WO2018030225A1 - Magnesium oxide granules - Google Patents

Magnesium oxide granules Download PDF

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Publication number
WO2018030225A1
WO2018030225A1 PCT/JP2017/027964 JP2017027964W WO2018030225A1 WO 2018030225 A1 WO2018030225 A1 WO 2018030225A1 JP 2017027964 W JP2017027964 W JP 2017027964W WO 2018030225 A1 WO2018030225 A1 WO 2018030225A1
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WO
WIPO (PCT)
Prior art keywords
magnesium oxide
content
weight
granules
oxide granules
Prior art date
Application number
PCT/JP2017/027964
Other languages
French (fr)
Japanese (ja)
Inventor
誠二 松井
紗希 伊東
Original Assignee
神島化学工業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 神島化学工業株式会社 filed Critical 神島化学工業株式会社
Priority to JP2018532962A priority Critical patent/JP6789297B2/en
Publication of WO2018030225A1 publication Critical patent/WO2018030225A1/en

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16—Inorganic salts, minerals or trace elements
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/22—Boron compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/10—Laxatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00—Drugs for disorders of the metabolism
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide

Definitions

  • the present invention relates to magnesium oxide granules and tablets containing magnesium oxide granules.
  • Magnesium oxide is widely used in various industrial fields such as pharmaceuticals, foodstuffs, vulcanization accelerators, pigments for paints and inks, and in particular, magnesium oxide tablets are widely used as pharmaceutical laxatives and mineral supplements. (For example, Patent Documents 1 to 3).
  • tablets are manufactured by compressing raw materials into tablets. Moreover, this compression molding process is called a tableting process. In the tableting process, the compression operation is continuous and performed at high speed. Under such conditions, distribution of stress and density occurs inside the tablet, and the internal structure is never uniform, which is considered to be the main cause of tableting failure and quality characteristic abnormality. .
  • Examples of the tableting trouble include capping, laminating, sticking, and picking.
  • Capping is a phenomenon in which a tablet is molded and then discharged from the mortar, or the tablet is peeled off in a cap shape after laminating
  • laminating is a phenomenon in which capping becomes worse and peels in layers along the side rather than the top surface It is.
  • Sticking is a phenomenon in which powder adheres to the wrinkles (compression rods) during the compression process and the tablet surface is damaged like a depression
  • chipping is a phenomenon in which the tablet surface is slightly damaged for the same reason.
  • the quality characteristic abnormality there is a state in which the tablet is cracked, chipped, powdered off or the like even under normal use conditions. Such a quality characteristic abnormality mainly occurs because the strength (hardness) of the tablet is insufficient.
  • Patent Document 4 describes that the tableting trouble and tablet strength can be improved by setting the specific surface area and activity of the magnesium oxide granules for use in pharmaceuticals and food additives within a specific range.
  • Magnesium oxide is particularly useful when it is used directly or indirectly, such as fertilizer, food, cosmetics, and pharmaceutical raw materials, or when it is intended to be in contact with the human body. A pure one is desired.
  • An object of the present invention is to provide magnesium oxide (granule) having excellent dissolution properties, a method for producing the same, and a tablet containing the magnesium oxide (granule).
  • Another object of the present invention is to provide magnesium oxide (granule) with few production defects (chips, cracks, etc.), a method for producing the same, and a tablet containing the magnesium oxide (granule).
  • Still another object of the present invention is to provide magnesium oxide (granule) that can improve dissolution and poor production while maintaining high purity, a method for producing the same, and a tablet containing the magnesium oxide (granule).
  • Another object of the present invention is to provide a method for efficiently producing the above magnesium oxide (granule).
  • the present inventors examined the magnesium oxide granules of Patent Document 4, but found that there was room for improvement in the dissolution property, which is an important characteristic of tablets. It was also found that there was room for further improvement in terms of chipping and cracking of the tablets.
  • the present invention has a B (boron) content of 0.05% by weight or less, a Ca (calcium) content of 0.03 to 1.8% by weight, and a pure content (Assay) of 95 to 99%.
  • the BET specific surface area may be, for example, about 5 to 60 m 2 / g.
  • the representative magnesium oxide of the present invention has a B content of 0.03% by weight or less, a Ca content of 0.05 to 1.5% by weight, an purity of 96 to 99%, BET Magnesium oxide (granule) having a specific surface area of 10 to 50 m 2 / g is included.
  • Magnesium oxide may be derived from seawater.
  • the present invention satisfies the following (1) and / or (2), and is used directly or indirectly for ingestion or contact with animals (for example, selected from food use, pharmaceutical use and cosmetic use) Magnesium oxide (granules) for use in at least one application.
  • animals for example, selected from food use, pharmaceutical use and cosmetic use
  • Magnesium oxide (granules) for use in at least one application.
  • B content is 0.05% by weight or less
  • Ca content is 0.03 to 1.8% by weight
  • Such magnesium oxide may have a purity of about 95 to 99%.
  • the present invention includes a method for producing the above magnesium oxide (granule).
  • a method for producing the above magnesium oxide (granule) may include at least a step of removing B from seawater.
  • B may be removed from seawater with a chelate resin.
  • the present invention includes a tablet containing the magnesium oxide (granule).
  • magnesium oxide and tablets containing it can be improved by adjusting the B content, Ca content, and pure content. Therefore, for example, the following method is also included in the present invention.
  • a method for improving or improving the dissolution properties of tablets containing magnesium oxide granules by adjusting the B content in the magnesium oxide (granules) to 0.05% by weight or less.
  • the B content is adjusted to 0.03% by weight or less, the Ca content is adjusted to 0.05 to 1.5% by weight, and the pure content (Assay) is adjusted to 95 to 99%.
  • magnesium oxide (granule) having excellent dissolution properties can be provided.
  • magnesium oxide granule with few manufacturing defects (chips, cracks, etc.) can be provided.
  • such magnesium oxide can improve elution and production defects while maintaining high purity (95% or more, preferably 96% or more). Moreover, even if the dissolution property and the manufacturing defect are improved, the tablet hardness is not impaired, and the improvement of the dissolution property and the manufacturing defect and the high hardness can be achieved at the same time.
  • the magnesium oxide and magnesium oxide tablet of the present invention are particularly useful in applications (for example, fertilizers, foods, pharmaceuticals, cosmetics, etc.) that are ingested or contacted directly or indirectly with animals (particularly humans).
  • a method for efficiently producing the above magnesium oxide (granule) can be provided.
  • raw materials such as seawater can be used, it can be manufactured easily (and inexpensively), and is extremely useful and practical.
  • the magnesium oxide of the present invention satisfies a specific B (boron) and / or Ca (calcium) content.
  • the content (content ratio) of B in magnesium oxide is, for example, 0.1% by weight or less (for example, 0.08% by weight or less), preferably 0.05% by weight or less (for example, 0.04% by weight or less). ), More preferably 0.03% by weight or less (for example, 0.02% by weight or less), and particularly 0.015% by weight or less.
  • the lower limit of the content of B is not particularly limited, and may be, for example, 0% by weight (or detection limit), such as 0.00001% by weight, 0.0001% by weight, 0.001% by weight, etc. It may be. An appropriate range may be set by appropriately combining these numerical values (for example, 0.00001 to 0.05% by weight, etc., and the following description of numerical values is the same).
  • the Ca content (content ratio) in the magnesium oxide can be selected from the range of 0.03% by weight or more (for example, 0.03 to 2% by weight), for example, 0.03 to 1.8% by weight (for example, 0.04 to 1.6% by weight), preferably 0.05 to 1.5% by weight (eg 0.08 to 1.5% by weight), more preferably 0.1 to 1.5% by weight ( For example, it may be about 0.2 to 1.5% by weight), particularly about 0.3 to 1.5% by weight (for example, 0.4 to 1.5% by weight), and 0.5% by weight or more ( For example, it may be 0.5 to 1.5% by weight).
  • fills both the range of said B content, and the range of Ca content, as long as either of these is satisfied, it is not necessary to satisfy the content rate of the other. .
  • the magnesium oxide of the present invention may contain elements other than Mg, B and Ca.
  • elements include, but are not limited to, non-metallic elements [for example, C (carbon), S (sulfur), halogen (for example, Cl (chlorine), etc.)], metal elements or metalloid elements [for example, Typical metal elements (for example, alkali or alkaline earth metals such as Na (sodium); Al (aluminum), Si (silicon), etc.), transition metal elements (for example, Fe (iron), Zn (zinc), etc.), etc. ] Etc. are mentioned. These elements may be contained in magnesium oxide alone or in combination of two or more.
  • typical elements are silicon, sodium, halogen (such as chlorine), and the like.
  • Magnesium oxide containing such an element may be derived from seawater, for example.
  • desired physical properties / characteristics excellent elution properties, few manufacturing defects, etc.
  • the content of other elements in the magnesium oxide can be appropriately selected according to the type of element.
  • the silicon content is, for example, 0.001% by weight or more (eg, 0.001 to 0.1% by weight), preferably 0.005 to 0.07% by weight, and more preferably 0.01 to 0%. It may be about 0.05% by weight.
  • the sodium content is, for example, 0.0001% by weight or more (eg, 0.0001 to 0.1% by weight), preferably 0.0005 to 0.05% by weight, and more preferably 0.001 to 0%. It may be about 0.01% by weight.
  • the chlorine content is, for example, 0.0001% by weight or more (eg, 0.0001 to 0.1% by weight), preferably 0.0005 to 0.05% by weight, and more preferably 0.001 to 0%. It may be about 0.01% by weight.
  • the content of Pb (lead) may be 1 ppm or less (for example, about 0.1 ppm),
  • the content of As (arsenic) may be 4 ppm or less (for example, about 1 ppm).
  • the ratio of each element in magnesium oxide can be measured by, for example, ICP emission spectroscopy (ICP-AES method), ICP mass spectrometry (ICP-MS method), or the like.
  • the purity of magnesium oxide is not particularly limited, but may be required to be high purity depending on the application. On the other hand, if the purity is too high, desired physical properties and characteristics may be impaired.
  • the purity of magnesium oxide can be selected from a high purity range, for example, 90% or more (eg, 93 to 99.5%), and preferably 95% or more (eg, 95%). To 99%), more preferably 96 to 99% (for example, 96.3 to 98.5%), particularly 96 to 98%.
  • the BET specific surface area of magnesium oxide can be selected from a range of, for example, about 1 to 100 m 2 / g (for example, 3 to 80 m 2 / g), and preferably 5 to 60 m 2 / g (for example, 8 to 55 m 2 / g). ), More preferably 10 to 50 m 2 / g (for example, 12 to 45 m 2 / g), particularly about 15 to 40 m 2 / g (for example, 20 to 35 m 2 / g).
  • the method for measuring the BET specific surface area is not particularly limited as long as it is a method usually used in this field.
  • a nitrogen adsorption method may be used.
  • a measurement sample (magnesium oxide granule) heat-treated in a nitrogen gas atmosphere as a pretreatment may be measured by a nitrogen gas adsorption method with a BET specific surface area measuring device.
  • the pretreatment may be performed, for example, at about 130 ° C. for about 30 minutes in a nitrogen gas atmosphere.
  • the apparatus and the BET specific surface area measuring apparatus used for the pretreatment are not particularly limited, and any apparatus normally used in this field may be used.
  • the bulk density of magnesium oxide may be, for example, about 700 to 1200 g / L, preferably about 850 to 1000 g / L, and more preferably about 900 to 950 g / L.
  • the bulk density may be a bulk density specified by the Japanese Pharmacopoeia.
  • the shape of the magnesium oxide may be usually a granule (granular, powdery or granular).
  • the average particle diameter of magnesium oxide is not particularly limited and can be selected according to the use and the like, and may be, for example, about 200 to 700 ⁇ m, preferably about 250 to 600 ⁇ m, and more preferably about 300 to 500 ⁇ m.
