JP2006347961A - Method for producing powdered vitamin e pharmaceutical preparation - Google Patents
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本発明は、粉末状ビタミンＥ製剤の製造方法に関する。 The present invention relates to a method for producing a powdered vitamin E preparation.
従来、脂溶性のビタミン類を粉末化する方法として、脂溶性のビタミン類をアラビアガムあるいはゼラチンを含む水溶液に加えて乳化し、得られた乳化液を噴霧乾燥する方法が主として用いられている。しかし、アラビアガムには原料事情に問題があり、またゼラチンにはアレルゲン表示の問題があることから、近年これらに替わるものとして加工澱粉を用いた方法が提案されている。それらは、例えば、油溶性物質および化工澱粉を水に加えて乳化し、乳化液を乾燥することを特徴とする乳化粉末の製造方法（特許文献１参照）、脂溶性物質、加工澱粉および糖類に水を加えて乳化し、該乳化液を乾燥した乳化粉末の製造方法（特許文献２参照）などである。 Conventionally, as a method for powdering fat-soluble vitamins, a method in which fat-soluble vitamins are added to an aqueous solution containing gum arabic or gelatin and emulsified, and the resulting emulsion is spray-dried is mainly used. However, gum arabic has a problem in raw material circumstances, and gelatin has a problem of allergen labeling. In recent years, a method using modified starch has been proposed as an alternative to these. They include, for example, an oil-soluble substance and a modified starch added to water to emulsify the emulsion, and the emulsion is dried (see Patent Document 1), a fat-soluble substance, a modified starch and a saccharide. For example, a method for producing an emulsified powder obtained by adding water to emulsify and drying the emulsion (see Patent Document 2).
しかし、上記の方法で得られる粉末製剤の流動性は必ずしも良いとは言えず、流動性改善のために例えば含水二酸化ケイ素などの流動性付与物質を配合することが必要であった。 However, the fluidity of the powder preparation obtained by the above method is not necessarily good, and it has been necessary to add a fluidity-imparting substance such as hydrous silicon dioxide for improving the fluidity.
本発明は、賦形剤として加工澱粉を使用し、且つ得られた粉末が自由流動性を有する粉末状ビタミンＥ製剤の製造方法を提供することを目的とする。 An object of this invention is to provide the manufacturing method of the powdery vitamin E formulation which uses processed starch as an excipient | filler and the obtained powder has free-flow property.
本発明者は、上記課題に対して鋭意、検討を行った結果、粘度の異なる二種類のアルケニルコハク酸エステル化澱粉を賦形剤として抽出ビタミンＥを粉末化することにより、流動性に優れた粉末状ビタミンＥ製剤が得られることを見出し、この知見に基づいて本発明をなすに至った。
すなわち、本発明は、
（１）抽出ビタミンＥを含有する油相と、１５質量％に調整した水溶液の粘度が５ミリパスカル秒以上１００ミリパスカル秒未満のアルケニルコハク酸エステル化澱粉（Ａ）と
１５質量％に調整した水溶液の粘度が１００〜２５０ミリパスカル秒のアルケニルコハク酸エステル化澱粉（Ｂ）とを含有する水相とを乳化し、得られた水中油型乳化組成物を乾燥処理することを特徴とする粉末状ビタミンＥ製剤の製造方法、
（２）乾燥処理が噴霧乾燥であることを特徴とする前記（１）に記載の粉末状ビタミンＥ製剤の製造方法、
（３）アルケニルコハク酸エステル化澱粉がオクテニルコハク酸エステル化澱粉であることを特徴とする前記（１）または（２）に記載の粉末状ビタミンＥ製剤の製造方法、からなっている。
As a result of diligently examining the above problems, the present inventor was excellent in fluidity by powdering extracted vitamin E using two types of alkenyl succinate esterified starches having different viscosities as excipients. It discovered that a powdery vitamin E formulation was obtained and came to make this invention based on this knowledge.
That is, the present invention
(1) The viscosity of an oil phase containing extracted vitamin E and an aqueous solution adjusted to 15% by mass is adjusted to 15% by mass with alkenyl succinate esterified starch (A) having a viscosity of 5 millipascal seconds or more and less than 100 millipascal seconds. A powder characterized by emulsifying an aqueous phase containing an alkenyl succinic esterified starch (B) having an aqueous solution viscosity of 100 to 250 millipascal seconds, and subjecting the resulting oil-in-water emulsion composition to a drying treatment. Method for producing vitamin E preparation,
(2) The method for producing a powdered vitamin E preparation according to (1), wherein the drying treatment is spray drying,
(3) The method for producing a powdered vitamin E preparation according to (1) or (2) above, wherein the alkenyl succinate esterified starch is octenyl succinate esterified starch.
本発明で得られる粉末状ビタミンＥ製剤は優れた自由流動性を有する。
本発明で得られる粉末状ビタミンＥ製剤を使用することにより、計量の際の作業性が改善される。
The powdered vitamin E preparation obtained in the present invention has an excellent free flowing property.
