JP2009084157A - Method for producing oil and fat-coated powder - Google Patents

Method for producing oil and fat-coated powder Download PDF

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JP2009084157A
JP2009084157A JP2007251539A JP2007251539A JP2009084157A JP 2009084157 A JP2009084157 A JP 2009084157A JP 2007251539 A JP2007251539 A JP 2007251539A JP 2007251539 A JP2007251539 A JP 2007251539A JP 2009084157 A JP2009084157 A JP 2009084157A
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powder
zein
fat
oil
coating
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Koichi Tanimizu
浩一 谷水
Toshihiro Sato
俊宏 佐藤
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NOF Corp
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NOF Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing an oils and fats-coated powder covering taste components sufficiently, and excellent in masking effect, taste, tablet-forming property and also in preservation stability. <P>SOLUTION: This method for producing the oils and fats-covered powder containing the taste components comprises the following (A) to (C) processes. (A) A process of covering zein on the powder containing the taste components. (B) A process of obtaining the covered powder by colliding hydrogenated oils and fats powder having 1 to 50 μm mean particle diameter, 50 to 80°C melting point and ≤0.6 peak intensity ratio (19°/21° intensity ratio) of the peak intensity at 2θ (19°) to the peak intensity at 2θ (21°) in X-ray diffraction measurements by using CuKα beam as a light source to the zein-coated powder in a condition that the powder temperature becomes ≤45°C. (C) A process of tempering the covered powder prepared by the above process (B) at 35 to 60°C for 1 to 200 hr. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、呈味成分の油脂被覆粉末の製造方法に関する。詳しくは、呈味成分上にゼイン及び油脂を二重に被覆した油脂被覆粉末の製造方法であり、呈味のマスキング、舌触り、保存安定性及び打錠性に優れた油脂被覆粉末の製造方法を提供する。   The present invention relates to a method for producing a fat-and-oil coated powder as a taste component. Specifically, it is a method for producing an oil-coated powder in which zein and fat are coated on a taste component, and a method for producing an oil-coated powder excellent in taste masking, touch, storage stability and tableting properties. provide.

一般に、漢方生薬、医薬物または健康食品等は、その有効成分固有の苦味、えぐみ等があるため、服用しづらいとういう難点がある。そこで、味をマスキングする方法として、呈味成分の粉末に融点40℃以上の硬化油脂粉末を接触・衝突させてコーティングする方法(特許文献1)、粒径が50μm以下の呈味成分をゼラチン等の水溶性結合剤を用いて造粒後、これに硬化油脂微粉末を被覆する方法(特許文献2)、呈味成分を含む造粒物を賦形剤と油脂で攪拌造粒し、更にゼインでコーティングする方法(特許文献3)等がある。   In general, herbal medicines, pharmaceuticals, health foods, and the like have a difficulty that they are difficult to take because of their bitterness, puffiness and the like inherent in their active ingredients. Therefore, as a method for masking the taste, a method of coating the taste component powder by contacting and colliding with a hardened fat powder having a melting point of 40 ° C. or higher (Patent Document 1), a taste component having a particle size of 50 μm or less is gelatin or the like. After granulating using a water-soluble binder, a method of coating the hardened oil and fat fine powder (Patent Document 2), agglomerates containing a taste component are stirred and granulated with an excipient and an oil and fat, and zein (Patent Document 3) and the like.

しかしながら、特許文献1の製造方法によると、十分なマスキング効果が得られておらず、強い呈味を有することから服用を容易にするに至らなかった。これは、油脂粉体を衝突させる油脂被覆工程において、味をマスキングできるだけの十分な油脂による被覆ができていないことが考えられる。また、特許文献2の製造方法によると、油脂被覆の前に、呈味成分をゼラチン等の水溶性結合剤で造粒しているが、この場合でも十分な油脂被覆によるマスキング効果が得られるには至っていなかった。
また、特許文献1や2における製造方法では、製造される油脂被覆粉末において、打錠性が低下する、長期保存時に固着する等の問題があった。これは、最外層にある油脂が構造的に融着し易く、錠剤等の原料と使用する際の打錠性能や、粉末の長期保存安定性において不十分になるものと考えられる。
なお、最外層をゼイン等の蛋白質で被覆する製造方法(特許文献3)では、造粒物の粒度が大きくなり易い。また、ゼイン特有の舌触りの悪さが残り、服用に適さない。さらに、造粒工程を繰り返しており、生産効率も悪いとの問題点を有している。
However, according to the production method of Patent Document 1, a sufficient masking effect has not been obtained, and since it has a strong taste, it has not been easy to take. This is probably because the coating with fats and oils sufficient to mask the taste is not performed in the fat coating process in which the fat and oil powder collides. In addition, according to the production method of Patent Document 2, the taste component is granulated with a water-soluble binder such as gelatin before the oil coating. Even in this case, a sufficient masking effect by the oil coating is obtained. Was not reached.
Moreover, in the manufacturing method in patent document 1 and 2, there existed problems, such as tableting property falling in the fat-and-oil coating powder manufactured, and adhering at the time of long-term storage. This is considered to be because the oil and fat in the outermost layer is structurally easy to fuse, and the tableting performance when used with raw materials such as tablets and the long-term storage stability of the powder are insufficient.
In addition, in the manufacturing method (patent document 3) which coat | covers outermost layers with proteins, such as zein, the particle size of a granulated material tends to become large. In addition, Zein's peculiar feeling of tongue remains and it is not suitable for taking. Furthermore, the granulation process is repeated, and the production efficiency is poor.