  • the range of the particle diameter (minimum diameter to maximum diameter) is not particularly limited and can be selected depending on the application. For example, from the viewpoint of elution, 100 to 850 ⁇ m, preferably 150 to 500 ⁇ m, and more preferably 250 It may be about 350 ⁇ m. In addition, you may measure a particle size with a sieve shaker, for example.
  • the method for producing magnesium oxide of the present invention is not particularly limited as long as the above characteristics and physical properties can be obtained, and a conventional method may be used.
  • the magnesium oxide of the present invention includes a step of obtaining magnesium hydroxide by adding an alkali to a magnesium source (magnesium hydroxide production step), and a step of firing the obtained magnesium hydroxide to obtain magnesium oxide (firing step). It is preferable to manufacture through these.
  • examples of the magnesium source include seawater, magnesium chloride aqueous solution (brine), and seawater may be particularly preferably used.
  • seawater By using seawater, it is easy to obtain magnesium oxide having a predetermined concentration of calcium.
  • magnesium oxide having a low B (boron) content when magnesium oxide having a low B (boron) content is obtained as described above, a magnesium source having a previously reduced B content may be used.
  • seawater from which boron has been removed may be used as the magnesium source.
  • the production method of the present invention may include at least a step (boron separation step) of removing (or separating) boron from a magnesium source (particularly seawater).
  • the method for removing boron is not particularly limited.
  • B may be removed (separated) from the magnesium source with a chelate resin.
  • B can be removed by passing a magnesium source (seawater) through the chelate resin (water flow).
  • chelate resin examples include resins having a chelate functional group (eg, N-methylene glucamine) (eg, styrene-divinylbenzene copolymer, cellulose).
  • chelate resin chelate fiber
  • Kyrest company As a commercial item of chelate resin (chelate fiber), it can obtain from Kyrest company.
  • the alkali is not particularly limited, but typically a calcium hydroxide source may be used.
  • the calcium hydroxide source may be slaked lime, and the slaked lime may be in the form of lime milk.
  • the firing temperature is not particularly limited, but may be, for example, about 500 to 2000 ° C., preferably 600 to 1500 ° C., more preferably about 700 to 1200 ° C.
  • the firing time can also be appropriately selected, and may be, for example, 10 minutes to 10 hours, preferably 30 minutes to 5 hours, and more preferably about 1 to 3 hours.
  • the magnesium oxide obtained in the firing step may be usually pulverized according to a desired shape (for example, a granular shape). Therefore, the method of the present invention may further include a pulverization step of pulverizing the magnesium oxide obtained in the calcination step after the calcination step.
  • the baking state of the magnesium oxide obtained at the baking process is light baking (light baking state).
  • the activity of such lightly burned magnesium oxide (lightly burned magnesium) is, for example, about several to several hundreds m 2 / g (for example, 1 to 300 m 2 / g, preferably 2 to 100 m in terms of BET specific surface area). 2 / g).
  • magnesium oxide may be pressurized and pulverized as necessary.
  • the pressing conditions can be selected as appropriate, and the pressing device is not particularly limited, and a roller compactor or the like may be used.
  • the pulverization method is not particularly limited, and for example, pulverization may be performed using a granulator. Although it does not specifically limit as said granulator, For example, a roll granulator is mentioned. Specifically, the pulverization method may be a method in which magnesium oxide pressurized is passed through a gap between the rotated rolls and pulverized using a roll granulator in which the rolls are set in three vertical stages.
  • the pulverized magnesium oxide may have the same particle size or particle size by sieving as necessary.
  • the use of the magnesium oxide (granule) of the present invention is not particularly limited, and various uses [for example, Pigments, rubber additives (vulcanization accelerators, etc.), fertilizers, foods, cosmetics, pharmaceuticals, etc.].
  • magnesium oxide granule
  • tablet of the present invention are used for ingesting or contacting animals directly or indirectly (for example, for foods). , For pharmaceuticals, cosmetics, fertilizers, etc.).
  • food includes health foods such as foods for specified health use and functional foods for nutrition, in addition to general foods including health foods.
  • the food includes supplements (dietary supplements), feed and the like.
  • the magnesium oxide of the present invention may be formed into a desired form according to the use or the like, and may particularly constitute a tablet. That is, the magnesium oxide (tablet) of the present invention may be for tablets (for example, for direct compression tablets). Therefore, this invention includes the tablet containing the said magnesium oxide.
  • Tablets need only contain magnesium oxide, and may be formed with conventional additives (such as binders and disintegrants) depending on the application.
  • the binder is not particularly limited, and examples thereof include sodium carboxymethyl cellulose, low-substituted hydroxypropyl cellulose, crystalline cellulose, starch (for example, corn starch) and the like.
  • disintegrant is not particularly limited, and examples thereof include carboxymethylcellulose calcium, carmellose, low-substituted hydroxypropylcellulose, croscarmellose sodium, carmellose calcium, and carboxystarch sodium.
  • the tablet may further contain an excipient, a lubricant and the like.
  • the excipient is not particularly limited, and examples thereof include lactose, sucrose, mannitol, corn starch, and crystalline cellulose.
  • the lubricant is not particularly limited, and examples thereof include sucrose fatty acid ester, polyethylene glycol, talc, stearic acid or stearate (Na, Mg, or Ca salt).
  • tablets may optionally contain plasticizers, coating agents, anti-aggregation agents, solubilizers, sweeteners, sour agents, corrigents, pH adjusters, solubilizers, colorants, flavors, mineral sources (eg, calcium carbonate).
  • plasticizers coating agents, anti-aggregation agents, solubilizers, sweeteners, sour agents, corrigents, pH adjusters, solubilizers, colorants, flavors, mineral sources (eg, calcium carbonate).
  • coating agents e.g, anti-aggregation agents, solubilizers, sweeteners, sour agents, corrigents, pH adjusters, solubilizers, colorants, flavors, mineral sources (eg, calcium carbonate).
  • plasticizer examples include triethyl citrate, glycerin fatty acid ester, polyethylene glycol and the like.
  • coating agent examples include ethyl cellulose and hydroxypropyl methyl cellulose.
  • aggregation inhibitor examples include talc and calcium stearate.
  • solubilizer examples include sucrose fatty acid ester, sorbitan monostearate, sodium lauryl sulfate and the like.
  • sweetener examples include aspartame, saccharin, dipotassium glycyrrhizinate, stevia and the like.
  • acidulant (organic acid) examples include citric acid, malic acid, ascorbic acid, and fumaric acid.
  • Examples of the corrigent include l-menthol, sodium chloride, acesulfame potassium, sucralose and the like.
  • Examples of the pH adjuster include citrate, phosphate, carbonate, acetate, and the like.
  • Examples of the solubilizer include cyclodextrin, arginine, lysine, trisaminomethane and the like.
  • Examples of the colorant include yellow iron sesquioxide, iron sesquioxide, and copper chlorophyllin sodium.
  • Examples of the fragrance include orange oil, lemon oil, mint oil, eucalyptus oil and the like.
  • additives may be used alone or in combination of two or more, or different additives may be combined.
  • the content (mixing amount, content ratio) of the additive can be appropriately selected according to the type of the additive.
  • the blending amount of the binder is not particularly limited, but for example, 0.1 to 30 weight in the tablet %, Preferably 0.5 to 20% by weight, more preferably about 1 to 15% by weight.
  • the amount of the disintegrant is not particularly limited, but may be, for example, 0.1 to 30% by weight, preferably 0.5 to 10% by weight, more preferably 1 to 5% by weight in the tablet.
  • the proportion of magnesium oxide (granule) can be selected depending on the application and is not particularly limited.
  • it is 50% by weight or more (for example, 60% by weight or more), preferably 70% by weight or more (for example, 75 wt% or more), 80 wt% or more, 85 wt% or more, 90 wt% or more, or 95 wt% or more.
  • the tablet production method may be in accordance with a conventionally known method.
  • the magnesium oxide tablet of the present invention can be produced by mixing magnesium oxide (granule), a binder and a disintegrant (and other additives as necessary) and tableting (tabletting). Good.
  • the tableting method is not particularly limited, and may be a direct compression method (direct powder compression method), a wet granule compression method, or the like.
  • the direct compression method may be particularly preferably used.
  • the strength of the tablet can be selected depending on the application, but is, for example, 50 N or more (for example, 55 to 200 N), preferably 60 N or more (for example, 65 to 180 N), more preferably 70 N or more (for example, 70 to 150 N). In particular, it may be about 75N or more (for example, 75 to 120N).
  • Impurity analysis method (content): Measured by ICP-AES method.
  • the pure content was measured according to the United States Pharmacopoeia (United States Pharmacopia, USP).
  • BET specific surface area measurement method Measured by nitrogen adsorption method.
  • Tablet sample molding method in combination (magnesium oxide: 75%, crystalline cellulose: 10%, light calcium carbonate: 10%, croscarmellose sodium: 3%, magnesium stearate: 1%, citric acid: 1%)
  • the tablets were tableted at a tableting pressure of 5 kN using a rotary tableting machine equipped with a punch having a diameter of 8 mm and a radius of curvature of R10 mm to obtain magnesium oxide tablets having a weight of 300 mg and a thickness of 4.0 mm per tablet.
  • Dissolution rate measurement method Using a dissolution tester (manufacturer: Varian 70, VK7025), the dissolution test was performed according to the dissolution test paddle method listed in the Japanese Pharmacopoeia (test solution: No. 1 liquid, liquid temperature: 37 degreeC, rotation speed: 50 rpm, measurement time: 45 minutes). The amount of magnesium oxide eluted was measured by ICP-AES method. The measurement was performed with 3 vessels, and the average value was defined as the average dissolution rate.
  • Tablet hardness measurement method Tablet hardness was measured using a tablet breaking strength measuring device (Toyama Sangyo: TH303MP). Ten tablets were measured and the average value was determined.
  • Measure method of defective cracking rate Continuous tableting was performed, the chip was checked for cracks and cracks, and the number of shots where defects started to occur was counted. It is determined that the larger the number of shots, the smaller the defect rate.
  • Example 1 9600 mL of seawater was passed at a constant rate of 15 mL / mL-fiber / h to the chelate fiber (trade name: Cylest Fiber GRY-HW) manufactured by Crest, which was filtered and filled with column. Was removed.
  • the chelate fiber trade name: Cylest Fiber GRY-HW
  • a 300 mL alumina crucible was filled with 100 g of raw material and fired at 820 ° C. for 2 hours using an electric furnace to obtain a MgO sample.
  • a roll pressure of 1 MPa was applied to the MgO sample using a horizontal roller compactor made by Freund Turbo. Then, it grind
  • magnesium oxide granules (average particle size of about 400 ⁇ m).
  • Example 2 Magnesium oxide granules were obtained by performing the same operation as in Example 1 except that 10500 mL of seawater was passed through the chelate fiber at a constant rate of 15 mL / mL-fiber / h to remove B in the seawater. Using this, various properties and physical properties were measured or evaluated.
  • Example 3 Magnesium oxide granules were obtained by performing the same operation as in Example 1 except that 11400 mL of seawater was passed through the chelate fiber at a constant rate of 15 mL / mL-fiber / h to remove B in the seawater. Using this, various properties and physical properties were measured or evaluated.
  • Example 4 Magnesium oxide was prepared in the same manner as in Example 1 except that 51 mL of an 8.3N NaOH aqueous solution was added as an alkali raw material (Mg 2+ mol number: OH ⁇ mol number was 1.0: 1.8). Granules were obtained and used to measure or evaluate various properties and physical properties.
  • Example 5 Magnesium oxide was prepared in the same manner as in Example 1 except that 54 mL of an 8.3N NaOH aqueous solution was added as an alkali raw material (Mg 2+ mol number: OH ⁇ mol number was 1.0: 1.9). Granules were obtained and used to measure or evaluate various properties and physical properties.
