JPH10203965A - Production of covered preparation - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a simple method for producing a covered preparation of hydrophilic material such as L-ascorbic acid and other organic acids, having sufficient coverage. SOLUTION: This method for producing a covered preparation by covering the periphery of a hydrophilic core material with plural layers of a hydrophobic and thermally melting covering material comprises successively or separately adding the heated and melted covering material to the core material while stirring the core material at a temperature lower than a solidifying temperature of the covering material and solidifying the molten covering material to form plural covering material layers around the periphery of the core material.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing a coated preparation, and more particularly, to a method in which a useful hydrophilic substance, in particular, an organic substance such as an organic acid or a salt thereof is used as a core, and the surface of the core substance is formed by a plurality of methods. The present invention relates to a method for producing a stable coated preparation in which physical properties of the core substance are improved by reducing the external influence or the external influence on the core substance by coating the layer with a hydrophobic substance.

[0002]

2. Description of the Related Art Organic acids such as citric acid, fumaric acid and sorbic acid are widely used as sour agents, pH regulators, and for storage purposes. In addition, adverse effects due to low pH are often observed. In addition, L-ascorbic acid is widely used in various foods, health foods, feeds, pharmaceuticals, etc., such as use as a quality improving agent, use as a sour agent, use as a nutrient enhancer as vitamin C, use as a medicine, and the like. It is used. L
-The use of ascorbic acid as a quality improving agent is an application that effectively utilizes the oxidation / reduction ability in expectation of reactivity, but has a disadvantage that the reaction rate is too fast and the effect does not last for a long time. On the other hand, in the use as a fortifying agent, it is desirable that food and the like are stably maintained during processing and storage, but in a system where water, oxygen, metal salts, and the like coexist, it is difficult to stably maintain the system. Not only does the expected function not be exerted, but also in some cases, it has the disadvantage of adversely affecting other components due to oxidation and reduction reactions. Therefore, as one method of solving such a problem, conventionally, a method in which these organic acids are used as a core and the surface thereof is coated with a hydrophobic substance, for example, a fine powder of an organic acid is solidified at room temperature. A method to control the reactivity by preventing the contact with water, oxygen, etc. by wrapping it with a spray cooling method, a spray coating method, a method of spin-mixing and drying, etc., using a coating material such as a hot-melt oil or fat Have been.

[0003]

As such a method, oils and fats as a coating substance are brought into contact with and impinged on a core substance such as a powder of water-soluble vitamins or organic acids, and the coating substance is attached to the core substance. A method of obtaining a coated preparation by coating (JP-A-63-164863, JP-A-63-164864,
JP-A-63-258813), a method of mixing finely divided organic acids and molten fats and oils at a high temperature and spray cooling to obtain a fine powder formulation (JP-A-55-92661, JP-A-62-18).
No. 152, JP-A-64-3118, JP-A-64-31
No. 19), a method of dissolving fats and oils in a solvent and coating the surface of the organic acid while scattering the solvent with a fluidized bed apparatus (Japanese Patent Laid-Open No. 50-52221). Limited diameter, insufficient coverage, inability to manufacture high oil / fat coated products, poor workability, special equipment required, not suitable for manufacturing mononuclear particle products, not suitable for mass production, high price, etc. There is a problem. An object of the present invention is to improve such a problem.

[0004]

According to the study of the present inventors, the problems in the above-mentioned conventional method are that the uniform and thick coating cannot be easily formed, and the difficulty in the production makes it difficult to use the core material as a core material. It is caused by difficulty in controlling the reactivity of organic acids and the like and the dissolution rate from the coated preparation. Therefore, the present inventors have intensively studied to develop a coated preparation capable of freely controlling the reactivity and the dissolution rate by a simple production method. As a result, the fats and oils and / or waxes heated and melted are continuously or dividedly added to the L-ascorbic acid whose temperature has been adjusted in the stirring mixer, and the addition and solidification are repeated to deposit the fats and oils on the surface of the core material. When coated, a plurality of fat-coated preparations with a high fat content, a thick coating layer and mononuclear particles were formed, and it was found that this preparation could be applied to other hydrophilic core substances, and the present invention was completed.

