JP2019156719A - Method of uniformly dispersing mineral into granulated powder - Google Patents

Abstract

The present invention provides a technique capable of uniformly dispersing minerals in a granulated powder in granulation by a spray drying method or the like.
A granulated base powder, a mineral element inorganic salt or an inorganic acid salt, and a chelating agent are added to an aqueous solvent, mixed and stirred, and the mixture is used as a raw material solution for granulation. A method for dispersing minerals in the granulated powder, wherein a granulated powder having a uniform mineral content is obtained. In particular, a first step in which a granulated base powder is dispersed in an aqueous solvent to form an aqueous dispersion; an inorganic salt or inorganic acid salt of a mineral element is mixed in the aqueous dispersion, and the base powder and the inorganic salt or Second step of preparing a mixed solution in which inorganic acid salt is uniformly dispersed; Third step of adding a chelating agent to the mixed solution and stirring under weakly acidic to weakly alkaline conditions; Granulation using the mixed solution as a raw material solution A method having a fourth step of obtaining a granulated powder having a uniform mineral content by performing
[Selection] Figure 1

Description

  The present invention relates to the technical fields of food production and pharmaceutical preparation, and specifically relates to a technique for producing a supplement or pharmaceutical supplemented with minerals by a granulation method such as spray drying.

The five macronutrients, which are vitamins and minerals added to proteins, lipids and carbohydrates (carbohydrates), which are the three macronutrients, are essential for the maintenance and growth of the body's functions. Among these nutrients, most of the vitamins and minerals, which are micronutrients, cannot be synthesized in vivo and must be taken through food and drink.
Typical mineral elements such as iron, copper, and zinc are contained in trace metal elements whose abundance in the living body is very small (about 1 μg to 100 μg per 1 g body weight), but their essentiality has been recognized. In vivo, it is mainly involved in redox reactions as a conjugate with proteins.
These elements cause anemia, skin disorders, bone dysplasia, etc. due to insufficient intake. If these elements are insufficient, supplement with supplements or preparations based on these ingredients. Has been done. For example, for iron deficiency anemia and iron refractory / copper deficiency anemia, the therapeutic effects of intake of iron preparations and copper-added liquid food have been reported, respectively. In addition, regarding skin disorders, wound healing delays and taste disorders observed at the time of zinc deficiency, the therapeutic effect by ingestion of zinc supplements or preparations has been reported.

Examples of supplements and preparations include powders, granules, tablets (also referred to as tablets or tableting), capsules, and the like, and these are selected in consideration of raw material characteristics and applications.
These are produced from powders or granules prepared by mixing or granulating methods. For example, in the case of powders and granules, the powders and granules can be used as they are. On the other hand, tablets and capsules are agents intended to control release, such as tableting with a sustained release component added to the powders and granules prepared by the above method, and coating with a sustained release film. Manufactured by applying shape treatment.

The mixing method is a method of mixing a plurality of types of powders or granules using a V-type mixer or the like, and powders and granules prepared by this method are generally characterized in that the particle diameter tends to be non-uniform.
On the other hand, the granulation method is a method of improving moldability by processing powder or granules, and is roughly classified into a dry granule compression method and a wet granule compression method.
Dry granule compression methods include compression and fracture granulation methods using a roller compactor, and wet granule compression methods include stirring granulation method, rolling granulation method, extrusion granulation method, fluidized bed granulation method. And spray granulation. These methods are characterized in that the particle diameter and shape (spherical shape) of the prepared powder / granules can be made uniform, and among them, the spray granulation method is most excellent in terms of sample processing speed and fine particle formation.
A spray drying method (spray drying method), which is a typical spray granulation method, is generally a liquid raw material using water, an organic solvent or a mixture thereof as a solvent, or a powder (hereinafter referred to as an excipient) for the liquid raw material. This is a method of collecting a powder produced by spray spraying a mixed solution (solution or suspension) obtained by mixing a base powder) and drying the spray droplets with hot air. Examples of the base powder include starch and cellulose. At present, the spray drying method is used for the production of preparations, battery / electronic component materials, molding materials, and foods for drying, microparticulation, amorphization, agglomeration, or microencapsulation.

