JPH05221859A - Vitamin c granule - Google Patents

Abstract

PURPOSE:To provide the coated granule obtained by laminating specific protecting coat layers on a vitamin C core in a specified order and preventing the deterioration of the vitamin C contained therein even at a high temperature and at a high humidity. CONSTITUTION:The layer of fats and oils, the filmy layer of an edible material (e.g. corn protein, dammar resin, rosin, shellac), and the second layer of fats and oils are successively laminated to the surface of a core prepared from the crystal, powder or granule of vitamin C to provide the coated vitamin granule. The fats and oils used for the layer of the fats and oils include various fats and oils originated from animals and plants, and the first layer of the fats and oils is formed at a granule temperature of 45-60 deg.C and the temperature of the fats and oils of 80-170 deg.C, and the second layer of the fats and oils is also formed at a granule temperature of 40-60 deg.C and the temperature of the fats and oils of 120-170 deg.C, while using a sugar-coating pan. If necessary, the layer of powder such as albumen powder, fatty acid calcium salt powder or talc powder may further disposed on the first layer of the fats and the oils.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a vitamin C (hereinafter simply referred to as VC) granule and a method for producing the same, and in particular a coating which prevents deterioration of VC contained therein even at high temperature and high humidity. Regarding VC granules.

[0002]

2. Description of the Related Art In the field of livestock feed, various nutritional sources such as vitamins, minerals, amino acids, etc., and additives for improving palatability, such as sweeteners, have been used in recent years.
Mixed feeds containing flavors and the like have come to be produced, and for this purpose, vitamins and the like are added to the feeds to produce premixed products. Attempts have been made so far to mix VC in the production of such a compounded feed, but if it is mixed in the feed to make a premix, the potency as VC will be lost in a short time. Is known, and attempts to stably incorporate VC into feed as a premix have not yet been successful.

VC is also used by itself as a pharmaceutical agent for mammals including humans, but it is widely known that its potency is rapidly reduced depending on the preservation state in pharmaceutical applications.

The conventional stable VC production method is as follows.
A method of mixing lecithin and glycerin ester with VC (JP-B-56-16779), or a method of mixing oil and fat and sucrose fatty acid ester with VC (JP-B-57-4).
8050) and a method of spraying dissolved fats and oils on VC to coat them (Japanese Patent Laid-Open No. 64-3119), but these methods cannot be said to have completely covered VC.

[0005]

Therefore, when the premix is prepared by incorporating VC into the feed, the V
When C is used for pharmaceutical use in mammals including humans and other uses, it is required to establish means for stably storing VC for a long time.

[0006]

[Means for Solving the Problems] The inventors of the present invention are one of the reasons why VC mixed in feed or the like rapidly deteriorates and loses its potency.
One of them is the moisture that inevitably accompanies the feed, so we have conducted a diligent study based on the idea that VC stability can be improved by molding the VC into a form that is not affected by this moisture. As a result, they have found that when the VC is subjected to a multi-step coating process in a specific order, the VC granules having extremely high stability are obtained, and the present invention has been completed.

That is, the present invention relates to a VC core, and a VC granule having an oil and fat layer, a film layer of an edible material and a final oil and fat layer which are sequentially laminated on the surface of the VC. ..

The VC granules of the present invention are prepared by the following steps: (1) VC crystals, powders or granules are prepared as a core, and (2) a first oil coating is applied on the surface of the core, 3) A film coating is applied to the first oil / fat coated material with an edible material, and (4) An oil / fat coating is applied to the film coated material.

It can be obtained by performing the steps (1) to (4) in this order, or by repeating the steps (2) and (3) before the step (4).

Further, according to the present invention, in which the powder coating can be applied before the film coating of the edible material, according to the present invention, VC granules having extremely enhanced stability can be obtained by performing the above steps in that order. Obtainable. The VC granules of this VC granule are stable and less likely to deteriorate even under the conditions of high humidity and high temperature. Therefore, it is useful as a VC compounding agent when, for example, VC is mixed in feed. Besides, it is also preferable for use as a VC agent for medicine.