  • Example 6 Milk of lime a 111mL addition adjusted to CaO concentration equivalent 11.9 g / dL as alkaline material (Mg 2+ moles: OH - moles 1.0: a which was 2.0) and other than the can, as in Example 1 The same operation was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using the same.
  • Example 7 Except for baking at 850 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
  • Example 8 Except for baking at 760 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
  • Example 9 Except for baking at 1000 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
  • Example 10 Except for baking at 710 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
  • Example 11 In a 2 L-capacity polyethylene container, 48 g of MgCl 2 .6H 2 O as a magnesium raw material was weighed, and 100 mL of pure water was added and stirred to prepare an MgCl 2 aqueous solution. This aqueous NaOH 51mL of 8.3N was added slowly with stirring as an alkali material (Mg 2+ moles: OH - moles was 1.0: 1.8), Mg a (OH) 2 suspension Prepared.
  • MgCl 2 aqueous solution in which 48 g of MgCl 2 ⁇ 6H 2 O was dissolved in 100 mL of pure water, and then slowly add 51 mL of 8.3 N NaOH aqueous solution with stirring. The first seed crystal reaction was performed by stirring for 5 minutes. Such seed crystal reaction was repeated a total of 10 times.
  • Example 1 Except for the above operations, the same operations as in Example 1 were performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using the same.
  • magnesium hydroxide manufactured by Kamishima Chemical Industry Co., Ltd., grade name: # 200
  • the medium active MgO thus obtained had a BET specific surface area of 51 m 2 / g.
  • # 200 was fired at 1100 ° C. for 2 hours in an electric furnace to produce low activity MgO.
  • the low activity MgO thus obtained had a BET specific surface area of 3 m 2 / g.
  • magnesium oxide granules having a high purity that can be sufficiently applied to pharmaceutical and food applications and having a boron content within a predetermined range (for example, 0.05% by weight or less) are used.
  • magnesium oxide granules having a high dissolution rate and a calcium content ratio within a predetermined range (for example, 0.03 to 1.8% by weight) it is possible to efficiently obtain a tablet with less blurring. I understood it.
  • magnesium oxide granules that can improve elution and manufacturing defects (eg, cracks) while having high purity.
  • Such magnesium oxide granules can be applied to various uses, but are sufficiently high in purity, and in particular, used for ingesting or contacting animals directly or indirectly (for example, for foods, pharmaceuticals, and cosmetics). And the like for fertilizers).

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Abstract

Provided are magnesium oxide granules capable of improving elution properties of tablets and reducing defects in the production thereof. In the magnesium oxide granules, the content of B (boron) is controlled to not more than 0.05 wt%, the content of Ca (calcium) is controlled to 0.03-1.8 wt%, and the purity (assay) is controlled to 95-99%. The magnesium oxide granules have a high purity and, therefore, are appropriately usable particularly for foods, drugs, cosmetics, etc.

Description

酸化マグネシウム顆粒Magnesium oxide granules
　本発明は、酸化マグネシウム顆粒及び酸化マグネシウム顆粒を含む錠剤に関する。 The present invention relates to magnesium oxide granules and tablets containing magnesium oxide granules.
　酸化マグネシウムは、医薬品、食品、加硫促進剤、塗料・インキ用顔料等、様々な産業分野において広く使用されており、特に、酸化マグネシウムの錠剤は、医薬用緩下剤やミネラル補給剤等として多岐に使用されている（例えば、特許文献１～３）。 Magnesium oxide is widely used in various industrial fields such as pharmaceuticals, foodstuffs, vulcanization accelerators, pigments for paints and inks, and in particular, magnesium oxide tablets are widely used as pharmaceutical laxatives and mineral supplements. (For example, Patent Documents 1 to 3).
　一般的に、錠剤は原材料を圧縮成形して錠剤の形にすることで製造される。また、この圧縮成形する工程を打錠工程という。打錠工程においては、圧縮操作が連続的で、しかも高速で行われる。このような条件下では、錠剤内部に応力や密度に分布が生じ、内部構造は決して均一なものにならず、これが打錠障害や品質特性異常等を引き起こす主な原因になっていると考えられる。 Generally, tablets are manufactured by compressing raw materials into tablets. Moreover, this compression molding process is called a tableting process. In the tableting process, the compression operation is continuous and performed at high speed. Under such conditions, distribution of stress and density occurs inside the tablet, and the internal structure is never uniform, which is considered to be the main cause of tableting failure and quality characteristic abnormality. .
　前記打錠障害としては、キャッピング、ラミネーティング、スティッキング、ピッキング等がある。キャッピングは、錠剤を成型した後、臼から排出する過程又は排出後に錠剤が帽子状に剥離する現象であり、ラミネーティングはキャッピングがさらにひどくなり、錠剤上面ではなく側面に沿って層状に剥離する現象である。スティッキングは、圧縮行程で杵（圧縮棒）に粉末が付着し、錠剤表面が凹んだように損傷する現象であり、チッピングも同様の理由により、錠剤表面がわずかに損傷する現象である。これら打錠障害は、主に原材料の性質に起因して生じる。 </ RTI> Examples of the tableting trouble include capping, laminating, sticking, and picking. Capping is a phenomenon in which a tablet is molded and then discharged from the mortar, or the tablet is peeled off in a cap shape after laminating, and laminating is a phenomenon in which capping becomes worse and peels in layers along the side rather than the top surface It is. Sticking is a phenomenon in which powder adheres to the wrinkles (compression rods) during the compression process and the tablet surface is damaged like a depression, and chipping is a phenomenon in which the tablet surface is slightly damaged for the same reason. These tableting failures occur mainly due to the nature of the raw materials.
　また、前記品質特性異常として、通常の使用状況においても、錠剤に割れ、欠け、又は粉落ち等が発生するような状態が挙げられる。そのような品質特性異常は、主に錠剤の強度（硬度）が不足しているために生じる。 Also, as the quality characteristic abnormality, there is a state in which the tablet is cracked, chipped, powdered off or the like even under normal use conditions. Such a quality characteristic abnormality mainly occurs because the strength (hardness) of the tablet is insufficient.
　酸化マグネシウム錠剤の製造においても、特に純度の高い酸化マグネシウムを原材料とした場合、上記した打錠障害や品質特性異常が発生しやすくなるという課題があった。 Also in the manufacture of magnesium oxide tablets, there is a problem that the above-mentioned tableting troubles and quality characteristic abnormalities are liable to occur when magnesium oxide having a high purity is used as a raw material.
　このような中、特許文献４には、医薬品や食品添加用の酸化マグネシウム顆粒の比表面積と活性度を特定の範囲とすることで、打錠障害や錠剤強度を改善できると記載されている。 Under such circumstances, Patent Document 4 describes that the tableting trouble and tablet strength can be improved by setting the specific surface area and activity of the magnesium oxide granules for use in pharmaceuticals and food additives within a specific range.
　なお、酸化マグネシウムの用途として、肥料、食品、化粧品、医薬品原料のように、人体に直接あるいは間接的に摂取されたり、人体に接触する用途を想定する場合等においては、特に、酸化マグネシウムとして高純度のものが望まれる。 Magnesium oxide is particularly useful when it is used directly or indirectly, such as fertilizer, food, cosmetics, and pharmaceutical raw materials, or when it is intended to be in contact with the human body. A pure one is desired.
特開２００３－１４６８８９号公報JP 2003-146889 A ＷＯ２０１１／０３０６５９号パンフレットWO2011 / 030659 pamphlet 特開２００９－１３１１３号公報JP 2009-13113 A ＷＯ２０１５／１２８９４０号パンフレットWO2015 / 128940 pamphlet
　本発明の目的は、優れた溶出性を有する酸化マグネシウム（顆粒）、その製造方法及び前記酸化マグネシウム（顆粒）を含む錠剤を提供することにある。 An object of the present invention is to provide magnesium oxide (granule) having excellent dissolution properties, a method for producing the same, and a tablet containing the magnesium oxide (granule).
　本発明の他の目的は、製造不良（欠け、割れなど）の少ない酸化マグネシウム（顆粒）、その製造方法及び前記酸化マグネシウム（顆粒）を含む錠剤を提供することにある。 Another object of the present invention is to provide magnesium oxide (granule) with few production defects (chips, cracks, etc.), a method for producing the same, and a tablet containing the magnesium oxide (granule).
　本発明のさらに他の目的は、高純度を保持しつつ、溶出性や製造不良を改善できる酸化マグネシウム（顆粒）、その製造方法及び前記酸化マグネシウム（顆粒）を含む錠剤を提供することにある。 Still another object of the present invention is to provide magnesium oxide (granule) that can improve dissolution and poor production while maintaining high purity, a method for producing the same, and a tablet containing the magnesium oxide (granule).
　本発明の別の目的は、上記のような酸化マグネシウム（顆粒）を効率よく製造する方法を提供することにある。 Another object of the present invention is to provide a method for efficiently producing the above magnesium oxide (granule).
　本発明者らは、特許文献４の酸化マグネシウム顆粒について検討したが、錠剤における重要な特性である溶出性に改善の余地があることがわかった。また、錠剤の欠けや割れという点でも、さらなる改善の余地があることがわかった。 The present inventors examined the magnesium oxide granules of Patent Document 4, but found that there was room for improvement in the dissolution property, which is an important characteristic of tablets. It was also found that there was room for further improvement in terms of chipping and cracking of the tablets.
　一方、前記のように、医薬品や食品用途などでは、特に、高純度であることが要求されるが、本発明者らの検討によれば、不純物量と溶出性や製造不良とは関連性がなく、単に、不純物量を高レベルに低減するだけでは、溶出性や製造不良を改善しがたいことがわかった。 On the other hand, as described above, high purity is particularly required for pharmaceuticals and food applications, but according to the study by the present inventors, there is a relationship between the amount of impurities and elution and manufacturing defects. However, it was found that it is difficult to improve elution and manufacturing defects simply by reducing the amount of impurities to a high level.
　このような中、上記課題を解決するため、本発明者らは鋭意研究を行った結果、酸化マグネシウム（ＭｇＯ）顆粒におけるマグネシウム以外の種々の元素のうち、意外にも、Ｂ（ホウ素）及びＣａ（カルシウム）が溶出性や製造不良に関連していることを突き止め、これらの含有量を特定の範囲に調整すること、さらには、あえて９９％超といった超高純度とはせず、十分に医薬品用途等にも適用しうる所定の高純度範囲に調整することにより、錠剤において、酸化マグネシウムの溶出性や製造不良を効率よく改善できること（特にこれらを両立させて改善できること）を見出し、さらなる検討を重ねて本発明を完成した。 Under such circumstances, in order to solve the above-mentioned problems, the present inventors have conducted intensive studies. As a result, among various elements other than magnesium in magnesium oxide (MgO) granules, surprisingly, B (boron) and Ca Finding out that (calcium) is related to elution and manufacturing defects, adjusting the content of these to a specific range, and not dare to make it ultra-high purity of over 99%. By adjusting to a predetermined high purity range that can be applied to applications, etc., it was found that the dissolution of magnesium oxide and manufacturing defects can be efficiently improved in tablets (especially that both can be improved simultaneously), and further investigation The present invention was completed again.
　すなわち、本発明には、Ｂ（ホウ素）の含有量が０．０５重量％以下、Ｃａ（カルシウム）の含有量が０．０３～１．８重量％、純分（Assay）が９５～９９％である酸化マグネシウム（顆粒）が含まれる。 That is, the present invention has a B (boron) content of 0.05% by weight or less, a Ca (calcium) content of 0.03 to 1.8% by weight, and a pure content (Assay) of 95 to 99%. This includes magnesium oxide (granule).
　このような酸化マグネシウムにおいて、ＢＥＴ比表面積は、例えば、５～６０ｍ２／ｇ程度であってもよい。 In such magnesium oxide, the BET specific surface area may be, for example, about 5 to 60 m 2 / g.