特開昭63−164863号公報JP 63-164863 A 特開平11−308985号公報JP-A-11-308985 特開平6−24963号公報JP-A-6-24963

本発明は、呈味成分を十分に被覆でき、マスキング効果、舌触り、打錠性、保存安定性にも優れた油脂覆粉末の製造方法を提供することを目的とする。
そこで、まず、本発明では、呈味成分をゼインで被覆し、さらに、これを油脂で被覆すると、味のマスキング効果に優れ、舌触りの良い被覆粉末を製造できることを見出した。
次に、本発明は粉末を被覆している油脂の多形に注目した。
油脂の本質的な属性として、多形現象があり、トリアシルグリセロールには通常、数種類の結晶多形が存在しており、それらの分類と命名は、融点と副格子を基準にして以下のように整理されている。
α型・・・ヘキサゴナル(H)型副格子、不安定型
β’型・・O⊥型副格子、準安定型
β型・・・T//型副格子、安定型
ここで、油脂被覆時には不安定型であるα型油脂粉末を用い、打錠性、保存時には結晶多形をα型から安定型のβ型に転移させれば、打錠性や保存安定性を改質できる。
なお、α型からβ型の転移は、固相転移が知られており、融点50〜80℃での油脂であれば、融点の10〜30℃以下の温度に放置することにより、経時的に転移していく。
An object of this invention is to provide the manufacturing method of the oil-and-oil covering powder which can fully coat | cover a taste component and was excellent also in the masking effect, the touch, tableting property, and storage stability.
Therefore, first, in the present invention, it was found that when a taste ingredient is coated with zein and further coated with oils and fats, a coating powder with excellent taste masking effect and good touch can be produced.
Next, the present invention focused on the polymorphs of the fats and oils coating the powder.
An essential attribute of fats and oils is polymorphism, and triacylglycerol usually has several types of crystal polymorphs. Their classification and nomenclature are based on the melting point and sublattice as follows: Are organized.
α type ・ ・ ・ Hexagonal (H) type sublattice, unstable type β ′ type ・ ・ O⊥ type sublattice, metastable type β type ... T // type sublattice, stable type If a regular α-type oil and fat powder is used and the tablet polymorphism is changed from the α-type to the stable β-type during tableting and storage, the tableting and storage stability can be improved.
In addition, the transition from α-type to β-type is known as solid-phase transition, and if it is an oil with a melting point of 50 to 80 ° C., it can be left over at a temperature of 10 to 30 ° C. or less over time. Transition.

これらの多形を同定する一般的な手法は、X線回折法があり、回折条件は下記のブラックスの式によって与えられる。
2dsinθ=nλ(n=1、2、3・・・)
この式を満たす位置に回折ピークが現れる。ここでdは格子定数、θは回折(入射)角、λはX線の波長、nは自然数である。短面間隔に対応する回折ピークの2θ=16〜27°からは、結晶中の側面のパッキング(副格子)に関する情報が得られ、多形の同定を行うことができ、特にトリアシルグリセロールの場合、2θ=19、23、24°にβ型の特徴的ピークが、21°にα型に特徴的なピークが出現する。但し、X線の光源としてCuKα線(1.54Å)が最もよく利用される。
本発明はこれらの知見をもとに、被覆する油脂粉末の多形をβ型の特徴的ピークである2θ=19°のピーク強度とα型の特徴的ピークであるピーク強度比(19°/21°強度比)を用いて、その多形の状態を表すことにした。この比が0.6以下のとき、多形中、α型の比率が50%以上である場合に相当する。
そして、油脂粉末における被覆時の多形をα型とし、及び被覆した油脂の多形をβ型に転移すると、マスキング効果、舌触り、打錠性、保存安定性にも優れた覆粉体が製造できることを見出して、本発明を完成したものである。
A general method for identifying these polymorphs is an X-ray diffraction method, and diffraction conditions are given by the following Blacks equation.
2 d sin θ = nλ (n = 1, 2, 3,...)
A diffraction peak appears at a position satisfying this equation. Here, d is a lattice constant, θ is a diffraction (incident) angle, λ is an X-ray wavelength, and n is a natural number. From 2θ = 16 to 27 ° of the diffraction peak corresponding to the short face interval, information on the side packing (sublattice) in the crystal can be obtained, and polymorphism can be identified, particularly in the case of triacylglycerol. A characteristic peak of β type appears at 2θ = 19, 23, 24 °, and a characteristic peak of α type appears at 21 °. However, CuKα rays (1.54 Å) are most often used as an X-ray light source.
In the present invention, based on these findings, the polymorph of the oil / fat powder to be coated is converted into a β-type characteristic peak 2θ = 19 ° peak intensity ratio and an α-type characteristic peak intensity ratio (19 ° / 21 degree intensity ratio) was used to represent the polymorphic state. When this ratio is 0.6 or less, it corresponds to the case where the α-type ratio in the polymorph is 50% or more.
And when the polymorph of the oil / fat powder is α-type and the polymorph of the coated oil / fat is transferred to β-type, the coated powder with excellent masking effect, touch, tableting and storage stability is produced. The present invention has been completed by finding out what can be done.