By using the powdery vitamin E preparation obtained in the present invention, the workability during measurement is improved.
本発明で用いられる抽出ビタミンＥとしては、植物油が精製される過程で副生する脱臭留出物（脱臭スカム、脱臭スラッジまたはホットウエル油など）から回収されるビタミンＥであれば特に制限はなく、例えば、大豆油、ヒマワリ油、菜種油、綿実油、サフラワー油、トウモロコシ油、米糠油、ゴマ油、落花生油、パーム油などの脱臭留出物から分離・精製して得られる、α−、β−、γ−、δ−トコフェロールあるいはトコトリエノールを含む混合物が挙げられる。更に、該混合物をカラムクロマトグラフィー、蒸留または超臨界抽出などの操作により精製し、α−トコフェロール濃度あるいはトコトリエノール濃度を高めたものであっても良い。 The extracted vitamin E used in the present invention is not particularly limited as long as it is recovered from a deodorized distillate (such as deodorized scum, deodorized sludge or hot well oil) that is by-produced in the process of refining the vegetable oil. Α-, β-, obtained by separation and purification from deodorized distillates such as soybean oil, sunflower oil, rapeseed oil, cottonseed oil, safflower oil, corn oil, rice bran oil, sesame oil, peanut oil, palm oil, etc. , Γ-, δ-tocopherol or a mixture containing tocotrienol. Further, the mixture may be purified by an operation such as column chromatography, distillation or supercritical extraction to increase the α-tocopherol concentration or tocotrienol concentration.
本発明で用いられるアルケニルコハク酸エステル化澱粉は、例えば、馬鈴薯澱粉、コーンスターチ、ワキシーコーンスターチ、甘藷澱粉、小麦澱粉、米澱粉、タピオカ澱粉などの天然澱粉、またはこれらの化工澱粉（酸分解澱粉、酸化澱粉、酵素分解澱粉、エーテル化、エステル化、架橋化などの澱粉誘導体、湿熱処理澱粉、アルファー化澱粉など）を、アルカリ触媒の存在下に無水アルケニルコハク酸と反応させて得ることができる。無水アルケニルコハク酸のアルケニルの炭素数は約２〜２２、好ましくは約６〜１４がよく、具体的には、例えばヘキセニル無水コハク酸、オクテニル無水コハク酸、デセニル無水コハク酸、ドデセニル無水コハク酸、テトラデセニル無水コハク酸、ヘキサデセニル無水コハク酸、オクタデセニル無水コハク酸などが挙げられる。 The alkenyl succinic esterified starch used in the present invention is, for example, potato starch, corn starch, waxy corn starch, sweet potato starch, wheat starch, rice starch, tapioca starch, or other modified starch (acid-decomposed starch, oxidized starch). Starch, enzyme-degraded starch, starch derivatives such as etherification, esterification and crosslinking, wet heat-treated starch, pregelatinized starch, etc.) can be obtained by reacting with alkenyl succinic anhydride in the presence of an alkali catalyst. The number of carbon atoms of the alkenyl of the alkenyl succinic anhydride is preferably about 2 to 22, preferably about 6 to 14. Specifically, for example, hexenyl succinic anhydride, octenyl succinic anhydride, decenyl succinic anhydride, dodecenyl succinic anhydride, Examples include tetradecenyl succinic anhydride, hexadecenyl succinic anhydride, and octadecenyl succinic anhydride.
アルケニルコハク酸エステル化澱粉としては、澱粉とコハク酸のアルケニル誘導体とのエステルであれば特に制限はなく、例えばオクテニルコハク酸エステル化澱粉、デセニルコハク酸エステル化澱粉、ドデセニルコハク酸エステル化澱粉、テトラデセニルコハク酸エステル化澱粉、ヘキサデセニルコハク酸エステル化澱粉、およびオクタデセニルコハク酸エステル化澱粉、並びにこれら澱粉をα化または加水分解などの処理をしたものが挙げられる。これらの中でも、とりわけα化オクテニルコハク酸エステル化澱粉またはその塩が好ましい。 The alkenyl succinate esterified starch is not particularly limited as long as it is an ester of starch and an alkenyl derivative of succinic acid. For example, octenyl succinate esterified starch, decenyl succinate esterified starch, dodecenyl succinate esterified starch, tetradecenyl Examples thereof include succinic acid esterified starch, hexadecenyl succinic acid esterified starch, and octadecenyl succinic acid esterified starch, and those obtained by subjecting these starches to α-formation or hydrolysis. Among these, pregelatinized octenyl succinate esterified starch or a salt thereof is particularly preferable.