　本発明の代表的な酸化マグネシウムには、Ｂの含有量が０．０３重量％以下、Ｃａの含有量が０．０５～１．５重量％、純分（Assay）が９６～９９％、ＢＥＴ比表面積が１０～５０ｍ２／ｇである酸化マグネシウム（顆粒）が含まれる。 The representative magnesium oxide of the present invention has a B content of 0.03% by weight or less, a Ca content of 0.05 to 1.5% by weight, an purity of 96 to 99%, BET Magnesium oxide (granule) having a specific surface area of 10 to 50 m 2 / g is included.
　酸化マグネシウムは、海水に由来してもよい。 Magnesium oxide may be derived from seawater.
　また、本発明には、以下の（１）及び／又は（２）を充足する、動物に直接的又は間接的に摂取又は接触させる用途（例えば、食品用、医薬品用及び化粧品用から選択された少なくとも１種の用途）に使用するための酸化マグネシウム（顆粒）を含む。
　（１）Ｂの含有量が０．０５重量％以下
　（２）Ｃａの含有量が０．０３～１．８重量％ In addition, the present invention satisfies the following (1) and / or (2), and is used directly or indirectly for ingestion or contact with animals (for example, selected from food use, pharmaceutical use and cosmetic use) Magnesium oxide (granules) for use in at least one application.
(1) B content is 0.05% by weight or less (2) Ca content is 0.03 to 1.8% by weight
　このような酸化マグネシウムの純分（Assay）は、特に９５～９９％程度であってもよい。 Such magnesium oxide may have a purity of about 95 to 99%.
　本発明には、上記の酸化マグネシウム（顆粒）を製造する方法も含む。このような方法は、海水からＢを除去する工程を少なくとも含んでいてもよい。このような方法では、キレート樹脂により海水からＢを除去してもよい。 The present invention includes a method for producing the above magnesium oxide (granule). Such a method may include at least a step of removing B from seawater. In such a method, B may be removed from seawater with a chelate resin.
　本発明には、前記酸化マグネシウム（顆粒）を含む錠剤も包含する。 The present invention includes a tablet containing the magnesium oxide (granule).
　本発明では、Ｂの含有量、Ｃａの含有量、純分を調整することにより、酸化マグネシウムやそれを含む錠剤を改良できる。
　そのため、本発明には、例えば、下記の方法も包含する。 In the present invention, magnesium oxide and tablets containing it can be improved by adjusting the B content, Ca content, and pure content.
Therefore, for example, the following method is also included in the present invention.
　酸化マグネシウム（顆粒）におけるＢの含有量を０．０５重量％以下に調整し、酸化マグネシウム顆粒を含む錠剤の溶出性を向上又は改善する方法。 A method for improving or improving the dissolution properties of tablets containing magnesium oxide granules by adjusting the B content in the magnesium oxide (granules) to 0.05% by weight or less.
　酸化マグネシウム（顆粒）におけるＣａの含有量を０．０３～１．８重量％に調整し、酸化マグネシウム（顆粒）を含む錠剤の製造不良（例えば、錠剤の欠け及び／又は割れ）を低減する方法。 Method of adjusting Ca content in magnesium oxide (granule) to 0.03 to 1.8% by weight to reduce defective production (for example, chipping and / or cracking of tablet) containing magnesium oxide (granule) .
　酸化マグネシウム（顆粒）におけるＢの含有量を０．０３重量％以下、Ｃａの含有量を０．０５～１．５重量％、純分（Assay）を９５～９９％に調整し、酸化マグネシウム（顆粒）を含む錠剤の溶出性を向上又は改善するとともに、製造不良（例えば、錠剤の欠け及び／又は割れ）を低減する方法。 In the magnesium oxide (granule), the B content is adjusted to 0.03% by weight or less, the Ca content is adjusted to 0.05 to 1.5% by weight, and the pure content (Assay) is adjusted to 95 to 99%. A method of improving or improving the dissolution property of a tablet containing granules) and reducing manufacturing defects (for example, chipping and / or cracking of the tablet).
　本発明では、優れた溶出性を有する酸化マグネシウム（顆粒）を提供できる。 In the present invention, magnesium oxide (granule) having excellent dissolution properties can be provided.
　また、本発明では、製造不良（欠け、割れなど）の少ない酸化マグネシウム（顆粒）を提供することもできる。 Also, in the present invention, magnesium oxide (granule) with few manufacturing defects (chips, cracks, etc.) can be provided.
　特に、このような酸化マグネシウムでは、高純度（９５％以上、好ましくは９６％以上）を保持しつつ、溶出性や製造不良を改善できる。また、溶出性や製造不良を改善しても、錠剤硬度を損なうことがなく、溶出性や製造不良の改善と、高硬度とを両立させることもできる。 In particular, such magnesium oxide can improve elution and production defects while maintaining high purity (95% or more, preferably 96% or more). Moreover, even if the dissolution property and the manufacturing defect are improved, the tablet hardness is not impaired, and the improvement of the dissolution property and the manufacturing defect and the high hardness can be achieved at the same time.
　そのため、本発明の酸化マグネシウムや酸化マグネシウム錠剤は、動物（特にヒト）に直接的又は間接的に摂取又は接触させる用途（例えば、肥料、食品、医薬品、化粧品など）において、特に有用である。 Therefore, the magnesium oxide and magnesium oxide tablet of the present invention are particularly useful in applications (for example, fertilizers, foods, pharmaceuticals, cosmetics, etc.) that are ingested or contacted directly or indirectly with animals (particularly humans).
　また、本発明では、上記のような酸化マグネシウム（顆粒）を効率よく製造する方法を提供できる。特に、このような方法では、海水のような原料を使用できるため、簡易（しかも安価）に製造でき、極めて有用性・実用性が高い。 Further, in the present invention, a method for efficiently producing the above magnesium oxide (granule) can be provided. In particular, in such a method, since raw materials such as seawater can be used, it can be manufactured easily (and inexpensively), and is extremely useful and practical.
　［酸化マグネシウム］
　本発明の酸化マグネシウムは、特定のＢ（ホウ素）及び／又はＣａ（カルシウム）含有量を充足する。 [Magnesium oxide]
The magnesium oxide of the present invention satisfies a specific B (boron) and / or Ca (calcium) content.
　酸化マグネシウム中のＢの含有量（含有割合）は、例えば、０．１重量％以下（例えば、０．０８重量％以下）、好ましくは０．０５重量％以下（例えば、０．０４重量％以下）、さらに好ましくは０．０３重量％以下（例えば、０．０２重量％以下）、特に０．０１５重量％以下であってもよい。 The content (content ratio) of B in magnesium oxide is, for example, 0.1% by weight or less (for example, 0.08% by weight or less), preferably 0.05% by weight or less (for example, 0.04% by weight or less). ), More preferably 0.03% by weight or less (for example, 0.02% by weight or less), and particularly 0.015% by weight or less.
　なお、Ｂの含有量の下限値は、特に制限されず、例えば、０重量％（又は検出限界）であってもよく、０．００００１重量％、０．０００１重量％、０．００１重量％などであってもよい。
　なお、これらの数値を適宜組み合わせて適当な範囲を設定してもよい（例えば、０．００００１～０．０５重量％など、以下数値の記載について同じ）。 The lower limit of the content of B is not particularly limited, and may be, for example, 0% by weight (or detection limit), such as 0.00001% by weight, 0.0001% by weight, 0.001% by weight, etc. It may be.
An appropriate range may be set by appropriately combining these numerical values (for example, 0.00001 to 0.05% by weight, etc., and the following description of numerical values is the same).
　酸化マグネシウム中のＣａの含有量（含有割合）は、例えば、０．０３重量％以上（例えば、０．０３～２重量％）の範囲から選択でき、０．０３～１．８重量％（例えば、０．０４～１．６重量％）、好ましくは０．０５～１．５重量％（例えば、０．０８～１．５重量％）、さらに好ましくは０．１～１．５重量％（例えば、０．２～１．５重量％）、特に０．３～１．５重量％（例えば、０．４～１．５重量％）程度であってもよく、０．５重量％以上（例えば、０．５～１．５重量％）であってもよい。 The Ca content (content ratio) in the magnesium oxide can be selected from the range of 0.03% by weight or more (for example, 0.03 to 2% by weight), for example, 0.03 to 1.8% by weight (for example, 0.04 to 1.6% by weight), preferably 0.05 to 1.5% by weight (eg 0.08 to 1.5% by weight), more preferably 0.1 to 1.5% by weight ( For example, it may be about 0.2 to 1.5% by weight), particularly about 0.3 to 1.5% by weight (for example, 0.4 to 1.5% by weight), and 0.5% by weight or more ( For example, it may be 0.5 to 1.5% by weight).
　なお、酸化マグネシウムは、上記Ｂ含有量の範囲及びＣａ含有量の範囲をいずれも充足するのが好ましいが、これらのいずれか一方を充足する限り、必ずしも他方の含有割合を充足しなくてもよい。 In addition, although it is preferable that magnesium oxide satisfy | fills both the range of said B content, and the range of Ca content, as long as either of these is satisfied, it is not necessary to satisfy the content rate of the other. .
　本発明の酸化マグネシウムは、Ｍｇ、Ｂ及びＣａ以外の元素を含んでいてもよい。このような元素としては、特に、限定されないが、非金属元素［例えば、Ｃ（炭素）、Ｓ（硫黄）、ハロゲン（例えば、Ｃｌ（塩素）など）など］、金属元素又は半金属元素［例えば、典型金属元素（例えば、Ｎａ（ナトリウム）などのアルカリ又はアルカリ土類金属；Ａｌ（アルミニウム）、Ｓｉ（ケイ素）など）、遷移金属元素（例えば、Ｆｅ（鉄）、Ｚｎ（亜鉛）など）など］などが挙げられる。これらの元素は、単独で又は２種以上組み合わせて酸化マグネシウムに含有されていてもよい。 The magnesium oxide of the present invention may contain elements other than Mg, B and Ca. Examples of such elements include, but are not limited to, non-metallic elements [for example, C (carbon), S (sulfur), halogen (for example, Cl (chlorine), etc.)], metal elements or metalloid elements [for example, Typical metal elements (for example, alkali or alkaline earth metals such as Na (sodium); Al (aluminum), Si (silicon), etc.), transition metal elements (for example, Fe (iron), Zn (zinc), etc.), etc. ] Etc. are mentioned. These elements may be contained in magnesium oxide alone or in combination of two or more.
　これらのうち、代表的な元素は、ケイ素、ナトリウム、ハロゲン（塩素など）などである。このような元素を含む酸化マグネシウムは、例えば、海水に由来してもよい。本発明では、このような他の元素を含んでいても、所望の物性・特性（優れた溶出性、少ない製造不良など）を得ることができる。 Of these, typical elements are silicon, sodium, halogen (such as chlorine), and the like. Magnesium oxide containing such an element may be derived from seawater, for example. In the present invention, desired physical properties / characteristics (excellent elution properties, few manufacturing defects, etc.) can be obtained even when such other elements are contained.
　なお、酸化マグネシウム中の他の元素の含有量は、元素の種類等に応じて適宜選択できる。例えば、ケイ素の含有量は、例えば、０．００１重量％以上（例えば、０．００１～０．１重量％）、好ましくは０．００５～０．０７重量％、さらに好ましくは０．０１～０．０５重量％程度であってもよい。 It should be noted that the content of other elements in the magnesium oxide can be appropriately selected according to the type of element. For example, the silicon content is, for example, 0.001% by weight or more (eg, 0.001 to 0.1% by weight), preferably 0.005 to 0.07% by weight, and more preferably 0.01 to 0%. It may be about 0.05% by weight.
　また、ナトリウムの含有量は、例えば、０．０００１重量％以上（例えば、０．０００１～０．１重量％）、好ましくは０．０００５～０．０５重量％、さらに好ましくは０．００１～０．０１重量％程度であってもよい。 The sodium content is, for example, 0.0001% by weight or more (eg, 0.0001 to 0.1% by weight), preferably 0.0005 to 0.05% by weight, and more preferably 0.001 to 0%. It may be about 0.01% by weight.