  When manufacturing supplements or preparations containing minerals from granulated powder obtained by a granulation method such as spray drying, the amount of minerals to be ingested by the living body is very small. In this case, ensuring the uniformity of the mineral content in the granulated powder becomes an issue. In other words, if the mineral content in the granulated powder is not uniform, the mineral content contained in the prescribed amount of the supplement or preparation tableted or encapsulated as it is, or ingested as it is, is taken. This makes it difficult to supply a small amount of a predetermined amount of mineral components to the living body.

Patent Documents 1 to 5 can be cited as techniques for dispersing the element in the raw material powder by spray drying an aqueous dispersion or slurry obtained by mixing a raw material powder with a compound of a specific element by a spray drying method. For example, in Patent Document 1, one or more compounds of specific elements (magnesium, manganese, strontium, etc.) are mixed in an aqueous dispersion of ceramic raw material powder, and the elements are uniformly dispersed on the powder surface by spray drying. It discloses that a granulated powder is obtained.
However, Patent Document 1 does not describe the case where a powder other than the ceramic raw material powder is used, and does not mention the dispersion state of mineral elements (iron, copper, zinc, etc.) other than magnesium and manganese. In Patent Documents 2 to 5, the desired composite metal oxide sintering is performed by spray-drying an aqueous dispersion or slurry obtained by mixing a raw material powder containing a specific element together with a binder powder as appropriate, and firing it after appropriate pressure molding. Although it is disclosed that a body is obtained, there is no mention of the element dispersion state in the granulated powder obtained by spray drying.

JP 2003-342077 A JP 2002-316052 A JP 2003-300719 A JP 2005-330589 A JP 2009-298655 A

  This invention makes it a subject to provide the new method of disperse | distributing a mineral uniformly to granulated powder in granulation by a spray drying method etc.

As a result of diligent studies to solve the above problems, the inventors of the present invention have made it possible to mix minerals and chelating agents in an aqueous dispersion of a base powder before spray drying in granulation by spray drying. It has been found that a specific mineral can be uniformly dispersed in the powder.
Specifically, the present inventors mixed and stirred an inorganic salt solution of various mineral component metals in an aqueous dispersion of soluble starch powder as a base powder, and added various chelating agents having a carboxyl group to this.・ A mixture was obtained by stirring, and the relative standard deviation (RSD) of the contents of various mineral components was examined for a plurality of granulated powders obtained by spray drying. When using acid salts, RSD was significantly reduced for iron, copper, and zinc compared to when no chelating agent was used, and for copper and zinc, RSD was also decreased for cysteine salts and histidine salts. For copper, RSD is greatly reduced even when malate and tartrate are used, and for other mineral components, the type of chelating agent used Flip RSD is changed, the number of minerals, found that it is possible to reduce the RSD by using appropriate chelator.
The inventors further added a base powder, a mineral component, and a chelating agent to an aqueous solvent, changed the procedure when preparing a mixed solution by mixing and stirring, and the change in the procedure is performed after granulation. The effect of the mineral components in the powder on the dispersion status was examined.
The present invention has been made based on these findings by the present inventors.

The effect produced by adding the above-mentioned chelating agent is that the mineral component is mixed with the base material powder dispersion, and the mineral component is mixed with the base material due to the influence of the chelating agent in the mixed solution obtained by adding the chelating agent. This is considered to be caused by more uniform mixing with the powder.
Therefore, the above-mentioned effect is not limited to the granulated powder granulated by spray drying, but also a granulation method performed using a similar mixed solution, for example, a microencapsulation method by the spray granulation method (for example, the above mixed liquid A microencapsulated granulated powder obtained by a technique of dropping a spray droplet of a film material liquid onto the fixing liquid, or a technique of spraying the mixed liquid as a core material liquid and wrapping with the film material liquid) As well as granulated powders by other wet granulation methods (stirring granulation method, rolling granulation method, extrusion granulation method, fluidized bed granulation method, etc.), as long as the same mixed solution is used, the same It is reasonably expected to be obtained.