That is, the present invention relates to a method for producing a preparation in which a hydrophilic core material is coated with a plurality of layers of a hydrophobic heat-meltable coating material, the core material is treated at a temperature lower than the solidification temperature of the coating material. A method for producing a coated preparation characterized by solidifying while adding a coating substance heated and melted continuously or dividedly while mixing to form a plurality of coating substance layers around a core substance. It is. According to the present invention, the coating material and its coating amount, that is, the number of layers of the coating material, the addition rate is appropriately selected, by appropriately controlling the temperature,
It is possible to easily obtain a coated preparation of a hydrophilic core substance having excellent stability with controlled water elution property and controlled by the influence of external oxygen, enzymes, metals and the like or the external influence.

[0006]

DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, the core substance is not particularly limited as long as it is a hydrophilic substance having an appropriate particle size. For example, citric acid, fumaric acid, tartaric acid,
Water-soluble vitamins such as sorbic acid, L-ascorbic acid, nicotinic acid, pantothenic acid, amino acids, nucleic acids or their alkali metal salts (eg, potassium salt, sodium salt, etc.), alkaline earth metal salts (eg, , Calcium salts, magnesium salts, etc.), water-soluble non-organic acid vitamins such as vitamin B group, and sugars such as glucose and sucrose. These usually have an average particle size of 2000 μm or less,
It is preferably used in the form of a powder, granulated product or crystal having a size of 40 to 1000 μm.

As the coating substance, a hydrophobic heat-meltable substance is used, and as such a substance, the melting point is 50 to 90.
C., preferably about 60-80.degree. C., for example, vegetable and animal fats and oils, hydrogenation, fractionation, transesterification fats, fatty acids, fatty acid esters, vegetable and animals. And mineral natural waxes. Specific examples of fats and oils include, for example, hydrogenated soybean oil, hydrogenated beef tallow, hydrogenated rapeseed oil, hydrogenated fish oil, hydrogenated whale oil, hydrogenated castor oil, hydrogenated safflower oil, hydrogenated safflower oil, and the like. As a specific example of the fatty acid, a fatty acid having 14 to 28 carbon atoms and a melting point of about 50 to 90 ° C. (eg, palmitic acid, stearic acid, behenic acid, etc.)
Glycerin esters, sucrose esters, sorbitol esters, and glycerol esters having an action as a surfactant;
Propylene glycol esters and the like can also be used.

[0008] Specific examples of waxes include edible natural waxes such as candelilla wax, rice wax, carnauba wax, beeswax, and paraffin wax. In the present invention, these coating substances may be used alone or in combination of two or more. Further, a plurality of layers of the same coating substance may be formed, and depending on the combination of the coating substances, layers of different coating substances may be formed in combination. The coating material is used in an amount of 1 to 9 parts by weight based on 99 to 1 part by weight of the core substance, preferably 95 to 20 parts by weight, more preferably 90 to 40 parts by weight.
9 parts by weight, preferably 5 to 80 parts by weight, more preferably 10 to 60 parts by weight. If the amount of coating material is too small, the coating will be insufficient. The amount of coating material is selected such that it is coated with at least two or more coating materials. By providing a plurality of coating layers, a sufficient degree of coverage can be obtained, and a coated preparation of mononuclear particles having a thick coating layer with a high fat content can be obtained.

[0009] The production method of the present invention is carried out using a stirring and mixing device capable of adjusting the temperature. Such a device may be any device that can stir and mix the core material and the coating material, and is not particularly limited, but a screw type, a ribbon type, a paddle type, a high-speed flow type, and a rotating disk type capable of adjusting the temperature. It is preferable to use a stirring mixer such as the above because of easiness of operation and efficiency. For example, a stirring and mixing device such as a micro speed mixer (Takara Kogyo), a high speed mixer (Fukae Kogyo), a Nauta mixer and the like can be used. In order to carry out the production method of the present invention, for example, the core material is heated to a temperature equal to or lower than the solidification temperature of the coating material by using the above mixer, and the coating material heated and melted is continuously or divided into the core material. After solidification and addition are repeated while preventing binding of particles, the surface of the core material is uniformly coated with oils and fats etc. in a multi-layered or spiral shape, and then cooled.