　さらに、塩素の含有量は、例えば、０．０００１重量％以上（例えば、０．０００１～０．１重量％）、好ましくは０．０００５～０．０５重量％、さらに好ましくは０．００１～０．０１重量％程度であってもよい。 Further, the chlorine content is, for example, 0.0001% by weight or more (eg, 0.0001 to 0.1% by weight), preferably 0.0005 to 0.05% by weight, and more preferably 0.001 to 0%. It may be about 0.01% by weight.
　なお、用途等によっては、鉛やヒ素などの元素は極力少ないのが好ましく、例えば、酸化マグネシウムにおいて、Ｐｂ（鉛）の含有量は１ｐｐｍ以下（例えば、０．１ｐｐｍ程度）であってもよく、Ａｓ（ヒ素）の含有量は４ｐｐｍ以下（例えば、１ｐｐｍ程度）であってもよい。 Depending on applications, it is preferable that elements such as lead and arsenic are as low as possible. For example, in magnesium oxide, the content of Pb (lead) may be 1 ppm or less (for example, about 0.1 ppm), The content of As (arsenic) may be 4 ppm or less (for example, about 1 ppm).
　なお、酸化マグネシウム中における各元素の割合は、例えば、ＩＣＰ発光分光分析法（ＩＣＰ－ＡＥＳ法）、ＩＣＰ質量分析法（ＩＣＰ－ＭＳ法）などにより測定できる。 The ratio of each element in magnesium oxide can be measured by, for example, ICP emission spectroscopy (ICP-AES method), ICP mass spectrometry (ICP-MS method), or the like.
　酸化マグネシウムの純度は、特に限定されないが、用途によっては高純度であることが要求される場合がある。一方、高純度でありすぎると、所望の物性・特性を損なうおそれがある。 The purity of magnesium oxide is not particularly limited, but may be required to be high purity depending on the application. On the other hand, if the purity is too high, desired physical properties and characteristics may be impaired.
　このような観点から、酸化マグネシウムの純分（Assay）は、高純度範囲、例えば、９０％以上（例えば、９３～９９．５％）の範囲から選択でき、好ましくは９５％以上（例えば、９５～９９％）、さらに好ましくは９６～９９％（例えば、９６．３～９８．５％）、特に９６～９８％であってもよい。 From such a viewpoint, the purity of magnesium oxide can be selected from a high purity range, for example, 90% or more (eg, 93 to 99.5%), and preferably 95% or more (eg, 95%). To 99%), more preferably 96 to 99% (for example, 96.3 to 98.5%), particularly 96 to 98%.
　なお、純分は、例えば、米国薬局方（ＵＳＰ）に従って決定してもよい。具体的には、８００－９００℃±２５℃で恒量焼成し、恒量となった酸化マグネシウムを３２０ｍｇ量りとり、２Ｎ塩酸を２０ｍｌ加えて溶解させ１００ｍｌとし、ここから２０ｍｌをとり、緩衝液及びＥＢＴ指示薬を加え、０．１ｍｏｌ/ＬのＥＤＴＡ標準液で滴定することにより求めてもよい。 In addition, you may determine a pure part according to the US Pharmacopoeia (USP), for example. Specifically, constant weight firing at 800-900 ° C. ± 25 ° C., 320 mg of the constant magnesium oxide was weighed, 20 ml of 2N hydrochloric acid was added and dissolved to make 100 ml, and 20 ml was taken from this, buffer solution and EBT indicator And titration with a 0.1 mol / L EDTA standard solution.
　酸化マグネシウムのＢＥＴ比表面積は、例えば、１～１００ｍ２／ｇ（例えば、３～８０ｍ２／ｇ）程度の範囲から選択でき、好ましくは５～６０ｍ２／ｇ（例えば、８～５５ｍ２／ｇ）、さらに好ましくは１０～５０ｍ２／ｇ（例えば、１２～４５ｍ２／ｇ）、特に１５～４０ｍ２／ｇ（例えば、２０～３５ｍ２／ｇ）程度であってもよい。 The BET specific surface area of magnesium oxide can be selected from a range of, for example, about 1 to 100 m 2 / g (for example, 3 to 80 m 2 / g), and preferably 5 to 60 m 2 / g (for example, 8 to 55 m 2 / g). ), More preferably 10 to 50 m 2 / g (for example, 12 to 45 m 2 / g), particularly about 15 to 40 m 2 / g (for example, 20 to 35 m 2 / g).
　なお、ＢＥＴ比表面積の測定方法は、通常この分野で用いられる方法であればよく、特に限定されないが、例えば、窒素吸着法であってもよい。具体的には、例えば、前処理として窒素ガス雰囲気下で加熱処理した測定試料（酸化マグネシウム顆粒）を、ＢＥＴ比表面積測定装置にて窒素ガス吸着法で測定してもよい。前処理は、例えば、窒素ガス雰囲気下、約１３０℃で約３０分間としてもよい。前処理を行う際に用いる装置及びＢＥＴ比表面積測定装置は、特に限定されず、通常この分野で用いられるいずれの装置を用いてもよい。 The method for measuring the BET specific surface area is not particularly limited as long as it is a method usually used in this field. For example, a nitrogen adsorption method may be used. Specifically, for example, a measurement sample (magnesium oxide granule) heat-treated in a nitrogen gas atmosphere as a pretreatment may be measured by a nitrogen gas adsorption method with a BET specific surface area measuring device. The pretreatment may be performed, for example, at about 130 ° C. for about 30 minutes in a nitrogen gas atmosphere. The apparatus and the BET specific surface area measuring apparatus used for the pretreatment are not particularly limited, and any apparatus normally used in this field may be used.
　ＢＥＴ比表面積を上記のような範囲に調整することで、溶出性や製造不良の改善効果を損なうことなく、錠剤における硬度を高いものとしやすいようである。 It seems that by adjusting the BET specific surface area to the above range, it is easy to increase the hardness of the tablet without impairing the improvement effect of dissolution property and manufacturing failure.
　酸化マグネシウムのかさ密度は、例えば、７００～１２００ｇ／Ｌ、好ましくは８５０～１０００ｇ／Ｌ、さらに好ましくは９００～９５０ｇ／Ｌ程度であってもよい。
　なお、かさ密度は、日本薬局方に規定されるかさ密度であってもよい。 The bulk density of magnesium oxide may be, for example, about 700 to 1200 g / L, preferably about 850 to 1000 g / L, and more preferably about 900 to 950 g / L.
The bulk density may be a bulk density specified by the Japanese Pharmacopoeia.
　酸化マグネシウムの形状は、通常、顆粒（粒状、粉状又は粉粒状）であってもよい。また、酸化マグネシウムの平均粒径は、特に限定されず、用途等に応じて選択でき、例えば、２００～７００μｍ、好ましくは２５０～６００μｍ、さらに好ましくは３００～５００μｍ程度であってもよい。
　粒径（最小径～最大径）の範囲は、特に限定されず、用途等に応じて選択できるが、例えば、溶出性などの観点から、１００～８５０μｍ、好ましくは１５０～５００μｍ、さらに好ましくは２５０～３５０μｍ程度であってもよい。なお、粒径は、例えば、ふるい振とう器によって、測定してもよい。 The shape of the magnesium oxide may be usually a granule (granular, powdery or granular). Further, the average particle diameter of magnesium oxide is not particularly limited and can be selected according to the use and the like, and may be, for example, about 200 to 700 μm, preferably about 250 to 600 μm, and more preferably about 300 to 500 μm.
The range of the particle diameter (minimum diameter to maximum diameter) is not particularly limited and can be selected depending on the application. For example, from the viewpoint of elution, 100 to 850 μm, preferably 150 to 500 μm, and more preferably 250 It may be about 350 μm. In addition, you may measure a particle size with a sieve shaker, for example.
　本発明の酸化マグネシウムの製造方法は、上記のような特性・物性が得られる限り、特に限定されず、慣用の方法を利用してもよい。 The method for producing magnesium oxide of the present invention is not particularly limited as long as the above characteristics and physical properties can be obtained, and a conventional method may be used.
　特に、本発明の酸化マグネシウムは、マグネシウム源にアルカリを加えて水酸化マグネシウムを得る工程（水酸化マグネシウム生成工程）と、得られた水酸化マグネシウムを焼成して酸化マグネシウムを得る工程（焼成工程）とを経て、製造するのが好ましい。 In particular, the magnesium oxide of the present invention includes a step of obtaining magnesium hydroxide by adding an alkali to a magnesium source (magnesium hydroxide production step), and a step of firing the obtained magnesium hydroxide to obtain magnesium oxide (firing step). It is preferable to manufacture through these.
　水酸化マグネシウム生成工程において、マグネシウム源としては、海水、塩化マグネシウム水溶液（かん水）などが挙げられ、特に、海水を好適に使用してもよい。海水を使用することで、カルシウムを所定の濃度で有する酸化マグネシウムを得やすい。 In the magnesium hydroxide generation step, examples of the magnesium source include seawater, magnesium chloride aqueous solution (brine), and seawater may be particularly preferably used. By using seawater, it is easy to obtain magnesium oxide having a predetermined concentration of calcium.
　なお、マグネシウム源の種類にもよるが、前記のようにＢ（ホウ素）含有量が少ない酸化マグネシウムを得る場合に、マグネシウム源として、予めＢ含有量が低減されたものを使用してもよい。特に、マグネシウム源として、ホウ素が除去された海水を使用してもよい。 Although depending on the type of the magnesium source, when magnesium oxide having a low B (boron) content is obtained as described above, a magnesium source having a previously reduced B content may be used. In particular, seawater from which boron has been removed may be used as the magnesium source.
　このような場合、本発明の製造方法は、マグネシウム源（特に海水）からホウ素を除去（又は分離）する工程（ホウ素分離工程）を少なくとも含んでいてもよい。 In such a case, the production method of the present invention may include at least a step (boron separation step) of removing (or separating) boron from a magnesium source (particularly seawater).
　ホウ素分離工程において、ホウ素を除去する方法としては、特に限定されないが、例えば、キレート樹脂によりマグネシウム源からＢを除去（分離）してもよい。具体的には、マグネシウム源（海水）をキレート樹脂に通過（通水）させることで、Ｂを除去できる。 In the boron separation step, the method for removing boron is not particularly limited. For example, B may be removed (separated) from the magnesium source with a chelate resin. Specifically, B can be removed by passing a magnesium source (seawater) through the chelate resin (water flow).
　キレート樹脂としては、例えば、キレート官能基（例えば、Ｎ－メチレングルカミンなど）を有する樹脂（例えば、スチレン－ジビニルベンゼン共重合体、セルロースなど）などが挙げられる。なお、キレート樹脂（キレート繊維）の市販品としては、キレスト社などから入手できる。 Examples of the chelate resin include resins having a chelate functional group (eg, N-methylene glucamine) (eg, styrene-divinylbenzene copolymer, cellulose). In addition, as a commercial item of chelate resin (chelate fiber), it can obtain from Kyrest company.
　水酸化マグネシウム生成工程において、アルカリとしては、特に限定されないが、代表的には、水酸化カルシウム源を使用してもよい。特に、水酸化カルシウム源は、消石灰であってもよく、消石灰は石灰乳の形態であってもよい。水酸化カルシウム源を使用することで、カルシウムを所定の濃度で有する酸化マグネシウムを得やすい。 In the magnesium hydroxide production step, the alkali is not particularly limited, but typically a calcium hydroxide source may be used. In particular, the calcium hydroxide source may be slaked lime, and the slaked lime may be in the form of lime milk. By using a calcium hydroxide source, it is easy to obtain magnesium oxide having calcium at a predetermined concentration.