本発明は下記(1)及び(2)の発明である。
(1)下記の(A)〜(C)工程を含み、呈味成分を含有する油脂被覆粉末の製造方法。
(A)呈味成分を含有する粉末にゼインを被覆する工程。
(B)前記(A)工程で得られたゼイン被覆粉末に、平均粒径1〜50μm、融点50〜80℃であり、光源としてCuKα線を用いたX線回折測定における2θ(19°)のピーク強度と2θ(21°)のピーク強度比(19°/21°強度比)が0.6以下である硬化油脂粉末を、粉体温度が45℃以下となる条件で衝突させ、被覆粉末を得る工程。
(C)前記工程(B)で得られた被覆粉末を、35〜60℃において、1時間〜200時間テンパリングする工程。
The present invention includes the following inventions (1) and (2).
(1) A method for producing an oil-coated powder comprising the following steps (A) to (C) and containing a taste component.
(A) The process of coat | covering zein on the powder containing a taste component.
(B) The zein-coated powder obtained in the step (A) has an average particle diameter of 1 to 50 μm, a melting point of 50 to 80 ° C., and 2θ (19 °) in X-ray diffraction measurement using CuKα rays as a light source. Hardened oil and fat powder having a peak intensity ratio (19 ° / 21 ° intensity ratio) of peak intensity and 2θ (21 °) of 0.6 or less is collided under a condition that the powder temperature is 45 ° C. or less. Obtaining step.
(C) A step of tempering the coating powder obtained in the step (B) at 35 to 60 ° C. for 1 hour to 200 hours.

前記(1)の製造方法により得られた、平均粒径が100〜300μmである油脂被覆粉末。   An oil-coated powder having an average particle size of 100 to 300 μm obtained by the production method of (1).

本発明によれば、呈味成分を十分に被覆でき、マスキング効果、舌触り、打錠性、保存安定性にも優れた油脂覆粉末の製造方法を提供できる。   ADVANTAGE OF THE INVENTION According to this invention, the manufacturing method of the fat-and-oil covering powder which can fully coat | cover a taste component and was excellent also in the masking effect, the touch, the tableting property, and the storage stability can be provided.

本発明は、下記の(A)工程〜(C)工程を含むことを特徴とする。
(A)工程
本発明における(A)工程は、呈味成分について(B)工程での油脂被覆を容易にするため、呈味成分をゼインで被覆する工程である。
本発明に用いる呈味成分は、味を感じさせる粉末であれば特に限定するものではなく、生薬、ビタミンB類、ハーブ類、グルコサミン、L−ロイシン等の苦味成分、クエン酸、リンゴ酸等の酸味成分、砂糖、ステビア等の味を感じさせる粉末である。本発明の呈味成分は呈味物質それ自体の粉末であっても、デキストリン、澱粉等の粉末に呈味物質を含有させた粉末であってもよい。
粉末の平均粒径は1〜300μmであることが好ましい。1μmより小さい場合、表面積が大きくゼイン被覆の効果が低下し、300μmより大きい場合は、最終的に製造される油脂被覆粉末の舌触りに悪い影響を与え好ましくない。300μmより大きい場合は、所望の粒度に粉砕して使用してもよい。
The present invention is characterized by including the following steps (A) to (C).
(A) Process (A) Process in this invention is a process of coat | covering a taste component with zein, in order to make the oil-fat coating | coating in (B) process easy about a taste component.
The taste component used in the present invention is not particularly limited as long as it is a powder that gives a taste, and includes herbal medicines, vitamin Bs, herbs, bitterness components such as glucosamine and L-leucine, citric acid, malic acid and the like. It is a powder that makes you feel the taste of sour ingredients, sugar, stevia, etc. The taste component of the present invention may be a powder of the taste substance itself or a powder containing a taste substance in a powder such as dextrin or starch.
The average particle size of the powder is preferably 1 to 300 μm. If it is smaller than 1 μm, the surface area is large and the effect of zein coating is reduced, and if it is larger than 300 μm, the final touch of the oil-coated powder produced is adversely affected. If it is larger than 300 μm, it may be used after being pulverized to a desired particle size.