The VC granules according to the present invention are
Since it can be obtained only by laminating a specific protective coat layer on the core body in a specific order, the method for producing the VC granules is also included in the present invention.

The first step for the preparation of the protective coated VC granules of the present invention is the crystal of VC as a core,
To prepare powder or granules. In order to apply the protective coat uniformly and without defects to the surface of the core body, it is preferable to prepare a spherical or substantially spherical core body.

The spherical core is prepared by molding from VC crystals and VC powder using a known spherical granule molding machine. For example, VC crystal (42-83
A mesh (passed by Japan Pharmacopoeia XI amendment) or a VC powder (passed by 330 mesh) is granulated in a centrifugal fluidizing type granulator to obtain spherical granules of about 22 to 42 mesh. In this case, granulation may be performed in two steps. Of course, any of the known equipment and processes capable of preparing spherical granules can be used.

A first oil / fat coat is applied to the surface of the VC core body thus prepared. The fats and oils used for this fat and oil layer include various fats and oils of animal and vegetable origin, such as beef tallow, lard, sheep fat, soybean oil, rapeseed oil, sesame oil, cottonseed oil, olive oil, peanut oil, linseed oil. , Hardened oils such as herring oil; balmitic acid, stearic acid, myristic acid, het, borneo fat, and the like. Glycerin monofatty acid ester (for example, stearic acid monoglyceride, oleic acid monoglyceride), glycerin difatty acid ester, glycerin trifatty acid ester, sorbitan fatty acid ester, sucrose fatty acid ester, beeswax, paraffin, candelilla wax, carnauba wax and the like are further added to these oils and fats. It can also be used.

In the step of applying the first oil / fat coating, for example, to a crystal, powder or granulated VC core, the oil / fat is heated from a core temperature of about 40 ° C. to a temperature lower than the melting point of VC, preferably. About 45 to about 60 ° C., and oil temperature about 60 to
It is carried out in such a manner as to coat at about 175 ° C, preferably about 80 to about 170 ° C. The device used is a sugar-coated bread, but other devices can be used.

The oil-fat-coated core body is then subjected to powder coating, if desired. The powder used for this powder coating includes egg white powder, fatty acid calcium, talc, carnauba wax and the like.

The step of applying the powder coating is carried out, for example, in the centrifugal fluidizing device using the egg white powder, the fatty acid calcium powder and the egg white aqueous solution for the first oil and fat coated product. Of course, other devices can also be used as far as powder coating is possible. After this powder coating, the powder-coated VC granules are obtained by drying at room temperature to about 60 ° C., preferably at about 30 to about 45 ° C.

The particles of VC thus powder-coated or the particles of VC only coated with the first oil / fat and not powder-coated are then subjected to film coating. Examples of the material used for this film coat include corn protein (Twain), dammar resin, thunderac resin, ester gum, rosin and shellac, and known coating materials used for pharmaceuticals can also be used.

The step of applying the film coat is carried out, for example, by the VC coated with the oil and fat and the powder.
The particles or the VC particles coated only with the fat and oil are treated in a centrifugal fluidizer using a zein solution or a shellac alcohol solution.

The VC particles thus coated with the film are finally subjected to the second fat coating.

Examples of the oil and fat used for the second oil and fat coating include those similar to those used for the first oil and fat coating.

In the step of applying the second oil and fat coating, for example, the VC particles coated with the above-mentioned film are treated with oil and fat at a particle temperature of about 40 to about 60 ° C. and an oil and fat temperature of about 60 to about 1.
It is carried out at 50 ° C., preferably about 120 to about 150 ° C., in such a way as to coat in a sugar-coated pan.

The aggregate thus obtained was cut with an 18-mesh sieve to obtain VC spherical particles having a protective coat. Next, specific examples of production of VC granules of the present invention will be shown by Examples.