That is, this application provides the following invention.
<1> Granulation is performed using a mixed liquid obtained by adding a granulated base powder, an inorganic salt or mineral acid salt of a mineral element, and a chelating agent to a water solvent and mixing and stirring as a raw material solution. A method for dispersing minerals in a granulated powder, characterized in that a granulated powder having a uniform mineral content is obtained.
<2> The first step of dispersing the granulated base powder in an aqueous solvent to obtain an aqueous dispersion, and mixing the inorganic salt or inorganic acid salt of the mineral element in the aqueous dispersion after the completion of the first step, The second step, which is a mixed solution in which the material powder and the inorganic salt or inorganic acid salt are uniformly dispersed, the third step of adding a chelating agent to the mixed solution after completion of the second step and stirring under weakly acidic to weakly alkaline conditions, The granulation according to <1>, characterized by having a fourth step of obtaining a granulated powder having a uniform mineral content by performing granulation using the mixed solution after completion of the third step as a raw material solution. Mineral dispersion method in powder.
<3> Add the inorganic salt or inorganic acid salt of a mineral element and a chelating agent to the aqueous dispersion after the completion of the first process, in which the granulated base powder is dispersed in an aqueous solvent to form an aqueous dispersion. The second step of stirring under weakly acidic to weakly alkaline conditions, the third step of obtaining a granulated powder having a uniform mineral content by granulating using the mixed solution after the completion of the second step as a raw material solution The mineral dispersion method in the granulated powder as described in <1> characterized by having.
<4> The method according to any one of <1> to <3>, wherein the chelating agent is an organic acid salt or amino acid salt having one or more carboxyl groups that act as ligands for metal ions. .
<5> The method according to any one of <1> to <3>, wherein the mineral element is iron, copper, and / or zinc, and the chelating agent is citrate.
<6> The method according to any one of <1> to <3>, wherein the mineral element is copper and / or zinc, and the chelating agent is a cysteine salt or a histidine salt.
<7> The method according to any one of <1> to <3>, wherein the mineral element is copper and the chelating agent is malate or tartrate.
<8> The method according to any one of <1> to <7>, wherein granulation is performed by a spray drying method.

According to the present invention, minerals can be uniformly dispersed in the granulated powder during granulation by spray drying or the like.
As a result, by taking a prescribed amount of supplements or preparations consisting of the granulated powder uniformly containing a minute amount of mineral components or processed into tablets, capsules, etc. using a predetermined amount of this, a minute amount is prescribed. The amount of mineral components can be taken accurately and easily.

The schematic diagram of the spray dryer used for the granulation of this invention in the Example.

The present invention adds granulated base powder, mineral element inorganic salt or inorganic acid salt and a chelating agent to an aqueous solvent, and mixes and agitates the mixture to obtain a granulation. It is intended to obtain a method for dispersing minerals in the granulated powder, which is characterized by obtaining a granulated powder having a uniform mineral content.
As shown in Examples described later, the present inventors have confirmed the effects of the present invention with respect to several aspects in which the preparation procedure of the above mixed liquid that becomes a raw material solution for granulation is different.
Hereinafter, the mineral dispersion | distribution method to the granulated powder of this invention is demonstrated in detail for every specific aspect.

The 1st aspect of this invention can be divided and demonstrated to the following 4th processes from the 1st process.
The first step is a step of dispersing the granulated base powder in an aqueous solvent to obtain an aqueous dispersion.
Examples of the base powder include starch, soluble starch, saccharides (malt sugar, lactose, etc.), sugar alcohols (reduced malt sugar, sorbitol, etc.), cellulose, and derivatives thereof, and soluble starch is preferred. The soluble starch is obtained by reducing the degree of polymerization from starch, which is a polymer of α-glucose, and a commercially available soluble starch (also called soluble starch or starch (soluble)) can be used.
The additive concentration of the base powder is preferably about 4% by mass final concentration. In the first step, there is no problem even if the base powder is not uniformly dispersed in the aqueous dispersion.