本発明において、ゼインを被膜材として使用する。ゼインは、トウモロコシ由来の蛋白質であり、分子量は21,000〜25,000である。市販品としては、小林ツェインDP(小林香料株式会社)などが挙げられる。ゼインの被覆量は、工程Aにより得られるゼイン被覆粉末の4〜25質量%が好ましい。4質量%より少ない場合、被覆が十分でなく、油脂被覆をしても味のマスキング効果が不十分となる。一方、25質量%より多い場合は、製造される油脂被覆粉末を用い打錠した場合に錠剤の硬度が低下するので、好ましくない。
ゼインはアルコールに溶解し、ゼラチン等の造粒や結合に使用される他の水溶性物質と比べて油脂と親和性の被膜材であり、後の油脂被覆に適した膜素材である。
In the present invention, zein is used as a coating material. Zein is a protein derived from corn and has a molecular weight of 21,000-25,000. Examples of commercially available products include Kobayashi Zein DP (Kobayashi Fragrance Co., Ltd.). The coating amount of zein is preferably 4 to 25% by mass of the zein-coated powder obtained in step A. When the amount is less than 4% by mass, the coating is not sufficient, and the taste masking effect is insufficient even when the oil or fat is coated. On the other hand, when the amount is more than 25% by mass, the tablet hardness is lowered when tableting is performed using the produced oil-coated powder, which is not preferable.
Zein is a film material that dissolves in alcohol and is more compatible with fats and oils than other water-soluble substances used for granulation and binding, such as gelatin, and is suitable for later fat coating.

本発明において、中鎖トリグリセリドを使用するとゼインの被膜効果が高まり、味のマスキング効果が増す。ここで、中鎖トリグリセリドとは、グリセリン骨格に炭素数8〜10の脂肪酸がエステル化結合した油脂化合物であり、例えばカプリル酸トリグリセリド、カプリン酸トリグリセリドが挙げられる。本発明において使用する中鎖トリグリセリドは炭素数8と炭素数10の脂肪酸の両方を有する中鎖トリグリセリドが好ましい。中鎖トリグリセリドの市販品としてはパナセート810(商品名、日本油脂株式会社)、ココナードMT(商品名、花王株式会社)などが挙げられる。中鎖トリグリセリドの使用量は、ゼインの使用量の0.1〜20質量%が好ましい。0.1質量%より少ない場合、味マスキング効果が低下する。一方、20質量%より多い場合は、A工程のゼイン被覆時に団粒が生じる。   In the present invention, when medium chain triglyceride is used, the coating effect of zein is enhanced and the taste masking effect is increased. Here, the medium chain triglyceride is an oil and fat compound in which a fatty acid having 8 to 10 carbon atoms is esterified to a glycerin skeleton, and examples thereof include caprylic acid triglyceride and capric acid triglyceride. The medium chain triglyceride used in the present invention is preferably a medium chain triglyceride having both C8 and C10 fatty acids. Examples of commercially available medium-chain triglycerides include Panacet 810 (trade name, Nippon Oil & Fat Co., Ltd.), Coconut MT (trade name, Kao Corporation), and the like. The amount of medium chain triglyceride used is preferably 0.1 to 20% by weight of the amount of zein used. When it is less than 0.1% by mass, the taste masking effect is lowered. On the other hand, when it is more than 20% by mass, agglomerates are formed during the zein coating in the step A.

本発明の(A)工程の製造方法は、呈味成分を含有する粉末75〜96質量%の表面に、ゼイン4〜25質量%となるようにエタノール水溶液を噴霧する。   The manufacturing method of the (A) process of this invention sprays ethanol aqueous solution so that it may become 4-25 mass% of zein on the surface of powder 75-96 mass% containing a taste component.

呈味成分を含有する粉末の表面にゼインを被覆する際は、転動流動層コーティング装置を用い、処理容器内で流動化エアーによって流動化状態にした粉体により、ゼインのエタノール水溶液を噴霧することが好ましい。中鎖トリグリセリドを使用する場合は、ゼインのエタノール水溶液中に添加して用いることが好ましい。   When zein is coated on the surface of a powder containing a taste component, an aqueous ethanol solution of zein is sprayed with a powder fluidized with fluidized air in a processing vessel using a rolling fluidized bed coating apparatus. It is preferable. When using a medium chain triglyceride, it is preferable to add it to an aqueous ethanol solution of zein.