　焼成工程において、焼成温度は、特に限定されないが、例えば、５００～２０００℃、好ましくは６００～１５００℃、さらに好ましくは７００～１２００℃程度であってもよい。また、焼成時間も適宜選択でき、例えば、１０分～１０時間、好ましくは３０分～５時間、さらに好ましくは１～３時間程度であってもよい。 In the firing step, the firing temperature is not particularly limited, but may be, for example, about 500 to 2000 ° C., preferably 600 to 1500 ° C., more preferably about 700 to 1200 ° C. The firing time can also be appropriately selected, and may be, for example, 10 minutes to 10 hours, preferably 30 minutes to 5 hours, and more preferably about 1 to 3 hours.
　焼成工程で得られた酸化マグネシウムは、所望の形状（例えば、顆粒状）に応じて、通常、粉砕してもよい。そのため、本発明の方法は、焼成工程後、さらに、焼成工程で得られた酸化マグネシウムを粉砕する粉砕工程を含んでいてもよい。 The magnesium oxide obtained in the firing step may be usually pulverized according to a desired shape (for example, a granular shape). Therefore, the method of the present invention may further include a pulverization step of pulverizing the magnesium oxide obtained in the calcination step after the calcination step.
　なお、焼成工程で得られた酸化マグネシウムの焼成状態は、軽焼（軽焼状態）であるのが好ましい。このような軽焼状態の酸化マグネシウム（軽焼マグネシウム）の活性度は、例えば、ＢＥＴ比表面積で、数～数百ｍ２／ｇ程度（例えば、１～３００ｍ２／ｇ、好ましくは２～１００ｍ２／ｇ程度）であってもよい。 In addition, it is preferable that the baking state of the magnesium oxide obtained at the baking process is light baking (light baking state). The activity of such lightly burned magnesium oxide (lightly burned magnesium) is, for example, about several to several hundreds m 2 / g (for example, 1 to 300 m 2 / g, preferably 2 to 100 m in terms of BET specific surface area). 2 / g).
　粉砕工程では、必要に応じて酸化マグネシウムを加圧し、粉砕処理してもよい。加圧条件は適宜選択でき、加圧装置も特に限定されず、ローラーコンパクター等を用いてもよい。 In the pulverization step, magnesium oxide may be pressurized and pulverized as necessary. The pressing conditions can be selected as appropriate, and the pressing device is not particularly limited, and a roller compactor or the like may be used.
　粉砕方法は、特に限定されず、例えば、グラニュレーターを用いて粉砕してもよい。前記グラニュレーターとしては、特に限定されないが、例えば、ロールグラニュレーターが挙げられる。粉砕方法は、具体的には、ロールを縦に３段セットしたロールグラニュレーターを用いて、回転させたロールの隙間に加圧した酸化マグネシウムを通過させて粉砕させる方法であってもよい。 The pulverization method is not particularly limited, and for example, pulverization may be performed using a granulator. Although it does not specifically limit as said granulator, For example, a roll granulator is mentioned. Specifically, the pulverization method may be a method in which magnesium oxide pressurized is passed through a gap between the rotated rolls and pulverized using a roll granulator in which the rolls are set in three vertical stages.
　なお、粉砕後の酸化マグネシウム（顆粒）は、必要に応じて、篩別などにより、粒径又は粒度を揃えてもよい。 In addition, the pulverized magnesium oxide (granules) may have the same particle size or particle size by sieving as necessary.
　本発明の酸化マグネシウム（顆粒）の用途は、特に限定されず、種々の用途［例えば、
顔料、ゴム用添加剤（加硫促進剤など）、肥料、食品、化粧品、医薬品など］）に使用できる。 The use of the magnesium oxide (granule) of the present invention is not particularly limited, and various uses [for example,
Pigments, rubber additives (vulcanization accelerators, etc.), fertilizers, foods, cosmetics, pharmaceuticals, etc.].
　特に、本発明では、高純度の酸化マグネシウムを得ることができるため、特に、本発明の酸化マグネシウム（顆粒）や錠剤は、動物に直接的又は間接的に摂取又は接触させる用途（例えば、食品用、医薬品用、化粧品用、肥料用など）などとして好適である。 In particular, in the present invention, high-purity magnesium oxide can be obtained. In particular, the magnesium oxide (granule) and tablet of the present invention are used for ingesting or contacting animals directly or indirectly (for example, for foods). , For pharmaceuticals, cosmetics, fertilizers, etc.).
　なお、食品は、健康食品を含む一般食品の他、特定保健用食品、栄養機能食品などの保健機能食品も含む。また、食品には、サプリメント（栄養補助食品）、飼料なども含まれる。 In addition, food includes health foods such as foods for specified health use and functional foods for nutrition, in addition to general foods including health foods. In addition, the food includes supplements (dietary supplements), feed and the like.
　［錠剤］
　本発明の酸化マグネシウムは、用途等に応じて、所望の形態に成形してもよく、特に錠剤を構成してもよい。すなわち、本発明の酸化マグネシウム（錠剤）は、錠剤用（例えば、直打錠用）であってもよい。そのため、本発明には、前記酸化マグネシウムを含む錠剤を包含する。 [tablet]
The magnesium oxide of the present invention may be formed into a desired form according to the use or the like, and may particularly constitute a tablet. That is, the magnesium oxide (tablet) of the present invention may be for tablets (for example, for direct compression tablets). Therefore, this invention includes the tablet containing the said magnesium oxide.
　錠剤は、酸化マグネシウムを含んでいればよく、用途に応じて、慣用の添加剤（結合剤、崩壊剤など）ととともに形成してもよい。 Tablets need only contain magnesium oxide, and may be formed with conventional additives (such as binders and disintegrants) depending on the application.
　結合剤としては、特に限定されないが、例えば、カルボキシメチルセルロースナトリウム、低置換度ヒドロキシプロピルセルロース、結晶セルロース、デンプン（例えば、トウモロコシデンプン）などが挙げられる。 The binder is not particularly limited, and examples thereof include sodium carboxymethyl cellulose, low-substituted hydroxypropyl cellulose, crystalline cellulose, starch (for example, corn starch) and the like.
　また、崩壊剤としては、特に限定されないが、例えば、カルボキシメチルセルロースカルシウム、カルメロース、低置換度ヒドロキシプロピルセルロース、クロスカルメロースナトリウム、カルメロースカルシウム、カルボキシスターチナトリウムなどが挙げられる。 Further, the disintegrant is not particularly limited, and examples thereof include carboxymethylcellulose calcium, carmellose, low-substituted hydroxypropylcellulose, croscarmellose sodium, carmellose calcium, and carboxystarch sodium.
　また、錠剤は、さらに、賦形剤、滑沢剤等を含有してもよい。賦形剤としては、特に限定されないが、例えば、乳糖、白糖、マンニトール、コーンスターチ、結晶セルロースなどが挙げられる。また、滑沢剤としては、特に限定されないが、例えば、ショ糖脂肪酸エステル、ポリエチレングリコール、タルク、ステアリン酸又はステアリン酸塩（Ｎａ、Ｍｇ、又はＣａ塩）などが挙げられる。 Further, the tablet may further contain an excipient, a lubricant and the like. The excipient is not particularly limited, and examples thereof include lactose, sucrose, mannitol, corn starch, and crystalline cellulose. Further, the lubricant is not particularly limited, and examples thereof include sucrose fatty acid ester, polyethylene glycol, talc, stearic acid or stearate (Na, Mg, or Ca salt).
　さらに、錠剤は、所望により可塑剤、コーティング剤、凝集防止剤、可溶化剤、甘味料、酸味料、矯味料、ｐＨ調整剤、溶解補助剤、着色料、香料、ミネラル源（例えば、炭酸カルシウムなどのカルシウム源など）等の添加剤を１以上含有してもよい。 In addition, tablets may optionally contain plasticizers, coating agents, anti-aggregation agents, solubilizers, sweeteners, sour agents, corrigents, pH adjusters, solubilizers, colorants, flavors, mineral sources (eg, calcium carbonate). One or more additives such as a calcium source) may be contained.
　可塑剤としては、例えば、クエン酸トリエチル、グリセリン脂肪酸エステル、ポリエチレングリコール等があげられる。コーティング剤としては、例えば、エチルセルロース、ヒドロキシプロピルメチルセルロースなどがあげられる。凝集防止剤としては、例えば、タルク、ステアリン酸カルシウムなどがあげられる。可溶化剤としては、例えば、ショ糖脂肪酸エステル、モノステアリン酸ソルビタン、ラウリル硫酸ナトリウムなどがあげられる。甘味料としては、例えば、アスパルテーム、サッカリン、グリチルリチン酸二カリウム、ステビアなどがあげられる。酸味料（有機酸）としては、例えば、クエン酸、リンゴ酸、アスコルビン酸、フマル酸などがあげられる。矯味剤としては、例えば、ｌ－メントール、塩化ナトリウム、アセスルファムカリウム、スクラロースなどがあげられる。ｐＨ調整剤としては、例えば、クエン酸塩、リン酸塩、炭酸塩、酢酸塩などがあげられる。溶解補助剤としては、例えば、シクロデキストリン、アルギニン、リジン、トリスアミノメタンなどがあげられる。着色料としては、例えば、黄色三二酸化鉄、三二酸化鉄、銅クロロフィリンナトリウムなどがあげられる。香料としては、例えば、オレンジ油、レモン油、ハッカ油、ユーカリ油等があげられる。 Examples of the plasticizer include triethyl citrate, glycerin fatty acid ester, polyethylene glycol and the like. Examples of the coating agent include ethyl cellulose and hydroxypropyl methyl cellulose. Examples of the aggregation inhibitor include talc and calcium stearate. Examples of the solubilizer include sucrose fatty acid ester, sorbitan monostearate, sodium lauryl sulfate and the like. Examples of the sweetener include aspartame, saccharin, dipotassium glycyrrhizinate, stevia and the like. Examples of the acidulant (organic acid) include citric acid, malic acid, ascorbic acid, and fumaric acid. Examples of the corrigent include l-menthol, sodium chloride, acesulfame potassium, sucralose and the like. Examples of the pH adjuster include citrate, phosphate, carbonate, acetate, and the like. Examples of the solubilizer include cyclodextrin, arginine, lysine, trisaminomethane and the like. Examples of the colorant include yellow iron sesquioxide, iron sesquioxide, and copper chlorophyllin sodium. Examples of the fragrance include orange oil, lemon oil, mint oil, eucalyptus oil and the like.
　これらの添加剤は、それぞれ、単独で又は２種以上組み合わせてもよく、異なる添加剤を組み合わせてもよい。 These additives may be used alone or in combination of two or more, or different additives may be combined.
　添加剤の含有量（配合量、含有割合）は、添加剤の種類などに応じて適宜選択できる、例えば、結合剤の配合量は、特に限定されないが、例えば、錠剤中０．１～３０重量％、好ましくは０．５～２０重量％、さらに好ましくは１～１５重量％程度であってもよい。また、崩壊剤の配合量は、特に限定されないが、例えば、錠剤中０．１～３０重量％、好ましくは０．５～１０重量％、さらに好ましくは１～５重量％であってもよい。
　なお、錠剤において、酸化マグネシウム（顆粒）の割合は、用途等に応じて選択でき、特に限定されないが、例えば、５０重量％以上（例えば、６０重量％以上）、好ましくは７０重量％以上（例えば、７５重量％以上）であってもよく、８０重量％以上、８５重量％以上、９０重量％以上、９５重量％以上などであってもよい。 The content (mixing amount, content ratio) of the additive can be appropriately selected according to the type of the additive. For example, the blending amount of the binder is not particularly limited, but for example, 0.1 to 30 weight in the tablet %, Preferably 0.5 to 20% by weight, more preferably about 1 to 15% by weight. Further, the amount of the disintegrant is not particularly limited, but may be, for example, 0.1 to 30% by weight, preferably 0.5 to 10% by weight, more preferably 1 to 5% by weight in the tablet.