アルケニルコハク酸エステル化澱粉は、加水分解の度合いにより、また加水分解をする時期、即ちエステル化反応の前か後かにより、水溶液としたときの粘度が異なる。本発明においては、例えば１５質量％に調整した水溶液の粘度が約５ミリパスカル秒以上約１００ミリパスカル秒未満となるアルケニルコハク酸エステル化澱粉（Ａ）と１５質量％に調整した水溶液の粘度が約１００〜２５０ミリパスカル秒の範囲内となるアルケニルコハク酸エステル化澱粉（Ｂ）を選択して用いる。アルケニルコハク酸エステル化澱粉（Ａ）としては、１５質量％に調整した水溶液の粘度が約５ミリパスカル秒以上約１００ミリパスカル秒未満のオクテニルコハク酸エステル化澱粉が好ましい。具体的には、市販品の例えばカプシュールＳＴ（日本エヌエスシー社製）、ハイキャップ１００（日本エヌエスシー社製）、ピュリティガムＢＥ（日本エヌエスシー社製）、エマルスター３０Ａ（松谷化学工業社製）などを挙げることができる。また、アルケニルコハク酸エステル化澱粉（Ｂ）としては、１５質量％に調整した水溶液の粘度が約１００〜２５０ミリパスカル秒のオクテニルコハク酸エステル化澱粉が好ましい。具体的には、市販品の例えばエヌクリーマー４６（日本エヌエスシー社製）、エマルスターＥＭＳ−１０（松谷化学工業社製）などを挙げることができる。 Alkenyl succinic esterified starch has different viscosities when it is made into an aqueous solution depending on the degree of hydrolysis and the time of hydrolysis, that is, before or after the esterification reaction. In the present invention, for example, the viscosity of the aqueous solution adjusted to 15% by mass is alkenyl succinate esterified starch (A) having a viscosity of about 5 millipascal seconds or more and less than about 100 millipascal seconds, and the viscosity of the aqueous solution adjusted to 15% by mass is An alkenyl succinic esterified starch (B) that falls within the range of about 100 to 250 millipascal seconds is selected and used. As the alkenyl succinate esterified starch (A), an octenyl succinate esterified starch having a viscosity of an aqueous solution adjusted to 15% by mass of about 5 millipascal seconds or more and less than about 100 millipascal seconds is preferable. Specifically, commercially available products such as Capsule ST (manufactured by NSC Japan), High Cap 100 (manufactured by NSC Japan), Purity Gum BE (manufactured by NSC Japan), Emarustar 30A (manufactured by Matsutani Chemical Industry Co., Ltd.) ) And the like. Moreover, as an alkenyl succinate esterified starch (B), the octenyl succinate esterified starch whose viscosity of the aqueous solution adjusted to 15 mass% is about 100-250 millipascal second is preferable. Specific examples include commercially available products such as N Creamer 46 (manufactured by NSC Japan) and Emulstar EMS-10 (manufactured by Matsutani Chemical Industry Co., Ltd.).
本発明では、二種類のアルケニルコハク酸エステル化澱粉と水が混合され、水相として使用される。即ち、１５質量％に調整した水溶液の粘度が約５ミリパスカル秒以上約１００ミリパスカル秒未満のアルケニルコハク酸エステル化澱粉（Ａ）と１５質量％に調整した水溶液の粘度が約１００〜２５０ミリパスカル秒のアルケニルコハク酸エステル化澱粉（Ｂ）とを水に溶解した溶液が水相として好ましく使用される。上記（Ａ）と（Ｂ）の二種類のアルケニルコハク酸エステル化澱粉は別々に水に加えられ分散・溶解されても良く、また前記二種類のアルケニルコハク酸エステル化澱粉を予め紛体混合し、該混合物を水に加え分散・溶解しても良い。 In the present invention, two types of alkenyl succinate esterified starch and water are mixed and used as an aqueous phase. That is, the viscosity of the aqueous solution adjusted to 15% by mass and the viscosity of the aqueous solution adjusted to 15% by mass is about 100 to 250 mm. A solution obtained by dissolving Pascal second alkenyl succinic esterified starch (B) in water is preferably used as the aqueous phase. The two types of alkenyl succinic esterified starch of (A) and (B) above may be separately added to water and dispersed / dissolved, and the two types of alkenyl succinic esterified starch are previously mixed with powder, The mixture may be added to water and dispersed and dissolved.
アルケニルコハク酸エステル化澱粉（Ａ）とアルケニルコハク酸エステル化澱粉（Ｂ）の配合比率（重量比）には特に制限はなく、約１：９９〜約９９：１の任意の比率で使用してよい。好ましくは、アルケニルコハク酸エステル化澱粉（Ａ）（例えば、カプシュールＳＴ、ハイキャップ１００、ピュリティガムＢＥなど）とアルケニルコハク酸エステル化澱粉（Ｂ）（例えばエヌクリーマー４６など）とを混合して得られる混合物の１５質量％水溶液の粘度が約５０〜２００ミリパスカル秒の範囲になるように、アルケニルコハク酸エステル化澱粉（Ａ）とアルケニルコハク酸エステル化澱粉（Ｂ）との配合比率を定める。 There is no restriction | limiting in particular in the mixture ratio (weight ratio) of an alkenyl succinate esterified starch (A) and an alkenyl succinate esterified starch (B), It uses it by arbitrary ratios of about 1:99 to about 99: 1. Good. Preferably, alkenyl succinate esterified starch (A) (for example, Capsule ST, High Cap 100, Purity Gum BE, etc.) and alkenyl succinate esterified starch (B) (for example, N Creamer 46, etc.) are mixed. The blending ratio of the alkenyl succinate esterified starch (A) and the alkenyl succinate esterified starch (B) is determined so that the viscosity of the 15% by mass aqueous solution of the resulting mixture is in the range of about 50 to 200 millipascal seconds. .