In the second step of the above aspect of the present invention, the inorganic dispersion or inorganic acid salt of the mineral element is mixed in the aqueous dispersion after completion of the first step, and the base powder and the inorganic salt or inorganic acid salt are uniformly dispersed. It is the process of making a liquid.
As the mineral element, trace metal elements such as iron, copper, and zinc are suitable. As the inorganic salt or inorganic acid salt, an inorganic metal salt that generates ions (monovalent to trivalent cations or oxoanions) of the trace metal element in an aqueous solution is preferable.
As the additive concentration of the inorganic salt or inorganic acid salt, the final concentration as an element is preferably about 10 μg / L to 670 μg / L.
A magnetic stirrer can be used for stirring to uniformly disperse the base powder and the inorganic salt or inorganic acid salt.

The 3rd process of the said aspect of this invention is a process of adding a chelating agent to the liquid mixture after completion | finish of a 2nd process, and stirring on weakly acidic-weakly alkaline conditions.
As the chelating agent, an organic acid salt or amino acid salt having one or more carboxyl groups (COOH groups) acting as ligands for metal ions is preferable. Specifically, citrate, malate and tartrate, which are edible organic acid salts that can be used as food additives, and cysteine salt and histidine salt, which are edible amino acid salts, can be used, more preferably Citrate.
As the addition concentration, a final concentration of about 0.8% by mass is preferable. The pH of the mixed solution after addition of the chelating agent is preferably 3.0 or more and 9.0 or less, and the stirring time of the mixed solution under the pH condition is preferably about 1 hour.

The 4th process of the said aspect of this invention is a process of granulating using the liquid mixture after completion | finish of a 3rd process as a raw material solution, and obtaining the granulated powder with a uniform mineral content.
As the granulation method, for example, a spray drying method can be used. As the spray dryer used for spray drying, a lab scale spray dryer having a water evaporation capacity of 0.5 kg / h to 1.0 kg / h and a sample processing speed of 100 mL / h to 600 mL / h is suitable. As the spray nozzle, a two-fluid nozzle having a nozzle hole diameter of 0.7 mm and a supply gas flow rate of 200 L / h to 1000 L / h is suitable. As the drying tower temperature during the spray drying, an inlet temperature of 190 ° C and an outlet temperature of 90 ° C to 100 ° C are preferable. Moreover, as an average particle diameter of the granulated powder obtained, 2 micrometers-25 micrometers are preferable. Here, the average particle size can be measured by a laser diffraction particle size distribution measuring device such as Aerotrack LDSA-SPR (manufactured by Nikkiso Co., Ltd.).
In addition, since the granulated powder obtained by this spray drying is amorphized in the spray drying process, it is excellent in solubility in water as compared with the base powder.

The 2nd aspect of this invention can be divided and demonstrated to the following 3rd processes from the 1st process.
The first step of this embodiment is a step of dispersing the granulated base powder in an aqueous solvent to obtain an aqueous dispersion, as in the first embodiment.
The kind of base powder to be used, the addition concentration, etc. are the same as in the first embodiment.
The second step of this embodiment is a step of adding an inorganic salt or inorganic acid salt of a mineral element and a chelating agent to the aqueous dispersion after completion of the first step, and stirring under weakly acidic to weakly alkaline conditions.
The kind and addition amount of the inorganic salt or inorganic acid salt of the mineral element to be used, and the kind and addition amount of the chelating agent are the same as in the first embodiment.
The inorganic salt or inorganic acid salt of the mineral element and the chelating agent may be added simultaneously to the aqueous dispersion after completion of the first step, or may be added sequentially. When adding sequentially, the aqueous dispersion is mixed when the inorganic salt or inorganic acid salt of the mineral element is added as in the first aspect, and the base powder and the inorganic salt or inorganic acid salt are uniformly dispersed. Immediately add chelating agent without liquid.
The pH of the mixed solution after addition of the chelating agent is preferably 3.0 or more and 9.0 or less, and the stirring time of the mixed solution under the pH condition is preferably about 1 hour.
The third step of this embodiment is a step of granulating using the mixed solution after the completion of the second step as a raw material solution to obtain a granulated powder having a uniform mineral content.
The granulation method is the same as in the first embodiment.
As shown in Example 3 to be described later, according to the second aspect, it is possible to obtain a mineral dispersion effect that is substantially comparable to the first aspect with fewer steps than the first aspect.