Example 1 Granulation Step A centrifugal fluidized granulator was set to a rotor rotation speed of 150 rpm and slit air of 220 liters / minute, and 1000 g of pre-weighed VC crystal (42 to 83 mesh) was charged into the can body. Then, granulation was started at a spray air pressure of 1.0 kg / cm ² , a spray air flow rate of 15 l / min, and a spray liquid amount of 5 ml / min. At first, a binder (0.9% pullulan solution) was sprayed for 1 minute, and when VC became wet, a small amount (about 20 g / min) of VC (fine powder) was added by a spatula to perform granulation. The rotor rotation speed (maximum 300 rpm), binder spray liquid amount, VC (fine powder) input amount, etc. were adjusted appropriately while observing the state inside the can, and the primary granulation was completed in a granulation time of about 50 minutes. The amount of VC (fine powder) used in the primary granulation is 1000 g, and the amount of binder used is 200 g.
Met.

The granulated product was placed in a hopper and dried in a fluid dryer for 30 minutes at a suction temperature of 40 ° C. and a damper opening of 4. After the completion of drying, the product was passed through a 30-mesh sieve and the passed product was subjected to secondary granulation. For secondary granulation, the operation of primary granulation was repeated.

First oil and fat coating step 1000 g of the secondary granulated product was weighed and the product temperature was 45 ° C to 5 ° C.
The mixture was warmed to about 0 ° C., put into a sugar-coated bread, and the bread was slowly rotated (12 rpm). Next, soybean hydrogenated oil 9
5 g and glycerin monofatty acid ester 5 g 150
Melt at ℃ 2 into a rotating pan 2 to 3 times
This process was completed in about 50 minutes while being naturally cooled (45 ° C.). Only aggregates were cut with an 18-mesh sieve, and the passed product was used in the next step.

Powder coating step Using the above centrifugal fluidized granulation apparatus, the above oil and fat coated finished product 5
Using 00g as the core and 5% egg white aqueous solution as a binder,
A mixed powder of 150 g of dried egg white and 150 g of calcium fatty acid was coated. The operating conditions were the same as in the case of the primary and secondary granulation steps, but the amount of spray liquid was 4 ml / min because the viscosity of the binder was large. After finishing the powder mixing, coat with 50g of fatty acid calcium and add 1 rotor to adjust the surface.
I rotated it for about a minute. The amount of binder used is 270g,
The granulation time was about 60 minutes.

Next, the granulated product was dried in a fluidized dryer at room temperature for 10 minutes, at 50 ° C. for 40 minutes, and again at room temperature for 10 minutes.
Since aggregates were formed, they were cut with an 18-mesh sieve and the passed product was used in the next step.

Film-coating step 850 g of the product passed through the 18-mesh sieve in the previous step was added to a 2.5% zein solution (34 g of zein was mixed with 85% ethanol 1326).
which was used after being dissolved in 1 g) was coated with 4%. The product passed through the 18-mesh sieve is put into a fluidized granulator, and when the product temperature reaches 45 ° C., the spray air pressure is 0.8 kg / cm ² , the spray air flow rate is 10 l / min, and the spray liquid amount is 10 ml / min. Started. The number of rotations of the rotor was constant, but the amount of spray liquid was increased / decreased between 5 ml and 10 ml / min. From the middle of the process, talc was applied little by little with a spatula because the particles of the particles adhere to each other to form aggregates. The coat time was about 180 minutes. The product was cut through an 18-mesh sieve and the passed product was used in the next step.

Second oil-fat coating step A mixture of 90 g of soybean hydrogenated oil, 5 g of glycerin monofatty acid ester and 5 g of beeswax was added to 1000 g of the finished product of the previous step under the same conditions as those of the first oil-fat coating step (however, an oil-fat temperature of 130 ° C. Was used). Aggregates were cut with an 18-mesh sieve to obtain the objective VC spherical granules.

Example 2 First Oil and Fat Coating Step 50 kg of VC crystals were weighed, warmed to a product temperature of about 50 ° C., put into a sugar-coated bread, and the bread was slowly rotated (12 rpm). Next, 4.8 kg of soybean hydrogenated oil and 1.2 kg of glycerin monofatty acid ester dissolved at 170 ° C. were put into a rotating pan and allowed to cool naturally (45 ° C.) for about 90 minutes during this step. Ended. The agglomerates were cut and the 18 mesh screen passed product was used in the next step.