上記混合物の具体例としては、例えばカプシュールＳＴとエヌクリーマー４６の配合比率（重量比）を約１：１で混合して得られた混合物（混合物の１５質量％水溶液の粘度：約６０ミリパスカル秒）、ハイキャップ１００とエヌクリーマー４６の配合比率（重量比）を約１：１で混合して得られた混合物（混合物の１５質量％水溶液の粘度：約８２ミリパスカル秒）、ピュリティガムＢＥとエヌクリーマー４６の配合比率（重量比）を約１：１で混合して得られた混合物（混合物の１５質量％水溶液の粘度：約９０ミリパスカル秒）などを挙げることができる。 As a specific example of the above-mentioned mixture, for example, a mixture obtained by mixing the mixture ratio (weight ratio) of Capsule ST and N Creamer 46 at about 1: 1 (viscosity of 15% by weight aqueous solution of the mixture: about 60 millipascals). Second), a mixture obtained by mixing the mixing ratio (weight ratio) of the high cap 100 and Ncreamer 46 at about 1: 1 (viscosity of 15% by weight aqueous solution of the mixture: about 82 millipascal seconds), Purity Gum BE And a mixture ratio (weight ratio) of N Creamer 46 at about 1: 1 (viscosity of a 15% by weight aqueous solution of the mixture: about 90 millipascal second).
本発明で用いられる水としては、飲用可能なものであれば特に制限はなく、例えば蒸留水、イオン交換樹脂処理水、逆浸透膜処理水および限外ろ過膜処理水などの精製水、水道水、地下水または涌水などの天然水並びにアルカリイオン水などが挙げられる。 The water used in the present invention is not particularly limited as long as it is drinkable. For example, purified water such as distilled water, ion-exchange resin treated water, reverse osmosis membrane treated water and ultrafiltration membrane treated water, tap water Natural water such as ground water or brine, and alkali ion water.
本発明で言うところの粘度は、第７版食品添加物公定書記載「２８.粘度測定法」の「第２法回転粘度計法」に基づいて測定される。具体的な測定条件および操作条件を以下に示す。なお回転数は想定される粘度に応じて選択される。
［測定方法］
試料を入れた容器中にローターとガードを静かに入れ、試料の液面をローターの液浸マークに一致させる。スイッチを入れてから６０秒経過後の指針の示す目盛を読み取り、この指示値に、使用したローターの種類および回転数によって定まる換算乗数を乗じて、試料の粘度を算出する。
［操作条件］
測定装置 ブルックフィールド型粘度計
ローター １号
回転数 ６０、３０、１２または６回転／分のいずれか
測定 回転開始６０秒後
測定温度 ２５℃
The viscosity referred to in the present invention is measured based on the “second method rotational viscometer method” described in “28. Specific measurement conditions and operation conditions are shown below. The rotational speed is selected according to the assumed viscosity.
[Measuring method]
Gently place the rotor and guard into the container containing the sample, and align the liquid level of the sample with the immersion mark on the rotor. The scale indicated by the pointer 60 seconds after the switch is turned on is read, and the viscosity of the sample is calculated by multiplying this indicated value by a conversion multiplier determined by the type of rotor used and the number of rotations.
[Operation conditions]
Measuring device Brookfield viscometer Rotor No. 1 Rotation speed 60, 30, 12 or 6 rotations / minute Measurement 60 seconds after starting rotation Measurement temperature 25 ° C
本発明に係る水中油型乳化組成物１００質量％中には、前記抽出ビタミンＥ約５〜３０質量％、好ましくは約１０〜２５質量％、アルケニルコハク酸エステル化澱粉約１０〜３５質量％、好ましくは約１４〜３０質量％、残余が水となるように調整するのが好ましい。
また、水中油型乳化組成物の製造に用いられる水の量に特に制限はないが、得られる乳化組成物の固形分濃度が２０〜６０質量％となるよう調整するのが好ましい。
In 100% by mass of the oil-in-water emulsion composition according to the present invention, the extracted vitamin E is about 5 to 30% by mass, preferably about 10 to 25% by mass, alkenyl succinic acid esterified starch about 10 to 35% by mass, Preferably, it is adjusted to about 14 to 30% by mass, and the remainder is water.