As another aspect of the present invention, (1) In the first step, an inorganic salt or inorganic acid salt of a mineral element and a chelating agent are added simultaneously or sequentially to an aqueous solvent, and in the second step, A mode of adding granulated base powder, stirring sufficiently, and granulating this in the third step, (2) In the first step, adding an inorganic salt or inorganic acid salt of mineral element to the aqueous solvent In the second step, the granulated base powder is added thereto, in the third step, the chelating agent is added thereto, and the mixture is sufficiently stirred, and in the fourth step, the granulation is performed, (3) In the first step, a chelating agent is added to the aqueous solvent, in the second step, granulated base powder is added thereto, and in the third step, an inorganic salt or inorganic element of mineral element is added thereto. A mode in which an acid salt is added, sufficiently stirred, and granulated in the fourth step. And the like.
Although the mineral dispersion effect according to these embodiments is inferior to that of the first embodiment except for some mineral components, an excellent dispersion effect can be obtained in many mineral components as compared with the case where no chelating agent is used.

  Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited to these examples.

Example 1
Soluble starch powder (10 g), which becomes a base powder during spray drying, was dispersed in an aqueous solvent (about 230 mL) so that the final concentration was 4% by mass to obtain an aqueous dispersion.
This is mixed with sodium chloride solution, calcium carbonate solution and potassium dichromate solution, and nitrate solution of magnesium, manganese, iron, copper, zinc and selenium (all JCSS compatible metal standard solutions: manufactured by Kanto Chemical Co., Inc.) Diluted solution added, final concentration of each element as sodium 100μg / L, magnesium 540μg / L, calcium 45μg / L, chromium 20μg / L, manganese 500μg / L, iron 10μg / L, copper 160μg / L, zinc After adjusting to 670 μg / L and selenium 20 μg / L, the mixture was stirred until no solid suspended matter was visible.
To this, trisodium citrate dihydrate powder (2 g) was added as a chelating agent so that the final concentration was 0.8% by mass, the pH was adjusted to 6.9, and the volume was adjusted to 250 mL with an aqueous solvent, and stirred for 1 hour. did.
The obtained liquid mixture was spray-dried with a spray dryer (product name: B290) manufactured by Nihon Büch Corporation while stirring. At that time, a two-fluid nozzle (nozzle hole diameter 0.7 mm) was used for spraying the mixed liquid, and a glass drying tower for an aqueous solvent was used for drying the spray droplets. In addition, a tangential inflow cyclone type collection container was used for collecting the granulated powder. The spray drying conditions were an inlet temperature of 190 ° C., an outlet temperature of 92 ° C. to 98 ° C., a liquid feed rate of 10 mL / min, an air flow rate of 35 m ³ / h after passing through a dehumidifier, and a spray gas (nitrogen) flow rate of 600 L / h. The resulting granulated powder (7.8 g to 8.5 g) has a recovery rate from the starting powder (soluble starch powder and citrate powder) of 65 mass% to 70 mass% and an average particle size of 15.3 μm (when dispersed in water) ), The residual water content was 6.8% by mass.
Five sub-samples, 0.5g each, were collected from the resulting granulated powder, and after making a solution by high-temperature pressure acid decomposition using a microwave sample decomposition apparatus, an inductively coupled plasma mass spectrometer (ICP -MS) was used to quantify the concentration of each element, and the uniformity of the element distribution in the granulated powder was evaluated.
As a result, as shown in Table 1, the RSD of the element concentration between the five sub-samples is 0.70% sodium, 0.20% magnesium, 1.1% calcium, 0.78% chromium, 0.69% manganese, 3.6% iron, 1.1% copper, They were 0.79% zinc and 0.95% selenium. Among the RSD values, the values of magnesium, iron, copper, and zinc are smaller values than when spray-dried without the addition of the citrate, and compared to the RSD value when citrate is not used. This corresponds to a value of 1 / 3.8 for the magnesium concentration, 1 / 1.9 for the iron concentration, 1 / 2.6 for the copper concentration, and 1 / 2.8 for the zinc concentration.
From this, it can be said that by using citrate, the obtained granulated powder has improved the uniformity of the mineral content with respect to the specific mineral component.