転動流動層コーティング装置は、装置下部に回転ディスクが設置された流動層コーティング装置である。粉体は、装置内下部から流入した空気により流動化させ、更に回転ディスクの遠心力を加えることにより、流動層内壁を転がるように運動する。通常の流動状態に比べて、粉末の結合による造粒が抑制され、効率良く粉末に被覆ができる。これにゼイン溶液を噴霧乾燥できる装置であればよく、市販されている装置としては、(株)ダルトン製「商品名:ニューマルメラーザー」、(株)パウレック製「商品名:マルチプレックス」等が挙げられる。さらには回転ディスクの上面には、円錐形のコーン部と複数のブレードが設けられていることが好ましい。ブレードによる転動圧密作用により、団粒の発生が抑えられ、シャープな粒度分布を有する被覆粉体を得ることが可能となる。また、被膜が展延作用を受け、均一および強度の高い被覆粉体を得ることができる。
スプレーの方式は、回転ディスク上で転動運動する粉体の流れに、装置下方の側面から接線方向(回転ディスクの回転方向)にスプレー液を噴霧するタンジェンシャルスプレー方式が好ましい。一般的な流動層造粒装置に使用されるスプレー方式は、流動化した粉体の上部より下方に向けて液滴をスプレーするトップスプレー式であるが、タンジェンシャルスプレー方式は、コーティングゾーン内を運動する粉体に集中的にスプレー液を噴霧でき、粉体とスプレーノズルとの距離が常に一定に保たれるため、良好な被覆が可能となる。
The rolling fluidized bed coating apparatus is a fluidized bed coating apparatus in which a rotating disk is installed at the lower part of the apparatus. The powder is fluidized by the air flowing in from the lower part of the apparatus, and further moves by rolling the inner wall of the fluidized bed by applying a centrifugal force of the rotating disk. Compared to the normal fluid state, granulation due to the binding of powder is suppressed, and the powder can be coated efficiently. Any device capable of spray drying the zein solution may be used. Examples of commercially available devices include “Product Name: New Mullerer” manufactured by Dalton Co., Ltd. and “Product Name: Multiplex” manufactured by POWREC. Is mentioned. Furthermore, it is preferable that a conical cone portion and a plurality of blades are provided on the upper surface of the rotating disk. Due to the rolling compaction action by the blade, the generation of aggregates is suppressed, and a coated powder having a sharp particle size distribution can be obtained. Further, the coating film is subjected to a spreading action, and a uniform and high coated powder can be obtained.
The spray method is preferably a tangential spray method in which a spray liquid is sprayed in a tangential direction (rotating direction of the rotating disk) from the side surface below the apparatus to the flow of the powder rolling on the rotating disk. The spray method used in a general fluidized bed granulator is a top spray method in which droplets are sprayed downward from the top of the fluidized powder, while the tangential spray method is used in the coating zone. Since the spray liquid can be sprayed intensively on the moving powder and the distance between the powder and the spray nozzle is always kept constant, good coating is possible.

噴霧するゼインのエタノール水溶液は、エタノール水溶液100質量部に対して、ゼインを4〜25質量部を溶解させた溶液が好ましい。エタノール水溶液100質量部に対して、ゼインを4質量部未満使用する際は、ゼインのエタノール水溶液の噴霧工程時間が長くなり、製造効率が悪くなる。また、25質量部を超えるとゼインのエタノール水溶液の粘性が大きくなり、接着度が大きくなり、粉体間での凝集が起こり団粒形成しやすい。
中鎖トリグリセライドを添加する場合は、エタノール水溶液100質量部に対して中鎖トリグリセリドを0.1〜20質量部添加する。0.1質量部以上添加すると、団粒形成を防止し、シャープな粒度分布のゼイン被覆粉末を得られる。一方、20質量部を超えるとエタノール水溶液との分離が起こり、被覆が不均一となり好ましくない。
The ethanol solution of zein to be sprayed is preferably a solution in which 4 to 25 parts by mass of zein is dissolved with respect to 100 parts by mass of the ethanol aqueous solution. When less than 4 parts by mass of zein is used with respect to 100 parts by mass of the ethanol aqueous solution, the time for spraying the ethanol aqueous solution of zein becomes long, and the production efficiency deteriorates. On the other hand, when the amount exceeds 25 parts by mass, the viscosity of the zein aqueous ethanol solution increases, the degree of adhesion increases, and aggregation occurs between the powders, thereby forming aggregates.
When adding medium chain triglyceride, 0.1-20 mass parts of medium chain triglycerides are added with respect to 100 mass parts of ethanol aqueous solution. When 0.1 part by mass or more is added, formation of aggregates is prevented, and a zein-coated powder having a sharp particle size distribution can be obtained. On the other hand, when the amount exceeds 20 parts by mass, separation from the aqueous ethanol solution occurs, resulting in non-uniform coating.