In the tablet, the proportion of magnesium oxide (granule) can be selected depending on the application and is not particularly limited. For example, it is 50% by weight or more (for example, 60% by weight or more), preferably 70% by weight or more (for example, 75 wt% or more), 80 wt% or more, 85 wt% or more, 90 wt% or more, or 95 wt% or more.
　錠剤の製造方法は、従来公知の方法に従ってよい。例えば、本発明の酸化マグネシウム錠剤は、酸化マグネシウム（顆粒）、結合剤及び崩壊剤（必要に応じてさらに他の添加剤）を混合し、錠剤化する（打錠する）ことにより製造してもよい。 The tablet production method may be in accordance with a conventionally known method. For example, the magnesium oxide tablet of the present invention can be produced by mixing magnesium oxide (granule), a binder and a disintegrant (and other additives as necessary) and tableting (tabletting). Good.
　打錠方法としては、特に限定されず、直打法（直接粉末圧縮法）、湿式顆粒圧縮法などであってもよいが、本発明では、特に直打法を好適に利用してもよい。 The tableting method is not particularly limited, and may be a direct compression method (direct powder compression method), a wet granule compression method, or the like. In the present invention, the direct compression method may be particularly preferably used.
　錠剤の強度は、用途に応じて選択できるが、例えば、５０Ｎ以上（例えば、５５～２００Ｎ）、好ましくは６０Ｎ以上（例えば、６５～１８０Ｎ）、さらに好ましくは７０Ｎ以上（例えば、７０～１５０Ｎ）、特に７５Ｎ以上（例えば、７５～１２０Ｎ）程度であってもよい。 The strength of the tablet can be selected depending on the application, but is, for example, 50 N or more (for example, 55 to 200 N), preferably 60 N or more (for example, 65 to 180 N), more preferably 70 N or more (for example, 70 to 150 N). In particular, it may be about 75N or more (for example, 75 to 120N).
　次に、実施例を挙げて本発明をさらに具体的に説明するが、本発明はこれらの実施例により何ら限定されるものではなく、多くの変形が本発明の技術的思想内で当分野において通常の知識を有する者により可能である。 EXAMPLES Next, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples at all, and many variations are within the technical idea of the present invention. This is possible by those with ordinary knowledge.
　なお各種物性・特性は以下のように測定又は評価した。 Various physical properties and characteristics were measured or evaluated as follows.
　不純物の分析方法（含有量）：ＩＣＰ－ＡＥＳ法によって測定した。 Impurity analysis method (content): Measured by ICP-AES method.
　純分（Ａｓｓａｙ）の測定方法：純分は、米国薬局方（Ｕｎｉｔｅｄ　Ｓｔａｔｅｓ　Ｐｈａｒｍａｃｏｐｅｉａ，ＵＳＰ）に従って測定した。 Method for measuring pure content: The pure content was measured according to the United States Pharmacopoeia (United States Pharmacopia, USP).
　ＢＥＴ比表面積の測定方法：窒素吸着法にて測定した。 BET specific surface area measurement method: Measured by nitrogen adsorption method.
　錠剤サンプルの成形方法：配合（酸化マグネシウム：７５％、結晶セルロース：１０％、軽質炭酸カルシウム：１０％、クロスカルメロースナトリウム：３％、ステアリン酸マグネシウム：１％、クエン酸：１％）にて、直径φ８ｍｍ、曲率半径Ｒ１０ｍｍの杵を装着したロータリー型打錠機にて、打錠圧５ｋＮで製錠し、１錠当たり重量３００ｍｇ、厚み４．０ｍｍの酸化マグネシウム錠剤を得た。 Tablet sample molding method: in combination (magnesium oxide: 75%, crystalline cellulose: 10%, light calcium carbonate: 10%, croscarmellose sodium: 3%, magnesium stearate: 1%, citric acid: 1%) The tablets were tableted at a tableting pressure of 5 kN using a rotary tableting machine equipped with a punch having a diameter of 8 mm and a radius of curvature of R10 mm to obtain magnesium oxide tablets having a weight of 300 mg and a thickness of 4.0 mm per tablet.
　溶出率の測定方法：溶出試験機（メーカー名：ＶＡＲＩＡＮ社製　ＶＫ７０２５）を用いて、日本薬局方に収載される溶出試験パドル法に準じて行った（試験液：日本薬局方崩壊試験法の第１液、液温度：３７℃、回転数：５０ｒｐｍ、測定時間：４５分）。溶出した酸化マグネシウムの量をＩＣＰ－ＡＥＳ法にて測定した。測定は３ベッセルで行い、その平均値を平均溶出率とした。 Dissolution rate measurement method: Using a dissolution tester (manufacturer: Varian 70, VK7025), the dissolution test was performed according to the dissolution test paddle method listed in the Japanese Pharmacopoeia (test solution: No. 1 liquid, liquid temperature: 37 degreeC, rotation speed: 50 rpm, measurement time: 45 minutes). The amount of magnesium oxide eluted was measured by ICP-AES method. The measurement was performed with 3 vessels, and the average value was defined as the average dissolution rate.
　錠剤硬度の測定方法：錠剤破壊強度測定器（富山産業：ＴＨ３０３ＭＰ）を用いて錠剤硬度を測定した。錠剤１０粒測定して、その平均値を求めた。 Tablet hardness measurement method: Tablet hardness was measured using a tablet breaking strength measuring device (Toyama Sangyo: TH303MP). Ten tablets were measured and the average value was determined.
　カケワレ不良率の測定方法：連続打錠していき、錠剤のカケ・ワレをチェックし、不良が発生し始めたショット数を数えた。ショット数が多いほど、不良率は少ないと判断する。 Measure method of defective cracking rate: Continuous tableting was performed, the chip was checked for cracks and cracks, and the number of shots where defects started to occur was counted. It is determined that the larger the number of shots, the smaller the defect rate.
（実施例１）
　海水をろ過し、カラム充填されたキレスト社製のキレート繊維（商品名：キレストファイバーＧＲＹ－ＨＷ）に対し、海水を１５ｍＬ／ｍＬ－ｆｉｂｅｒ／ｈの一定速度で９６００ｍＬ通水し、海水中のＢを除去処理した。 (Example 1)
9600 mL of seawater was passed at a constant rate of 15 mL / mL-fiber / h to the chelate fiber (trade name: Cylest Fiber GRY-HW) manufactured by Crest, which was filtered and filled with column. Was removed.
　２０Ｌ容量のポリエチレン製容器に、Ｂを除去処理した海水４７２０ｍＬ（Ｍｇ２＋として０．２４ｍｏｌ相当）を秤量して攪拌し、これに硫酸を加えてｐＨを３に調製し、脱炭酸した。その後１００Ｌ容量のポリエチレン製容器に移した。これにアルカリ原料として１１．９ｇ／ｄＬ相当のＣａＯ濃度に調整した石灰乳を１００ｍＬ攪拌下にゆっくりと添加し（Ｍｇ２＋モル数：ＯＨ－モル数は１．０：１．８であった）、Ｍｇ（ＯＨ）２サスペンジョンを調製した。このＭｇ（ＯＨ）２サスペンジョンを種とし、その上から前述と同様にＢを除去処理および脱炭酸処理した海水４７２０ｍＬを加え、さらに１１．９ｇ／ｄＬ相当のＣａＯ濃度に調整した石灰乳１００ｍＬを攪拌下にゆっくりと添加後、５分間攪拌して、第１回目の種晶反応を行った。このような種晶反応を合計１０回繰り返した。 In a 20 L polyethylene container, 4720 mL of seawater from which B had been removed (equivalent to 0.24 mol as Mg 2+ ) was weighed and stirred, and sulfuric acid was added thereto to adjust the pH to 3, followed by decarboxylation. Thereafter, it was transferred to a 100 L capacity polyethylene container. This milk of lime adjusted to CaO concentration equivalent 11.9 g / dL as alkaline material was added slowly under 100mL stirring (Mg 2+ moles: OH - moles was 1.0: 1.8) , Mg (OH) 2 suspension was prepared. Using this Mg (OH) 2 suspension as a seed, 4720 mL of seawater from which B was removed and decarboxylated in the same manner as above was added, and 100 mL of lime milk adjusted to a CaO concentration equivalent to 11.9 g / dL was further stirred. After the slow addition, the mixture was stirred for 5 minutes to carry out the first seed crystal reaction. Such seed crystal reaction was repeated a total of 10 times.
　その後、脱水、固形分に対して１０倍量の純水で洗浄、乾燥して原料を得た。３００ｍＬ容量のアルミナ製るつぼに原料を１００ｇ充填し、電気炉を用いて、８２０℃で２時間焼成してＭｇＯ試料を得た。 Thereafter, dehydration, washing with 10 times the amount of pure water relative to the solid content, and drying were performed to obtain a raw material. A 300 mL alumina crucible was filled with 100 g of raw material and fired at 820 ° C. for 2 hours using an electric furnace to obtain a MgO sample.
　ＭｇＯ試料をフロイント・ターボ製の横型ローラーコンパクターを用いてロール圧力１ＭＰａをかけた。その後、グラニュレーター（日本グラニュレーター：ＧＲＮ１０３１）を用いて粉砕を行った。 A roll pressure of 1 MPa was applied to the MgO sample using a horizontal roller compactor made by Freund Turbo. Then, it grind | pulverized using the granulator (Nippon granulator: GRN1031).
　粉砕後、振動篩（２０ｍｅｓｈおよび６０ｍｅｓｈ）で篩別を行い、２０ｍｅｓｈオーバーと６０ｍｅｓｈアンダーの顆粒を取り除いて、酸化マグネシウム顆粒（平均粒径約４００μｍ）を作製した。 After pulverization, sieving was performed with a vibrating sieve (20 mesh and 60 mesh), and granules of 20 mesh over and 60 mesh under were removed to prepare magnesium oxide granules (average particle size of about 400 μm).
　得られた酸化マグネシウム顆粒を用いて、各種特性・物性を測定又は評価した。 Various characteristics and physical properties were measured or evaluated using the obtained magnesium oxide granules.
（実施例２）
　キレート繊維に対し、海水を１５ｍＬ／ｍＬ－ｆｉｂｅｒ／ｈの一定速度で１０５００ｍＬ通水して海水中のＢを除去処理した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 2)
Magnesium oxide granules were obtained by performing the same operation as in Example 1 except that 10500 mL of seawater was passed through the chelate fiber at a constant rate of 15 mL / mL-fiber / h to remove B in the seawater. Using this, various properties and physical properties were measured or evaluated.
（実施例３）
　キレート繊維に対し、海水を１５ｍＬ／ｍＬ－ｆｉｂｅｒ／ｈの一定速度で１１４００ｍＬ通水して海水中のＢを除去処理した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 3)
Magnesium oxide granules were obtained by performing the same operation as in Example 1 except that 11400 mL of seawater was passed through the chelate fiber at a constant rate of 15 mL / mL-fiber / h to remove B in the seawater. Using this, various properties and physical properties were measured or evaluated.
（実施例４）
　アルカリ原料として８．３ＮのＮａＯＨ水溶液を５１ｍＬ添加（Ｍｇ２＋モル数：ＯＨ－モル数は１．０：１．８であった）した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 Example 4
Magnesium oxide was prepared in the same manner as in Example 1 except that 51 mL of an 8.3N NaOH aqueous solution was added as an alkali raw material (Mg 2+ mol number: OH − mol number was 1.0: 1.8). Granules were obtained and used to measure or evaluate various properties and physical properties.
（実施例５）
　アルカリ原料として８．３ＮのＮａＯＨ水溶液を５４ｍＬ添加（Ｍｇ２＋モル数：ＯＨ－モル数は１．０：１．９であった）した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 5)
Magnesium oxide was prepared in the same manner as in Example 1 except that 54 mL of an 8.3N NaOH aqueous solution was added as an alkali raw material (Mg 2+ mol number: OH − mol number was 1.0: 1.9). Granules were obtained and used to measure or evaluate various properties and physical properties.