Example 2
As chelating agent added in the third step, L (-)-sodium malate, (+)-sodium tartrate, L-cysteine hydrochloride monohydrate or L-histidine instead of trisodium citrate dihydrate A raw material mixture for granulation was prepared in the same manner as in Example 1 except that hydrochloride monohydrate was used, and granulation was performed by a spray drying method.
The resulting granulated powder (7.7 g to 8.2 g) has a recovery rate from the starting powder (soluble starch powder and organic acid salt powder or amino acid salt powder) of 64% by mass to 68% by mass and an average particle size of 14.0 μm. ˜17.6 μm (when dispersed in water) and residual water content was 7.3% by mass to 7.8% by mass.
Three sub-samples, 0.5 g each, were collected from the resulting granulated powder, dissolved in high-temperature pressure acid decomposition using a microwave sample decomposition device, and then each element was measured using ICP-MS. The concentration was quantified and the uniformity of element distribution in the granulated powder was evaluated.
As a result, as shown in Table 2, the RSD of the element concentration among the three sub-samples is 0.14% to 2.7% sodium, 0.25% to 1.7% magnesium, and calcium according to the organic acid salt or amino acid salt used. In the range of 0.27% to 1.6%, chromium 0.20% to 2.0%, manganese 0.80% to 2.5%, iron 7.2% to 10.8%, copper 0.07% to 2.1%, zinc 1.2% to 11.3%, selenium 0.68% to 1.7% changed.
Among the RSD values, the following mineral component concentrations when using the following organic acid salt or amino acid salt are smaller than those when spray drying without adding the organic acid salt or amino acid salt powder. In other words, the RSD value when malic acid was used was equivalent to 1/3 of the magnesium concentration and 1/17 of the copper concentration, compared to the RSD value when malic acid was not used. When used, this corresponds to a sodium concentration of 4.9, magnesium concentration of 2.2, calcium concentration of 2.9, and copper concentration of 41. The concentration corresponds to a value of 2.1 / zinc, and the zinc concentration corresponds to a value of 1/1. When histidine hydrochloride is used, the copper concentration corresponds to a value of 1/1. 4 and the zinc concentration corresponds to a value of 1 / 1.7.
From this, it can be said that by using these organic acid salt or amino acid salt, the obtained granulated powder has improved uniformity of mineral content with respect to the specific mineral component.

Example 3
A raw material mixture for granulation was prepared in the same manner as in Example 1 except that the procedure for preparing the raw material mixture for granulation was changed, and granulated by a spray drying method. The changed procedure is shown below together with the procedure in the first embodiment.