ゼイン及び中鎖トリグリセリドを溶解させるエタノール水溶液は60〜90質量%エタノール水溶液が好ましい。ここでエタノール水溶液中のエタノール濃度が60質量%未満ではゼインの溶解量が低くなる。また、90質量%を超えると溶液がゲル化しやすく好ましくない。   The ethanol aqueous solution in which zein and medium chain triglycerides are dissolved is preferably a 60 to 90% by mass ethanol aqueous solution. Here, when the ethanol concentration in the ethanol aqueous solution is less than 60% by mass, the amount of zein dissolved is low. Moreover, when it exceeds 90 mass%, a solution will gelatinize easily and is unpreferable.

(A)工程により得られたゼイン被覆粉末の平均粒径は、100〜300μmであることが好ましい。100μm未満の場合は、ゼイン被膜へ硬化油脂粉末を衝突させる際に、付着力、硬化油脂被膜の展延力が低下し、300μmを超える場合、本発明の油脂被覆粉末の舌触りが悪くなる。ここで、(A)工程における平均粒径の調整は、造粒を抑制できる上記のゼイン被覆の条件で行う。後に粉砕により所望の平均粒径に調整しても、粒子の割れによる芯材表面が露出することになり、マスキング効果を低下するので好ましくない。   The average particle size of the zein-coated powder obtained by the step (A) is preferably 100 to 300 μm. When the thickness is less than 100 μm, when the hardened oil / fat powder collides with the zein coating, the adhesive force and the spreading force of the hardened oil / fat coating are reduced. Here, the adjustment of the average particle diameter in the step (A) is performed under the above zein coating conditions capable of suppressing granulation. Even if it is adjusted to a desired average particle size by pulverization later, the surface of the core material due to cracking of the particles will be exposed and the masking effect will be reduced, which is not preferable.

(B)工程
本発明における(B)工程は、前記(A)工程で得られたゼイン被覆粉末を油脂被覆する工程である。
本工程に使用する硬化油脂粉末の融点が50〜80℃であることが好ましい。50℃未満の場合には、硬化油脂をゼイン被覆粉末に被覆させる工程において、固結状態になりやすいので好ましくない。また、融点が80℃を超える硬化油脂を使用する場合は、ゼイン被覆粉末への付着力が低下し、被覆状態が悪くなる。
融点が50〜80℃である硬化油脂粉末としては、菜種硬化油、パーム硬化油、大豆硬化油、ハイエルシン酸菜種硬化油、牛脂硬化油等が挙げられ、これらを1種または2種以上の混合油脂を使用する。硬化油脂は一般的な水素添加により調製されたものを使用するが、ヨウ素価が3.0以下の硬化油脂は、(C)工程におけるテンパリングにより、より機密な結晶構造を形成し、味のマスキング効果、打錠性及び保存安定性が高くなり好ましい。更には、ヨウ素価が0.3以下の菜種硬化油、大豆硬化油、ハイエルシン酸菜種硬化油は、脂肪酸組成が高純度のステアリン酸となり、更に機密な結晶構造を形成するため好ましい。
(B) Process (B) process in this invention is a process of oil-fat-coating the zein coating powder obtained at the said (A) process.
It is preferable that melting | fusing point of the hardened oil and fat powder used for this process is 50-80 degreeC. When it is less than 50 ° C., it is not preferable because it tends to be consolidated in the step of coating the zein-coated powder with the hardened fat. Moreover, when using the hardened fats and oils whose melting | fusing point exceeds 80 degreeC, the adhesive force to zein coating | coated powder falls and a coating state worsens.
Examples of the hardened oil and fat powder having a melting point of 50 to 80 ° C. include rapeseed hardened oil, hardened palm oil, hardened soybean oil, hardened high erucic acid rapeseed oil, hardened beef tallow oil, etc., and these may be used alone or in combination of two or more. Use oils and fats. Hardened fats and oils prepared by general hydrogenation are used, but hardened fats and oils having an iodine value of 3.0 or less form a more confidential crystal structure by tempering in the step (C), and mask the taste. The effect, tableting property and storage stability are increased, which is preferable. Furthermore, rapeseed hydrogenated oil, soybean hardened oil, and high erucic acid rapeseed hardened oil having an iodine value of 0.3 or less are preferable because the fatty acid composition becomes highly pure stearic acid and forms a more secret crystal structure.

また、本発明に使用する硬化油脂粉末は、トリアシルグリセロールの含有量が95質量%以上のものが好ましい。硬化油脂には、モノグリセロール、ジグリセロール、脂肪酸等の不純物が含まれるが、これらの不純物は、機密な結晶構造の形成を阻害するからである。   In addition, the hardened oil / fat powder used in the present invention preferably has a triacylglycerol content of 95% by mass or more. Hardened fats and oils contain impurities such as monoglycerol, diglycerol, and fatty acids, and these impurities hinder the formation of a secret crystal structure.