Moreover, there is no restriction | limiting in particular in the quantity of the water used for manufacture of an oil-in-water emulsion composition, However, It is preferable to adjust so that solid content concentration of the obtained emulsion composition may be 20-60 mass%.
本発明に係る水中油型乳化組成物の製造方法は特に限定されず、公知の方法を用いて行うことができる。以下に好ましい水中油型乳化組成物の製造方法を例示する。
例えば、水にアルケニルコハク酸エステル化澱粉（Ａ）とアルケニルコハク酸エステル化澱粉（Ｂ）を加えて約４０〜８０℃、好ましくは約６０〜８０℃に加熱して溶解して水相とする。該水相を攪拌しながら、この中に約１００℃以下、好ましくは約６０〜１００℃に保温された抽出ビタミンＥをゆっくり加え、高速回転式分散・乳化機を用いて、回転数約４０００〜２００００ｒｐｍにて、攪拌時間約１０〜６０分間で乳化する方法により本発明に係る水中油型乳化組成物を製造することができる。
The manufacturing method of the oil-in-water type emulsion composition which concerns on this invention is not specifically limited, It can carry out using a well-known method. Examples of the preferred method for producing an oil-in-water emulsion composition are as follows.
For example, alkenyl succinic esterified starch (A) and alkenyl succinic esterified starch (B) are added to water and heated to about 40 to 80 ° C., preferably about 60 to 80 ° C., and dissolved to form an aqueous phase. . While stirring the aqueous phase, slowly add extracted vitamin E kept at about 100 ° C. or less, preferably about 60-100 ° C., and use a high-speed rotary dispersion / emulsifier to rotate the rotation speed to about 4000 The oil-in-water emulsified composition according to the present invention can be produced by a method of emulsifying at 20000 rpm with a stirring time of about 10 to 60 minutes.
上記水中油型乳化組成物を製造するための装置としては特に限定されず、例えば、攪拌機、加熱用のジャケットおよび邪魔板などを備えた通常の攪拌・混合槽を用いることができる。装備する攪拌機としては、ＴＫホモミクサー（特殊機化工業社製）またはクレアミックス（エムテクニック社製）などの高速回転式分散・乳化機が好ましく用いられる。
また、これらの装置で乳化した液を、高圧式均質化処理機を使用して、さらに均質化してもよい。ここで高圧式均質化処理機としては、例えばＡＰＶゴーリンホモジナイザー（ＡＰＶ社製）、マイクロフルイダイザー（マイクロフルイデックス社製）、アルティマイザー（スギノマシン社製）またはナノマイザー（大和製罐社製）などを好ましく使用することができる。上記均質化処理機に代えて、例えば超音波乳化機などの均質化処理機を用いてもよい。
The apparatus for producing the oil-in-water emulsion composition is not particularly limited, and for example, a normal stirring / mixing tank equipped with a stirrer, a heating jacket, a baffle plate, and the like can be used. As a stirrer to be equipped, a high-speed rotary dispersing / emulsifying machine such as TK homomixer (made by Tokushu Kika Kogyo Co., Ltd.) or Claremix (made by M Technique Co., Ltd.) is preferably used.
Moreover, you may further homogenize the liquid emulsified with these apparatuses using a high-pressure-type homogenizer. Here, examples of the high-pressure homogenizer include an APV gorin homogenizer (manufactured by APV), a microfluidizer (manufactured by Microfluidics), an optimizer (manufactured by Sugino Machine), or a nanomizer (manufactured by Daiwa Steel). Can be preferably used. Instead of the homogenizer, a homogenizer such as an ultrasonic emulsifier may be used.
得られる水中油型乳化組成物中の油分の平均粒子径は約１０μm以下、好ましくは約０．０５〜５μm、更に好ましくは約０．１〜１μmである。該平均粒子径が０．０５μm未満であると、粉末の水への分散、溶解性が低下するため好ましくない。また１０μm以上であると、乳化組成物自体の保存安定性が不安定となる恐れがある。 The average particle size of oil in the obtained oil-in-water emulsion composition is about 10 μm or less, preferably about 0.05 to 5 μm, more preferably about 0.1 to 1 μm. When the average particle diameter is less than 0.05 μm, the dispersion and solubility of the powder in water are not preferred. If it is 10 μm or more, the storage stability of the emulsified composition itself may be unstable.