Film Coating Step Shellac coating was performed on 50 kg of the granules obtained in the previous step using a 5% shellac solution (prepared by diluting a 15% ethanol solution of shellac with 100% ethanol). That is, the granules were put into a centrifugal fluidized granulator, and when the temperature of the product reached 30 ° C, the spray air pressure was reduced to 0.
Coating was started at 8 kg / cm ² , a spray air flow rate of 40 l / min, and a spray liquid amount of 160 to 220 ml / min. The rotor speed is constant, but the spray amount is 1
Increased and decreased between 60 and 220 ml / min. From the middle of the process, cornstarch was sprinkled little by little on the spatula because the particles stick together and form aggregates. The coating time was 140 minutes. The agglomerates were cut and the 18 mesh screen passed product was used in the next step.

Second oil and fat coating step 50 kg of the finished product of the previous step is put into a sugar-coated bread, and the bread is rotated while rotating at 10 to 12 rpm).
A product (kg, 132 ° C.) in which kg and 2.2 kg of glycerin monofatty acid ester were dissolved was added and coated while naturally cooling. Then, the aggregate was cut with an 18-mesh sieve to obtain the desired product.

Example 3 The first oil and fat coating step and the film coating step described in Example 2 were repeated. Then, the obtained granules 50
Put kg into a sugar-coated pan and rotate the pan (10
~ 12 rpm), a product obtained by dissolving 8.8 kg of soybean hydrogenated oil and 2.2 kg of glycerin monofatty acid ester (product temperature 13
(9 ° C.) was added and coating was performed while cooling naturally. Then, the aggregate was cut with an 18-mesh sieve to obtain the desired product.

Example 4 The first oil and fat coating step and the film coating step described in Example 2 were repeated. Then, the obtained granules 50
Put kg into a sugar-coated pan and rotate the pan (10
~ 12 rpm), a product obtained by dissolving 8.8 kg of soybean hydrogenated oil and 2.2 kg of glycerin monofatty acid ester therein (product temperature 14
(0 ° C.) was added and coating was performed while cooling naturally. Then, the aggregate was cut with an 18-mesh sieve to obtain the desired product.

Comparative Example 1 An 18-mesh sieve-passed product was obtained by repeating only the first fat coating process described in Example 2 above.

Comparative Example 2 An 18-mesh sieve-passed product was obtained by repeating only the first oil and fat coating step and the film coating step described in Example 2.

Next, when the VC granules obtained in Examples 1 and 2 and Comparative Examples 1 and 2 were blended into a feed premix and kept at 40 ° C. and 80% humidity, , VC content was tested as to how it changed over time. The results are shown in Table 1 below.

[0039]

[Table 1]

Next, the above Examples 1 to 4 and Comparative Examples 1 to
The following dissolution test was performed using the VC granules obtained in 2 above to determine the dissolution rate of VC.

Dissolution test (shaking method) 0.1 to 0.3 g of a sample was precisely weighed in a 50 ml centrifuge tube and purified water 3
After adding 0 ml and stoppering, using a reciprocating shaker at room temperature, shaking with an amplitude of 80 mm and a shaking frequency of 150 times / min for 10 minutes and 60 minutes, and then using a small amount of filter paper (No 5A Toyo filter paper) Filtration was performed while washing the inside of the centrifuge tube and the filter paper with purified water, L-alcorbic acid was measured using the filtrate as a sample solution, and the elution rate was determined. This L ascorbic acid is quantified by the Japanese Pharmacopoeia XI amendment "alcorbic acid"
It was carried out according to the method described in the section (C-page 35). The results are shown in Table 2.

[0042]

[Table 2]

Claims (1)

[Claims] 1. Vitamin C granules comprising a vitamin C core, and an oil and fat layer, a film layer of an edible material, and finally an oil and fat layer, which are sequentially laminated on the surface of the core.