The production method of the present invention is particularly suitable for producing a coated preparation of L-ascorbic acid. For example, powdered, granulated or crystalline L-ascorbic acid having a particle diameter of 2000 μm or less can be used. 100 parts by weight of the coating material is mixed at a temperature not higher than the solidification temperature of the coating material, for example, 40 to 70 ° C., and the heated and melted coating material is continuously or divided and added in an amount of 1 to 10000 parts by weight. By repeating the solidification, an L-ascorbic acid-coated preparation in which a coating substance is multi-layered on the surface of L-ascorbic acid is obtained.

Thus, according to the production method of the present invention, a hydrophilic core substance can be coated by a simple method using only a stirring and mixing apparatus, and a multi-layer, thick coating layer, which has conventionally been difficult. There is an advantage that a preparation in which mononuclear particles are coated with a hydrophobic coating substance can be produced. The resulting coated formulation is
In the fields of medicine, food, feed, etc., depending on the intended use of the core substance, stabilization of the unstable core substance, water elution rate of the core substance, adjustment of reactivity (sustained release), flavor of the core substance It can be used for release control (prevention of release of acidity and odor). For example, it is possible to prevent the adverse effect of the low pH of the organic acid and the instability of L-ascorbic acid due to water, oxygen, metals and the like, and also to prevent the influence of L-ascorbic acid on other components. Can be. It can also be used for sustained release of taste components in chewing gum and the like.

[0012]

The present invention will be described in more detail with reference to the following Examples, Comparative Examples and Use Examples, but the present invention is not limited thereto. Example 1 500 g of L-ascorbic acid (average particle size: 350 μm) was charged into a jacketed high-speed fluid mixer (high-speed mixer LSF-2, manufactured by Fukae Kogyo Co., Ltd.), and heated to 60 ° C. while stirring. Hold and continue stirring. Under stirring, 100 g of a heated melt of soy hardened oil (melting point 68 ° C.) prepared separately is divided into two portions, and 50 g of one of the fats and oils is added and uniformly coated. After the addition and coating, the product was cooled to a product temperature of 40 ° C. to obtain a fat-coated preparation of L-ascorbic acid. Comparative Example 1 The same procedure as in Example 1 was repeated except that the molten fat was not divided into two parts, to thereby obtain a L-ascorbic acid-coated preparation by adding the molten fat at once.

As a result of comparing the appearance of the oil / fat coated preparation obtained in Example 1 and the oil / fat comparative preparation obtained in Comparative Example 1 and the water elution rate of L-ascorbic acid, the coated product of Comparative Example 1 was 0.5 cm in diameter. A large number of the above aggregates occurred, and the number of fine-grained products was slight, whereas the coated product of Example 1 had a small amount of clumps and about 90% of the fine-grained products having a diameter of 500 μm or less. Further, regarding the fine-grain fraction of the coated articles of Comparative Example 1 and Example 1,
When the water elution rate of L-ascorbic acid was compared, the comparative product eluted in about 2 minutes, whereas the coated product of the example was about 40 minutes, which was a remarkable coating effect. That is, as in Comparative Example 1, when they are added simultaneously, they do not become mononuclear particles, cannot be coated in a large amount, and cannot delay the dissolution rate.

Example 2 500 g of L-ascorbic acid (average particle size: 120 μm) was charged into a jacketed high-speed fluid mixer (high-speed mixer LSF-2, manufactured by Fukae Kogyo) and heated to 50 ° C. with stirring. Stirring was continued. Then, under stirring, a heated melt 200 of hardened soybean oil (melting point 68 ° C) prepared separately was added.
g was continuously added at a rate of 10 g / min and uniformly coated, and then cooled to a product temperature of 40 ° C. to obtain an L-ascorbic acid-coated preparation. This product was hardly agglomerated and was a fine-grained product having an average particle size of 155 μm.