次に水中油型乳化組成物は乾燥され粉末化される。乾燥方法としては、例えば、噴霧乾燥、ドラム乾燥、ベルト乾燥、真空乾燥あるいは真空凍結乾燥などが挙げられるが、好ましくは噴霧乾燥である。本発明で使用される噴霧乾燥装置に特に制限はなく、噴射式噴霧乾燥装置または回転円盤式噴霧乾燥装置など公知の装置を使用することができる。また、噴霧乾燥の操作条件に特に制限は無く、例えば、乳化組成物を加圧ノズル式噴霧乾燥装置に供給し、熱風入口温度約１５０〜２７０℃、排気温度約７０〜１３０℃の条件下で噴霧乾燥し、乾燥物をサイクロンで捕集することにより、流動性の良い粉末状ビタミンＥ製剤を得ることができる。得られる粉末状ビタミンＥ製剤の平均粒子径は約２０〜２００μｍ、好ましくは約５０〜１００μｍである。また得られる粉末状ビタミンＥ製剤の乾燥減量は約１０質量％以下、好ましくは約７質量％以下、更に好ましくは約５質量％以下である。 Next, the oil-in-water emulsion composition is dried and powdered. Examples of the drying method include spray drying, drum drying, belt drying, vacuum drying, and vacuum freeze drying, and spray drying is preferable. There is no restriction | limiting in particular in the spray-drying apparatus used by this invention, Well-known apparatuses, such as a spray-type spray-drying apparatus or a rotary disk type spray-drying apparatus, can be used. There are no particular restrictions on the operating conditions for spray drying. For example, the emulsified composition is supplied to a pressure nozzle type spray drying apparatus, and the hot air inlet temperature is about 150 to 270 ° C. and the exhaust temperature is about 70 to 130 ° C. By spray-drying and collecting the dried product with a cyclone, a powdery vitamin E preparation with good fluidity can be obtained. The average particle size of the obtained powdered vitamin E preparation is about 20 to 200 μm, preferably about 50 to 100 μm. The loss on drying of the obtained powdered vitamin E preparation is about 10% by mass or less, preferably about 7% by mass or less, more preferably about 5% by mass or less.
本発明で得られる粉末状ビタミンＥ製剤の好ましい実施態様の一例は、該製剤１００質量％中、ビタミンＥを約１０〜７０質量％、好ましくは約２０〜６０質量％、アルケニルコハク酸エステル化澱粉（Ａ）とアルケニルコハク酸エステル化澱粉（Ｂ）の混合物を約３０〜９０質量％、好ましくは約４０〜８０質量％を含む粉末である。 An example of a preferred embodiment of the powdered vitamin E preparation obtained in the present invention is an alkenyl succinic acid esterified starch having about 10 to 70% by weight, preferably about 20 to 60% by weight of vitamin E in 100% by weight of the preparation. It is a powder containing about 30 to 90% by mass, preferably about 40 to 80% by mass of a mixture of (A) and alkenyl succinic esterified starch (B).
尚、本発明になる粉末状ビタミンＥ製剤中には、本発明の目的・効果を阻害しない範囲で、例えば賦形剤、流動性付与物質などを加えることができる。賦形剤としては、例えば、ブドウ糖、果糖などの単糖、ショ糖、乳糖、麦芽糖などの二糖、デキストリン、粉末水飴などのでん粉分解物、マルトトリオース、マルトテトラオース、マルトペンタオース、マルトヘキサオースなどのマルトオリゴ糖類、ソルビトール、マンニトール、マルチトール、粉末還元水飴、粉末還元パラチノースなどの糖アルコール類などが挙げられる。また流動性付与物質としては、例えば、リン酸三カルシウム、微粒二酸化ケイ素などが挙げられる。 In the powdered vitamin E preparation according to the present invention, for example, an excipient, a fluidity-imparting substance and the like can be added within a range not inhibiting the purpose and effect of the present invention. Examples of excipients include monosaccharides such as glucose and fructose, disaccharides such as sucrose, lactose and maltose, starch decomposition products such as dextrin and starch syrup, maltotriose, maltotetraose, maltopentaose, malto Examples include malto-oligosaccharides such as hexaose, sugar alcohols such as sorbitol, mannitol, maltitol, powdered reduced starch syrup, and powdered reduced palatinose. Examples of the fluidity imparting substance include tricalcium phosphate and fine silicon dioxide.
以下、実施例をもって本発明を具体的に説明する。もちろん、本発明が以下に記載された実施例に限定されるものではないことは言うまでもない。 Hereinafter, the present invention will be specifically described with reference to examples. Of course, it goes without saying that the present invention is not limited to the examples described below.
[参考例]
以下の実施例または比較例で使用するオクテニルコハク酸エステル化澱粉の粘度を表１に示す。
[Reference example]
Table 1 shows the viscosity of the octenyl succinic esterified starch used in the following Examples or Comparative Examples.