（実施例６）
　アルカリ原料として１１．９ｇ／ｄＬ相当のＣａＯ濃度に調整した石灰乳を１１１ｍＬ添加（Ｍｇ２＋モル数：ＯＨ－モル数は１．０：２．０であった）した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 6)
Milk of lime a 111mL addition adjusted to CaO concentration equivalent 11.9 g / dL as alkaline material (Mg 2+ moles: OH - moles 1.0: a which was 2.0) and other than the can, as in Example 1 The same operation was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using the same.
（実施例７）
　８５０℃で２時間焼成した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 7)
Except for baking at 850 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
（実施例８）
　７６０℃で２時間焼成した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 8)
Except for baking at 760 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
（実施例９）
　１０００℃で２時間焼成した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 Example 9
Except for baking at 1000 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
（実施例１０）
　７１０℃で２時間焼成した以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Example 10)
Except for baking at 710 ° C. for 2 hours, the same operation as in Example 1 was performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using this.
（実施例１１）
　２Ｌ容量のポリエチレン製容器に、マグネシウム原料としてＭｇＣｌ２・６Ｈ２Ｏを４８ｇ秤量し、純水１００ｍＬを加えて攪拌し、ＭｇＣｌ２水溶液を調製した。これにアルカリ原料として８．３ＮのＮａＯＨ水溶液５１ｍＬを攪拌下にゆっくりと添加し（Ｍｇ２＋モル数：ＯＨ－モル数は１．０：１．８であった）、Ｍｇ（ＯＨ）２サスペンジョンを調製した。 (Example 11)
In a 2 L-capacity polyethylene container, 48 g of MgCl 2 .6H 2 O as a magnesium raw material was weighed, and 100 mL of pure water was added and stirred to prepare an MgCl 2 aqueous solution. This aqueous NaOH 51mL of 8.3N was added slowly with stirring as an alkali material (Mg 2+ moles: OH - moles was 1.0: 1.8), Mg a (OH) 2 suspension Prepared.
　このＭｇ（ＯＨ）２サスペンジョンを種とし、その上からＭｇＣｌ２・６Ｈ２Ｏを４８ｇ純水１００ｍＬで溶解したＭｇＣｌ２水溶液を加え、さらに８．３ＮのＮａＯＨ水溶液５１ｍＬを攪拌下にゆっくりと添加後、５分間攪拌して、第１回目の種晶反応を行った。このような種晶反応を合計１０回繰り返した。 Using this Mg (OH) 2 suspension as a seed, add MgCl 2 aqueous solution in which 48 g of MgCl 2 · 6H 2 O was dissolved in 100 mL of pure water, and then slowly add 51 mL of 8.3 N NaOH aqueous solution with stirring. The first seed crystal reaction was performed by stirring for 5 minutes. Such seed crystal reaction was repeated a total of 10 times.
　上記の操作を行った以外は、実施例１と同様な操作を行って酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 Except for the above operations, the same operations as in Example 1 were performed to obtain magnesium oxide granules, and various properties and physical properties were measured or evaluated using the same.
（比較例１）
　以下のようにして、特許文献４（ＷＯ２０１５／１２８９４０号パンフレット）の実施例３に記載の酸化マグネシウム顆粒を得、これを用いて、各種特性・物性を測定又は評価した。 (Comparative Example 1)
In the following manner, magnesium oxide granules described in Example 3 of Patent Document 4 (WO2015 / 128940 pamphlet) were obtained, and various properties and physical properties were measured or evaluated using the magnesium oxide granules.
　すなわち、水酸化マグネシウム（神島化学工業社製、グレード名：＃２００）を電気炉で、９００℃で２時間焼成して中活性ＭｇＯを製造した。このようにして得られた中活性ＭｇＯは、ＢＥＴ比表面積５１ｍ２／ｇであった。一方で、同じ＃２００を電気炉で１１００℃で２時間焼成して低活性ＭｇＯを製造した。このようにして得られた低活性ＭｇＯは、ＢＥＴ比表面積３ｍ２／ｇであった。
　上記で得られたＢＥＴ比表面積５１ｍ２／ｇの中活性ＭｇＯと３ｍ２／ｇの低活性ＭｇＯの割合が、中活性ＭｇＯ：低活性ＭｇＯ＝４０：６０（重量％）となるように混合したものを用いてＭｇＯ顆粒を作成した。 That is, magnesium hydroxide (manufactured by Kamishima Chemical Industry Co., Ltd., grade name: # 200) was fired at 900 ° C. for 2 hours in an electric furnace to produce medium active MgO. The medium active MgO thus obtained had a BET specific surface area of 51 m 2 / g. On the other hand, the same # 200 was fired at 1100 ° C. for 2 hours in an electric furnace to produce low activity MgO. The low activity MgO thus obtained had a BET specific surface area of 3 m 2 / g.
The proportion of low activity MgO active MgO and 3m 2 / g in the resultant BET specific surface area 51m 2 / g in the above is, medium-active MgO: low activity MgO = 40: 60 were mixed so that (wt%) A MgO granule was prepared using the above.
　各種特性・物性を下記表に示す。 Various properties and physical properties are shown in the table below.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　上記表の結果から明らかなように、医薬品や食品用途にも十分適用しうる高純度でありながら、ホウ素の含有割合が所定の範囲（例えば、０．０５重量％以下）の酸化マグネシウム顆粒を用いることで、溶出率の高い錠剤、カルシウムの含有割合が所定の範囲（例えば、０．０３～１．８重量％）の酸化マグネシウム顆粒を用いることで、カケワレの少ない錠剤を、それぞれ効率良く得られることがわかった。 As is clear from the results in the above table, magnesium oxide granules having a high purity that can be sufficiently applied to pharmaceutical and food applications and having a boron content within a predetermined range (for example, 0.05% by weight or less) are used. By using magnesium oxide granules having a high dissolution rate and a calcium content ratio within a predetermined range (for example, 0.03 to 1.8% by weight), it is possible to efficiently obtain a tablet with less blurring. I understood it.
　また、さらにＢＥＴ比表面積の調整により、溶出性やカケワレを改善しつつ、高硬度の錠剤が得られることもわかった。 Furthermore, it was also found that by adjusting the BET specific surface area, tablets with high hardness can be obtained while improving the dissolution property and cracking.
　そして、特に、ホウ素含量、カルシウム含量及びＢＥＴ比表面積（さらには純度）を組み合わせて調整することで、優れた溶出性、カケワレの低減効果、高硬度のいずれも損なうことなく、これらを高いレベルで両立できることがわかった。 In particular, by adjusting the boron content, calcium content, and BET specific surface area (and purity) in combination, these can be achieved at a high level without losing any of the excellent elution properties, reduction effect of cracks, and high hardness. It turns out that both are compatible.
　本発明によれば、高純度でありながら、溶出性や製造不良（カケワレなど）を改善できる酸化マグネシウム顆粒を提供できる。このような酸化マグネシウム顆粒は、種々の用途に適用できるが、十分な高純度であるため、特に、動物に直接的又は間接的に摂取又は接触させる用途（例えば、食品用、医薬品用、化粧品用、肥料用など）などとして好適である。 According to the present invention, it is possible to provide magnesium oxide granules that can improve elution and manufacturing defects (eg, cracks) while having high purity. Such magnesium oxide granules can be applied to various uses, but are sufficiently high in purity, and in particular, used for ingesting or contacting animals directly or indirectly (for example, for foods, pharmaceuticals, and cosmetics). And the like for fertilizers).

Claims (14)

  1. 　Ｂの含有量が０．０５重量％以下、Ｃａの含有量が０．０３～１．８重量％、純分が９５～９９％である酸化マグネシウム顆粒。 Magnesium oxide granules having a B content of 0.05% by weight or less, a Ca content of 0.03 to 1.8% by weight, and a pure content of 95 to 99%.
  2. 　ＢＥＴ比表面積が５～６０ｍ２／ｇである請求項１記載の酸化マグネシウム顆粒。 The magnesium oxide granule according to claim 1, having a BET specific surface area of 5 to 60 m 2 / g.
  3. 　Ｂの含有量が０．０３重量％以下、Ｃａの含有量が０．０５～１．５重量％、純分が９６～９９％、ＢＥＴ比表面積が１０～５０ｍ２／ｇである、請求項１又は２記載の酸化マグネシウム顆粒。 The B content is 0.03% by weight or less, the Ca content is 0.05 to 1.5% by weight, the pure content is 96 to 99%, and the BET specific surface area is 10 to 50 m 2 / g. The magnesium oxide granule according to 1 or 2.
  4. 　酸化マグネシウムが海水に由来する請求項１～３のいずれかに記載の酸化マグネシウム顆粒。 The magnesium oxide granule according to any one of claims 1 to 3, wherein the magnesium oxide is derived from seawater.
  5. 　以下の（１）及び／又は（２）を充足する、動物に直接的又は間接的に摂取又は接触させる用途に使用するための酸化マグネシウム顆粒。
    　（１）Ｂの含有量が０．０５重量％以下
    　（２）Ｃａの含有量が０．０３～１．８重量％     Magnesium oxide granules for satisfying the following (1) and / or (2) for use in direct or indirect ingestion or contact with animals.
    (1) B content is 0.05% by weight or less (2) Ca content is 0.03 to 1.8% by weight
  6. 　純分が９５～９９％である請求項５記載の酸化マグネシウム顆粒。 The magnesium oxide granule according to claim 5, having a pure content of 95 to 99%.
  7. 　食品用、医薬品用及び化粧品用から選択された少なくとも１種の用途に使用する請求項５又は６記載の酸化マグネシウム顆粒。 The magnesium oxide granule according to claim 5 or 6, which is used for at least one application selected from foods, pharmaceuticals and cosmetics.
  8. 　海水からＢを除去する工程を少なくとも含む請求項１～７のいずれかに記載の酸化マグネシウム顆粒の製造方法。 The method for producing magnesium oxide granules according to any one of claims 1 to 7, comprising at least a step of removing B from seawater.
  9. 　キレート樹脂により海水からＢを除去する請求項８記載の製造方法。 The manufacturing method of Claim 8 which removes B from seawater with chelate resin.
  10. 　請求項１～７のいずれかに記載の酸化マグネシウム顆粒を含む錠剤。 A tablet comprising the magnesium oxide granules according to any one of claims 1 to 7.
  11. 　酸化マグネシウム顆粒におけるＢの含有量を０．０５重量％以下に調整し、酸化マグネシウム顆粒を含む錠剤の溶出性を向上又は改善する方法。 A method for improving or improving the dissolution properties of tablets containing magnesium oxide granules by adjusting the B content in the magnesium oxide granules to 0.05% by weight or less.
  12. 　酸化マグネシウム顆粒におけるＣａの含有量を０．０３～１．８重量％に調整し、酸化マグネシウム顆粒を含む錠剤の製造不良を低減する方法。 A method for reducing defective production of tablets containing magnesium oxide granules by adjusting the Ca content in the magnesium oxide granules to 0.03 to 1.8% by weight.
  13. 　酸化マグネシウム顆粒におけるＢの含有量を０．０３重量％以下、Ｃａの含有量を０．０５～１．５重量％、純分を９５～９９％に調整し、酸化マグネシウム顆粒を含む錠剤の溶出性を向上又は改善するとともに、製造不良を低減する方法。 Elution of tablets containing magnesium oxide granules by adjusting the B content in the magnesium oxide granules to 0.03% by weight or less, the Ca content to 0.05 to 1.5% by weight, and the pure content to 95 to 99% A method of improving manufacturing performance and reducing manufacturing defects.
  14. 　製造不良が、錠剤の欠け及び／又は割れである請求項１２又は１３に記載の方法。 The method according to claim 12 or 13, wherein the production failure is chipping and / or cracking of the tablet.
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JP2009209048A (en) * 2008-02-29 2009-09-17 Tomita Pharmaceutical Co Ltd Medicinal magnesium oxide
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