本発明の硬化油脂粉末の平均粒径は1〜50μmのものを使用することが好ましい。平均粒径が1μmより小さくするには工業的に容易ではなく、また、50μmより大きい場合、(A)工程で得られたゼイン被覆粉末表面に付着できないことがあり、良好な油脂被膜を形成できない。硬化油脂の被膜量は、(A)工程で得られたゼイン被覆粉末60〜97質量%、硬化油脂3〜40質量%であることが好ましい。硬化油脂の被膜量が3質量%より低い場合、味のマスキング効果が不十分となり、また、40質量%より高い場合、被覆量に対して過剰な硬化油脂粉末が槽内壁に付着して固結する。   The average particle diameter of the hardened oil / fat powder of the present invention is preferably 1 to 50 μm. When the average particle size is smaller than 1 μm, it is not industrially easy. When the average particle size is larger than 50 μm, it may not adhere to the surface of the zein-coated powder obtained in the step (A), and a good oil film cannot be formed. . The coating amount of the hardened oil / fat is preferably 60 to 97% by weight of the zein-coated powder obtained in the step (A) and 3 to 40% by weight of the hardened oil / fat. When the coating amount of the hardened fat is lower than 3% by mass, the taste masking effect is insufficient, and when it is higher than 40% by weight, excessive hardened fat powder adheres to the inner wall of the tank and solidifies. To do.

本発明において、光源としてCuKα線を用いたX線回折測定における2θ(19°)のピーク強度と2θ(21°)のピーク強度比(19°/21°強度比)が0.6以下である硬化油脂粉末を被覆に用いる。このピーク強度比(19°/21°強度比)は、前記のようにα型結晶多形及びβ型結晶多形の割合の指標となるものであり、本発明はピーク強度比(19°/21°強度比)が0.6以下のα型結晶多形に富む多形の硬化油脂粉末を用いることを特徴とする。
ピーク強度比(19°/21°強度比)が0.6を超える場合は、β型に富む硬化油脂粉末であり、ゼイン被膜との付着力低下の原因となる。
なお、ピーク強度比(19°/21°強度比)が0.6以下の硬化油脂粉末は、硬化油脂を融点以上の熱で溶解し、これを急速に冷却して再結晶化させ、粉砕機等で平均粒径1〜50μmにまで粉砕することで容易に得ることができる。油脂の再結晶化には、硬化油脂を板状またはフレーク状にし、これを粉砕する方法や、スプレークーリングにより、粉砕することなく平均粒径1〜50μmの硬化油脂粉末を得る方法等がある。
In the present invention, the peak intensity ratio between 2θ (19 °) and 2θ (21 °) (19 ° / 21 ° intensity ratio) in an X-ray diffraction measurement using CuKα rays as a light source is 0.6 or less. Hardened fat powder is used for coating. This peak intensity ratio (19 ° / 21 ° intensity ratio) serves as an index of the ratio of α-type crystal polymorph and β-type crystal polymorph as described above. In the present invention, the peak intensity ratio (19 ° / 21 ° A polymorphic hardened oil / fat powder rich in α-type crystal polymorphism having a 21 ° intensity ratio of 0.6 or less is used.
When the peak intensity ratio (19 ° / 21 ° intensity ratio) exceeds 0.6, it is a hard fat powder rich in β-type, which causes a decrease in adhesion to the zein film.
In addition, the hardened oil and fat powder having a peak intensity ratio (19 ° / 21 ° intensity ratio) of 0.6 or less is obtained by dissolving the hardened oil and fat with heat equal to or higher than the melting point and rapidly cooling and recrystallizing it. Etc., and can be easily obtained by pulverizing to an average particle size of 1 to 50 μm. For recrystallization of fats and oils, there are a method in which hardened fats and oils are made into a plate or flake shape and pulverized, and a method of obtaining hardened fats and oils having an average particle diameter of 1 to 50 μm without pulverizing by spray cooling.

本発明において硬化油脂被膜を形成する工程は、(A)工程により得られたゼイン被覆粉末に硬化油脂粉末を衝突させてゼイン被覆粉末の全周囲表面に硬化油脂を固着させて被覆する工程である。高速攪拌混合機としては、奈良機械(株)製「諸品名:OMダイザー」、(株)パウレック製「商品名:バーチカルグラニュレーター」が挙げられる。
衝突条件は固体状の硬化油脂粉末がゼイン被覆粉末と衝突する条件であり、粉体温度が45℃以下であることが好ましい。45℃を超える場合、硬化油脂が軟化して槽内で固結するおそれがある。
In the present invention, the step of forming the hardened oil / fat coating is a step in which the hardened oil / fat powder collides with the zein-coated powder obtained in the step (A) and the hardened fat / oil is fixed on the entire peripheral surface of the zein-coated powder. . Examples of the high-speed stirring mixer include “Product Name: OM Dizer” manufactured by Nara Machinery Co., Ltd., and “Product Name: Vertical Granulator” manufactured by Paulek Co., Ltd.
The collision condition is a condition in which the solid hardened oil / fat powder collides with the zein-coated powder, and the powder temperature is preferably 45 ° C. or less. When it exceeds 45 degreeC, there exists a possibility that hardened fats and oils may soften and it may solidify in a tank.