［実施例１］
１）５Ｌ容ステンレス製ビーカーに精製水１８５０ｍｌを入れ８０℃に加温する。
２）ＴＫホモミクサー（型式：ＭＡＲＫ２．５；特殊機化工業社製）で低速で攪拌しながら、カプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇを溶解し、水相とした。
３）抽出ビタミンＥ（製品名：理研Ｅオイル８０５；理研ビタミン社製，ビタミンＥ含量約８０質量％）６００ｇを約８０℃まで加熱し、油相とした。
４）ＴＫホモミクサーで低速で撹拌しながら、上記２）の水相に上記３）の油相を徐々に加え、その後１００００ｒｐｍで１５分間攪拌・乳化し、得られた乳化液を更にＡＰＶゴーリンホモジナイザー（型式：ＬＡＢ１０００；ＡＰＶ社製）にて３４．３ＭＰａで１回処理し、均質化液を得た。
５）上記４）の均質化液を、加圧ノズル式噴霧乾燥装置（型式：Ｌ−８ｉ；大川原化工機社）にて、熱風入口温度１７０℃、排気温度８０℃の条件下で噴霧乾燥し、乾燥物をサイクロンで捕集することにより粉末状ビタミンＥ製剤（実施品１）を約８８０ｇ得た。得られた粉末の乾燥減量は約４．３質量％であった。
[Example 1]
1) Put 1850 ml of purified water in a 5 L stainless steel beaker and heat to 80 ° C.
2) While stirring at low speed with a TK homomixer (model: MARK2.5; manufactured by Tokushu Kika Kogyo Co., Ltd.), 200 g of Capsule ST (manufactured by NSC Japan) and 200 g of Ncreamer 46 (manufactured by NSC Japan) were dissolved. And made into an aqueous phase.
3) 600 g of extracted vitamin E (product name: Riken E Oil 805; manufactured by Riken Vitamin Co., Ltd., vitamin E content of about 80% by mass) was heated to about 80 ° C. to obtain an oil phase.
4) While stirring at low speed with a TK homomixer, gradually add the oil phase of 3) above to the aqueous phase of 2) above, then stir and emulsify for 15 minutes at 10000 rpm, and the resulting emulsion is further added to an APV gorin homogenizer ( (Model: LAB1000; manufactured by APV) was processed once at 34.3 MPa to obtain a homogenized liquid.
5) The homogenized liquid of the above 4) is spray-dried under the conditions of a hot air inlet temperature of 170 ° C. and an exhaust temperature of 80 ° C. in a pressure nozzle type spray drying device (model: L-8i; Okawara Chemical Co., Ltd.). The dried product was collected with a cyclone to obtain about 880 g of a powdered vitamin E preparation (Example 1). The loss on drying of the obtained powder was about 4.3% by mass.
［実施例２］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、ハイキャップ１００（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇを使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（実施品２）を約８８０ｇ得た。得られた粉末の乾燥減量は約４．３質量％であった。
[Example 2]
In place of 200 g of Capsule ST (manufactured by NSC Japan) and 200 g of N Creamer 46 (manufactured by NSC Japan) described in 2) of Example 1, 200 g of high cap 100 (manufactured by NSC Japan) The same procedure as in Example 1 was carried out except that 200 g of N Creamer 46 (manufactured by NSC Japan) was used, and about 880 g of a powdered vitamin E preparation (practical product 2) was obtained. The loss on drying of the obtained powder was about 4.3% by mass.
［実施例３］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、ピュリティガムＢＥ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇを使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（実施品３）を約８８０ｇ得た。得られた粉末の乾燥減量は約４．４質量％であった。
[Example 3]
In place of 200 g of Capsule ST (manufactured by NSC Japan) and 200 g of N Creamer 46 (manufactured by NSC Japan) described in 2) of Example 1, 200 g of Purity Gum BE (manufactured by NSC Japan) The same procedure as in Example 1 was carried out except that 200 g of N Creamer 46 (manufactured by NSC Japan) was used, and about 880 g of a powdered vitamin E preparation (practical product 3) was obtained. The loss on drying of the obtained powder was about 4.4% by mass.
［比較例１］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、カプシュールＳＴ（日本エヌエスシー社製）を４００ｇ使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（比較品１）を約８５０ｇ得た。得られた粉末の乾燥減量は約４．５質量％であった。
[Comparative Example 1]
In place of 200 g of Capsule ST (made by NSC Japan) and 200 g of N Creamer 46 (made by NSC Japan) described in 2) of Example 1, 400 g of Capsule ST (made by NSC Japan) was used. Except for using it, it carried out similarly to Example 1, and obtained about 850g of powdery vitamin E preparations (comparative product 1). The loss on drying of the obtained powder was about 4.5% by mass.
［比較例２］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、ハイキャップ１００（日本エヌエスシー社製）を４００ｇ使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（比較品２）を約８５０ｇ得た。得られた粉末の乾燥減量は約４．５質量％であった。
[Comparative Example 2]
400 g of High Cap 100 (manufactured by NSC Japan) was replaced with 200 g of Capsule ST (manufactured by NSC Japan) and 200 g of N Creamer 46 (manufactured by NSC Japan) described in 2) of Example 1. Except for using it, it carried out similarly to Example 1, and obtained about 850g of powdery vitamin E preparations (comparative product 2). The loss on drying of the obtained powder was about 4.5% by mass.