なお、この実施例においては、キレート剤として、実施例１と同様に、クエン酸三ナトリウム二水和物を用いている。
これらの手順により調製した原料混合液を噴霧乾燥することにより得られた各造粒粉末から5個の副試料、各0.5gを分取し、マイクロ波試料分解装置を用いた高温加圧酸分解による溶液化を行った後、ICP-MSを用いて各元素濃度を定量し、造粒粉末における元素分布の均一性を評価した。
その結果を、実施例１の結果と併せて、表４に示す。表４に示すとおり、５個の副試料間での元素濃度のRSDは、造粒用の混合液を作成する手順に応じて、ナトリウム0.68%〜4.7%、マグネシウム0.20 %〜0.77%、カルシウム0.64%〜1.9%、マンガン0.69%〜1.5%、鉄3.6%〜11.6%、銅0.57%〜1.4%、亜鉛0.79%〜1.5%の範囲で変化した。
当該RSD値のうち、以下の混合液作成手順を用いた場合の以下のミネラル成分濃度のRSD値については、実施例１の混合液作成手順を用いた場合と匹敵する値、あるいは、より小さい値となった：すなわち、検討パターン（１）の手順で混合液を作成した場合の鉄、銅、および亜鉛の濃度のRSD値は、実施例１の混合液作成手順を用いた場合のRSD値と比べて、鉄濃度で0.97分の1、銅濃度で1.0分の1、亜鉛濃度で0.72分の1であり、実施例１の混合液作成手順を用いた場合とほぼ匹敵した。また、検討パターン（２）の手順で混合液を作成した場合の銅、検討パターン（３）の手順で混合液を作成した場合のカルシウム、並びに、検討パターン（４）の手順で混合液を作成した場合のカルシウム、および銅の濃度のRSD値は、実施例１の混合液作成手順を用いた場合のRSD値と比べて、それぞれ1.7分の1、1.6分の1、1.7分の1、および1.9分の1であった。
これらのことから、上記手順で混合液を作成することにより、得られた造粒粉末は、上記特定のミネラル成分について、実施例１と匹敵し、あるいは、それを上回り、ミネラル含量の均一性が向上したといえる。
また、上記RSD値のうち、以下の混合液作成手順を用いた場合の以下のミネラル成分濃度のRSD値については、実施例１の混合液作成手順においてクエン酸塩を用いなかった場合より小さい値となった：検討パターン（１）の手順で混合液を作成した場合の鉄、銅、および亜鉛、検討パターン（２）の手順で混合液を作成した場合のマグネシウム、銅、および亜鉛、検討パターン（３）の手順で混合液を作成した場合のマグネシウム、カルシウム、銅、および亜鉛、並びに、検討パターン（４）の手順で混合液を作成した場合のマグネシウム、カルシウム、銅、および亜鉛。
これらのことから、上記手順で混合液を作成することにより、得られた造粒粉末は、上記特定のミネラル成分について、実施例１の混合液作成手順においてクエン酸塩を用いなかった場合よりも、ミネラル含量の均一性が向上したといえる。