Example 3 10 kg of L-ascorbic acid (average particle diameter 350 μm) was charged into a jacketed high-speed flow mixer (Microspeed mixer MS25, manufactured by Takara Koki), heated to 50 ° C. while stirring, and stirred. Continued. 5 kg of a heated melt of rapeseed oil (melting point 68 ° C) prepared under stirring
Was added continuously at a rate of 300 g / min to coat uniformly, and then cooled to a product temperature of 40 ° C. to obtain a fat-coated formulation of L-ascorbic acid.

Example 4 500 g of L-ascorbic acid (average particle size: 350 μm) and 50 g of hardened soybean oil were mixed with a high-speed fluidized mixer equipped with a jacket (high-speed mixer LSF-2, manufactured by Fukae Kogyo).
The mixture was heated to 70 ° C. while stirring to melt the hardened soybean oil, and then stirring was continued. This is stirred at 50 ° C.
And solidify (primary coating), then harden soybean oil 5
A mixed melt of 0 g and 10 g of glycerin fatty acid ester (Emulgy MS, RIKEN Vitamin) is added and solidified (2
Then, the mixture was cooled at 20 ° C. to obtain a two-layer oil-fat coating formulation of L-ascorbic acid.

Example 5 500 g of anhydrous citric acid (average particle size of 550 μm) was mixed with a jacketed high-speed fluid mixer (High Speed Mixer LS).
F-2 type, manufactured by Fukae Kogyo Co., Ltd.)
And continued stirring. To this, while stirring, 500 g of a heated melt of separately prepared soybean hardened oil (melting point 68 ° C.)
After adding continuously at a rate of 3 g / min and coating uniformly,
The product was cooled to a product temperature of 40 ° C. to obtain a fat-coated preparation of citric acid.

Use Example 1 The oil- and fat-coated preparation of L-ascorbic acid obtained in Example 1 was filled in hard capsules of gelatin and stored at 40 ° C. for one week.
The capsules filled with ascorbic acid turned brown, while those filled with the oil-coated preparation did not change color at all. Use Example 2 The oil / fat coating formulation of L-ascorbic acid obtained in Example 3 was blended with a feed material for shrimp cultivation, added with water, molded and stored as a moist pellet product. L-ascorbic acid, which was not used, decomposed in a short period of time during production and storage, whereas that using an oil-coated preparation remained for a long period of time. Use Example 3 When chewing gum containing 1% of the oil-coated preparation of citric acid obtained in Example 5 was chewed, the control chewing gum using citric acid not coated with oil had a strong acidity at first, and during chewing. While the acidity weakened in a short time, the chewing gum containing the oil / fat coating preparation showed little change in the acidity during mastication and lasted for a long time.

[0019]

As described above, according to the present invention,
A hydrophilic core substance, such as an organic acid, can be multi-layer coated with a large amount of a coating substance using only a stirring / mixing device capable of adjusting the temperature, and the elution of the core substance is small even when immersed in water. In addition, improvement of the stability of the core material, prevention of reduction in flavor, and the like can be expected effectively.

Claims (7)

[Claims] In producing a preparation in which a hydrophilic core material is coated with a plurality of layers of a hydrophobic heat-meltable coating material, the core material is mixed at a temperature equal to or lower than the solidification temperature of the coating material. A method for producing a coated preparation, characterized by solidifying while continuously or separately adding a coating material that has been heated and melted to form a plurality of coating material layers around a core material. 2. The method according to claim 1, wherein the core substance is an organic substance selected from the group consisting of organic acids, organic acid salts, non-organic acid vitamins and saccharides. 3. The method according to claim 2, wherein the core substance is L-ascorbic acid. 4. The method according to claim 1, wherein the coating substance is selected from the group consisting of fats and oils, fatty acids, fatty acid esters and waxes. 5. The method according to claim 1, wherein a plurality of layers of the same coating substance are formed. 6. The method according to claim 1, wherein layers of different coating materials are formed. 7. The method according to claim 1, wherein the coating is performed using a stirring and mixing device capable of adjusting the temperature.