［比較例３］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、ピュリティガムＢＥ（日本エヌエスシー社製）４００ｇを使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（比較品３）を約８５０ｇ得た。得られた粉末の乾燥減量は約４．５質量％であった。
[Comparative Example 3]
Instead of 200 g of Capsule ST (manufactured by NSC Japan) and 200 g of N Creamer 46 (manufactured by NSC Japan) described in 2) of Example 1, 400 g of Purity Gum BE (manufactured by NSC Japan) was used. Except for using it, it carried out similarly to Example 1, and obtained about 850g of powdery vitamin E preparations (comparative product 3). The loss on drying of the obtained powder was about 4.5% by mass.
［比較例４］
実施例１の２）に記載されているカプシュールＳＴ（日本エヌエスシー社製）２００ｇとエヌクリーマー４６（日本エヌエスシー社製）２００ｇに替えて、エヌクリーマー４６（日本エヌエスシー社製）を４００ｇ使用する以外は実施例１と同様に実施し、粉末状ビタミンＥ製剤（比較品４）を約８５０ｇ得た。得られた粉末の乾燥減量は約４．５質量％であった。
[Comparative Example 4]
400g of N Creamer 46 (manufactured by NSC Japan) was replaced with 200g of Capsule ST (manufactured by NSC Japan) and 200g of N Creamer 46 (manufactured by NSC Japan) described in 2) of Example 1. Except for using it, it carried out similarly to Example 1, and obtained about 850g of powdery vitamin E preparations (comparative product 4). The loss on drying of the obtained powder was about 4.5% by mass.
［試験例１］
実施例１〜３および比較例１〜４で得た粉末状ビタミンＥ製剤（実施品１〜３、比較品１〜４）の紛質を評価するため、粉末の安息角を測定した。結果を表２に示した。
[Test Example 1]
In order to evaluate the powder quality of the powdered vitamin E preparations (Examples 1 to 3, Comparative Products 1 to 4) obtained in Examples 1 to 3 and Comparative Examples 1 to 4, the angle of repose of the powder was measured. The results are shown in Table 2.
〈安息角の測定方法〉
安息角測定器（井元製作所社製）使用。試料粉末をロートの穴から静かに注入して水平板の上に堆積させ、形成される円錐の頂点がロートの下端に達したときの底面の半径と円錐の高さから安息角を測定した。尚、ロートの下端から水平板までの距離は４０ｍｍとした。
<Measurement method of repose angle>
Use angle of repose measuring instrument (Imoto Seisakusho). The sample powder was gently injected from the hole of the funnel and deposited on the horizontal plate, and the angle of repose was measured from the radius of the bottom surface and the height of the cone when the top of the cone formed reached the lower end of the funnel. The distance from the lower end of the funnel to the horizontal plate was 40 mm.
実施品１〜３は４０度以下の安息角を示し、極めて流動性が良かった。 Examples 1 to 3 exhibited an angle of repose of 40 degrees or less, and were extremely fluid.
［試験例２］
実施例１〜３および比較例１〜４で得た粉末状ビタミンＥ製剤（実施品１〜３、比較品１〜４）各５００ｇをチャック付ポリエチレン袋（２４０×１７０×０．０８ｍｍ）に充填し、４０℃で１ヶ月保存した。試験終了後、袋から内容物を取り出し、その状態を観察した。結果を表３に示した。
[Test Example 2]
500 g each of powdered vitamin E preparations (Examples 1 to 3, Comparative Examples 1 to 4) obtained in Examples 1 to 3 and Comparative Examples 1 to 4 are filled in a polyethylene bag with a chuck (240 × 170 × 0.08 mm). And stored at 40 ° C. for 1 month. After the test, the contents were removed from the bag and the state was observed. The results are shown in Table 3.
本発明で得られる粉末状ビタミンＥ製剤は、そのままあるいは他の粉末成分と混合して、医薬品、食品などの分野で、栄養強化を目的としてあるいは酸化防止剤として利用することができる。
The powdered vitamin E preparation obtained in the present invention can be used as it is or mixed with other powder components for the purpose of enhancing nutrition or as an antioxidant in the fields of pharmaceuticals and foods.
Claims (3)
The method for producing a powdered vitamin E preparation according to claim 1 or 2, wherein the alkenyl succinate esterified starch is octenyl succinate esterified starch.
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| JP2018166465A (en) * | 2017-03-30 | 2018-11-01 | 理研ビタミン株式会社 | Powdery antioxidant for powdery food |
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| JP2009247350A (en) * | 2008-04-10 | 2009-10-29 | Sato Shokuhin Kogyo Kk | Method for producing powder containing alcohol |
| JP2016174573A (en) * | 2015-03-20 | 2016-10-06 | アサヒビール株式会社 | Powdered liquor |
| JP2018166465A (en) * | 2017-03-30 | 2018-11-01 | 理研ビタミン株式会社 | Powdery antioxidant for powdery food |
| JP6990518B2 (en) | 2017-03-30 | 2022-02-03 | 理研ビタミン株式会社 | Powdered Food Powdered Antioxidant |
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