In this example, trisodium citrate dihydrate was used as the chelating agent, as in Example 1.
Five sub-samples and 0.5 g each were collected from each granulated powder obtained by spray-drying the raw material mixture prepared by these procedures, and subjected to high-temperature pressure acid decomposition using a microwave sample decomposition device After the solution was made by the method, the concentration of each element was quantified using ICP-MS, and the uniformity of the element distribution in the granulated powder was evaluated.
The results are shown in Table 4 together with the results of Example 1. As shown in Table 4, the RSD of the element concentration between the five sub-samples is 0.68% to 4.7% sodium, 0.20% to 0.77% magnesium, 0.64% calcium, depending on the procedure for preparing the mixture for granulation. It varied in the range of% ~ 1.9%, manganese 0.69% ~ 1.5%, iron 3.6% ~ 11.6%, copper 0.57% ~ 1.4%, zinc 0.79% ~ 1.5%.
Among the RSD values, the RSD value of the following mineral component concentration when using the following mixed liquid preparation procedure is a value comparable to or smaller than that when using the mixed liquid preparation procedure of Example 1. In other words, the RSD values of the iron, copper, and zinc concentrations when the mixed solution was prepared by the procedure of the examination pattern (1) are the same as the RSD values when the mixed solution preparing procedure of Example 1 was used. In comparison, the iron concentration was 0.97 / 1, the copper concentration was 1 / 1.0, and the zinc concentration was 0.72 and was almost comparable to the case of using the mixed liquid preparation procedure of Example 1. Also, copper when the mixed solution is prepared by the procedure of the examination pattern (2), calcium when the mixed solution is prepared by the procedure of the examination pattern (3), and the mixed solution by the procedure of the examination pattern (4) The RSD values of the calcium and copper concentrations when compared with the RSD values when using the mixed liquid preparation procedure of Example 1 are respectively 1.7 / 1, 1.6 / 1, 1.7 / 1, and It was 1 / 1.9.
From these facts, the granulated powder obtained by preparing the mixed solution by the above procedure is comparable to or exceeding Example 1 with respect to the specific mineral component, and the uniformity of the mineral content is It can be said that it has improved.
In addition, among the RSD values described above, the RSD value of the following mineral component concentration when using the following mixed liquid preparation procedure is smaller than that when citrate is not used in the mixed liquid preparation procedure of Example 1. It became: Iron, copper, and zinc when the mixed solution was prepared by the procedure of the examination pattern (1), magnesium, copper, and zinc when the mixed solution was prepared by the procedure of the examination pattern (2), the examination pattern Magnesium, calcium, copper, and zinc when the mixed solution is prepared by the procedure of (3), and magnesium, calcium, copper, and zinc when the mixed solution is prepared by the procedure of the examination pattern (4).
From these things, the granulated powder obtained by preparing a liquid mixture in the above procedure is more specific than the case where citrate was not used in the liquid mixture preparation procedure of Example 1 for the specific mineral component. It can be said that the uniformity of the mineral content has been improved.

  The mineral dispersion technology in the granulated powder according to the present invention can uniformly disperse minerals in food production and preparation production based on granulation by spray drying or the like, so that general foods containing mineral components (health supplements, nutrition Manufacture of supplementary foods, nutrition-adjusted foods and nutritional therapy foods, health functional foods (special health foods, nutritional functional foods and functional labeling foods) and special-purpose foods, and solid preparations of pharmaceuticals or agricultural chemicals (solid dispersion) It can be used for the production of body preparations.

Claims (8)

  By adding granulated base powder, mineral element inorganic salt or inorganic acid salt and chelating agent to an aqueous solvent, mixing and stirring the mixture solution as a raw material solution, A method for dispersing minerals in a granulated powder, comprising obtaining a granulated powder having a uniform mineral content.   First step of making granulated base powder dispersed in aqueous solvent to form aqueous dispersion, mixing inorganic salt or inorganic acid salt of mineral element in aqueous dispersion after completion of first step, The second step, which is a mixed solution in which inorganic salt or inorganic acid salt is uniformly dispersed, the third step, the third step of adding a chelating agent to the mixed solution after completion of the second step, and stirring under weakly acidic to weakly alkaline conditions The granulated powder according to claim 1, comprising a fourth step of obtaining a granulated powder having a uniform mineral content by performing granulation using the mixed liquid after completion as a raw material solution. Mineral dispersion method.   1st step of dispersing granulated base powder in aqueous solvent to make aqueous dispersion, adding mineral element inorganic salt or inorganic acid salt and chelating agent to aqueous dispersion after completion of first step, weakening The second step of stirring under acidic to weakly alkaline conditions, and the third step of obtaining a granulated powder having a uniform mineral content by performing granulation using the mixed solution after completion of the second step as a raw material solution The method for dispersing minerals in the granulated powder according to claim 1.   The method according to any one of claims 1 to 3, wherein the chelating agent is an organic acid salt or amino acid salt having one or more carboxyl groups acting as ligands for metal ions.   The method according to claim 1, wherein the mineral element is iron, copper and / or zinc and the chelating agent is citrate.   The method according to any one of claims 1 to 3, wherein the mineral element is copper and / or zinc, and the chelating agent is a cysteine salt or a histidine salt.   The method according to claim 1, wherein the mineral element is copper and the chelating agent is malate or tartrate.   The method according to claim 1, wherein the granulation is performed by a spray drying method.

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