a size of 894.96 nm can be confirmed, and an electron micrograph of 3000 magnification is shown in FIG. 2B.

Example 4 Preparation of Powder Microcapsules

In order to increase storage stability as well as pH stability of the powdered microcapsules, the powdered microcapsules prepared in Example 3 were treated with a 0.1% by weight polyvinylpyrrolidone (PVP) solution.

Experimental Example 1 pH Resistance Test

The resistance to pH 2 and pH 8 of the microcapsules obtained in Examples 1 to 4 was examined by the following method. In the pH resistance test, the microcapsule powder was dissolved in 1% by weight in a phosphate buffer adjusted to pH 2 and 8, and the size and shape of the microcapsules were examined under 400 magnification using an optical microscope.

3a to 3c is a result of pH resistance of the microcapsules according to Example 1, Figure 4a to 4c is a result of pH resistance of the microcapsules according to Example 2, coenzyme Q10 microcapsules compared to the coenzyme Q10 of Figure 1 The crystal phase was not visible in Esau and therefore all of the coenzyme Q10 were successfully converted into solution phase and further encapsulated.

In addition, as shown in Table 1, the ratio of the microcapsules of less than 2.5μm was slightly higher than the agitated Example 1 in the sonicated Example 2, but there was no significant difference between them.

On the other hand, in the investigation of pH resistance, there was no difference between the preparation methods in pH2 PBS, but the capsule was slightly larger than dH2O, which was determined to increase the adhesiveness between capsules and thus the size of the capsule by fusion.

In addition, at pH 8 the capsules became significantly unstable with both treatments, thus increasing the bursting of the capsules. In particular, the instability of the microcapsules prepared by sonication was further increased, and the ratio of the microcapsules was reduced to 40% compared to 92% of the stirring treatment.

Therefore, it is inferred that the coenzyme Q10 microcapsules prepared by sonication are somewhat stable in pH 2, that is, gastric acid, but significantly destroyed in pH 8, the small intestine environment. It can be effectively delivered to my target site, that is, the small intestine.

In addition, the coenzyme Q10 powder of Example 3 prepared by spray drying was 96.8% of microcapsules less than 2,5 μm, and these microcapsules showed resistance at pH 2 and pH 8, accounting for 96.3% and 94.3%, respectively. It was. On the other hand, the crystalline form was somewhat seen in the capsule form at pH 8, which is considered to reflect the instability of some capsules.

In addition, in the case of Example 4, the PVP coated microcapsules showed high stability at both pH 2 and pH 8, therefore, in order to keep the microcapsules of coenzyme Q10 stable and further increase the stability of the product, PVP coating is an effective method. Judging.

TABLE 1

<Example 5 and Example 10> Preparation of powder microcapsules

Example 5 was mixed in the edible oil and fat so that the concentration of coenzyme Q10 is 100% by weight, and then mixed with the same amount of the wall material to produce a liquid microcapsule by sonicating a solution of coenzyme Q10 with a terminal concentration of 50% by weight.

Example 6 and Example 7 was used to recover the powder microcapsules in the A chamber and B cyclone using the liquid microcapsules prepared in Example 5 using a spray dryer (micro-engineering).

As a result, in the electron micrograph (x400) of the liquid microcapsules (a) and the powder microcapsules (b, c) as shown in FIGS. It can be seen that the polymer is formed, while the microcapsules of B cyclone (c) are somewhat uniform and less than the liquid microcapsules.

In addition, Example 8 was mixed with edible oil so that the concentration of coenzyme Q10 is 100% by weight, and then mixed with twice the wall material to prepare a liquid microcapsule by sonicating the solution of coenzyme Q10 with a terminal concentration of 25% by weight. .

In Example 9 and Example 10, the liquid microcapsules prepared in Example 8 were recovered by powder microcapsules using a micro-engineering spray dryer.

As a result, as shown in FIGS. 8A to 8C, the microcapsules of B cyclone (c) and the microcapsules of liquid microcapsules (x400) in the electron micrographs (x400) of the liquid microcapsules (a) and the powder microcapsules (b, c) and The microcapsules of the A chamber (b) tended to be somewhat large.

In this case, a large amount of soluble edible oils and wall materials were used, compared to the core material with a coenzyme qtene content of 25% by weight, and in particular, it is believed that the microcapsules were expanded in the aqueous solution due to the increase in the amount of water-soluble walls.

<Experimental example 2> Content stock of coenzyme kyuten

The particle size of the powder collected during the preparation of the powder microcapsules using the spray dryer in the above embodiment was investigated using a particle size analyzer. It was like

Therefore, as shown in Table 2, the number and ratio of microcapsules were similar in samples repeatedly collected, and in particular, the ratio of microcapsules having 1 μm or less was high as 91.6%.

TABLE 2

In addition, the distribution according to the size of the microcapsules in the sample collected when preparing the powder containing 25% by weight of coenzyme Q10 was as shown in Table 3.

Therefore, as shown in Table 3, the number and ratio of microcapsules were similar in the samples repeatedly collected, and especially the ratio of microcapsules of 1 μm or less was high as 87.4%, and the use amount of wall material was 50% by weight of coenzyme Q10 with relatively low amount. Although there are fewer nanometer-sized microcapsules than in powders, the morphology of the powder is considered very soft and advantageous to intake and manufacturing.

TABLE 3

As described above, the preparation method of the microcapsules according to the present invention can enhance the in vitro storage of coenzyme Q10 which is excellent in physiological activity as an antioxidant but is poorly soluble, and can be efficiently delivered to a target organ in vivo, in particular, poorly soluble. In order to increase the digestive absorption efficiency of the coenzyme Q10, merchants make it into a liquid phase, and furthermore, it has the advantage of using natural food material as a wall material for lowering production cost and reconstructing the stability of the product.

In particular, in order to minimize the denaturation due to gastric acid to produce an acid-resistant capsule, and can increase the content of coenzyme Q10 to 5, 25, 50% by weight depending on the purpose of prevention or treatment can be very useful.

Claims (7)

Dissolving coenzyme quene in at least one or more edible oils selected from the group consisting of soybean oil, perilla oil, pine oil and olive oil to prepare a coenzyme quene solution; One or more sugars selected from the group consisting of maltodextrin, cyclodextrin and modified starch; Flour extract; Milk protein; And mixing the gums to produce a wall material; And Method for producing a liquid microcapsule comprising the step of mixing the coenzyme Q10 solution and the wall material and stirring or sonicating to precipitate the microcapsules. The method of claim 1, wherein the stirring is performed for 30 seconds to 30 minutes. The method of claim 1, wherein the ultrasonic wave is treated for 30 seconds to 3 minutes. The method of claim 1, wherein the wall material is mixed in an amount of 1 to 10 parts by weight based on 1 part by weight of the coenzyme Q10 solution. delete Dissolving coenzyme quene in at least one or more edible oils selected from the group consisting of soybean oil, perilla oil, pine oil and olive oil to prepare a coenzyme quene solution; One or more sugars selected from the group consisting of maltodextrin, cyclodextrin and modified starch; Flour extract; Milk protein; And mixing the gums to produce a wall material; Mixing the coenzyme quene solution with the wall material and stirring or sonicating to precipitate liquid microcapsules; And Spray drying the liquid microcapsules to produce a microcapsule powder. The method of claim 6, further comprising the step of treating polyvinylpyrrolidone after the spray drying.

Images