(C)工程
本発明の(C)工程は、(B)工程でゼイン被覆粉末の表面に被覆されたα型多形に富む油脂をβ型多形に富む油脂に転移させる工程である。
本発明の(C)工程では油脂被覆粉末を35〜60℃で1〜200時間テンパリングすることにより、硬化油脂の結晶多形を不安定型のα型から安定型のβ型へ転移させる。
テンパリング温度が35℃より低い場合、転移に長時間を要し、生産性が悪くなる。また、テンパリング温度が60℃を超えた場合、硬化油脂の被膜が溶解し、呈味のマスキング効果が低くなる。
更には、テンパリング温度を40〜50℃とすると、テンパリング時間が1〜100時間に短縮でき、生産効率が高くなり好ましい。40℃以上とすると、固相転移速度が上昇するが、50℃を超えると、硬化油脂の融点によっては硬化油脂被膜が軟化し、被覆粒子同士が固結や被膜が剥がれるなどの問題を生じるおそれがある。
また、テンパリング時間は、ピーク強度比(19°/21°強度比)が2以上となるのに必要な時間以上が好ましい。
この工程(C)により、α型では、十分なマスキング効果、打錠性及び保存安定性が得られないが、β型へ転移することにより、マスキング効果、打錠性及び保存安定性が高くなる。
Step (C) Step (C) of the present invention is a step of transferring the fat rich in α-type polymorph coated on the surface of the zein-coated powder in step (B) to the fat rich in β-type polymorph.
In the step (C) of the present invention, the oil-coated powder is tempered at 35 to 60 ° C. for 1 to 200 hours, so that the crystal polymorph of the hardened fat is transferred from the unstable α-type to the stable β-type.
When the tempering temperature is lower than 35 ° C., the transition takes a long time and the productivity is deteriorated. Moreover, when a tempering temperature exceeds 60 degreeC, the film of hardened fats and oils will melt | dissolve and the masking effect of taste will become low.
Furthermore, when the tempering temperature is 40 to 50 ° C., the tempering time can be shortened to 1 to 100 hours, and the production efficiency is increased, which is preferable. If it is 40 ° C. or higher, the solid phase transition rate will increase, but if it exceeds 50 ° C., the hardened oil / fat coating may soften depending on the melting point of the hardened oil / fat, causing problems such as solidification of the coated particles and peeling of the coating. There is.
The tempering time is preferably longer than the time required for the peak intensity ratio (19 ° / 21 ° intensity ratio) to be 2 or more.
By this step (C), the α type cannot obtain a sufficient masking effect, tableting property and storage stability, but the transition to the β type increases the masking effect, tableting property and storage stability. .

本発明で得られる被覆粉末の平均粒径は100〜300μmであることが好ましい。平均粒径が100μmより小さい場合、呈味のマスキング効果が弱く、300μmより大きい場合、舌触りが悪くなる。
本発明で得られる被覆粉末は、苦味等の味を有する医薬品や健康食品の服用を容易にするために使用することができる。また、クエン酸、リンゴ酸などの酸味剤を被覆した本発明の被覆粉末を、ガムなどに添加することにより、噛むことにより、徐々に呈味を放出し、長時間呈味を維持する食品にも応用できる。
The average particle size of the coating powder obtained in the present invention is preferably 100 to 300 μm. When the average particle size is smaller than 100 μm, the taste masking effect is weak, and when it is larger than 300 μm, the tongue feel is poor.
The coated powder obtained in the present invention can be used to facilitate the taking of pharmaceuticals and health foods having a taste such as bitterness. In addition, by adding the coating powder of the present invention coated with a sour agent such as citric acid and malic acid to a gum, etc., by chewing it, the taste is gradually released and the food is maintained for a long time. Can also be applied.

以下、実施例及び比較例により更に詳細に説明するが、本発明はこれらに限定されるものではない。   Hereinafter, although an Example and a comparative example demonstrate in detail, this invention is not limited to these.

(融点、ヨウ素価測定法)
日本油化学会制定の基準油脂分析試験法に準じて行った。融点は「上昇融点法」を、ヨウ素価は「ウィイス−四塩化炭素法」を用いた。
(Measuring method of melting point and iodine number)
This was performed in accordance with the standard oil analysis method established by the Japan Oil Chemists' Society. For the melting point, the “rising melting point method” was used, and for the iodine value, the “Wiis-carbon tetrachloride method” was used.

(硬化油脂の純度)
約1gの硬化油脂粉末を正確に秤量し、30mLのクロロホルムに溶解し、ろ過する。ろ紙をクロロホルムで十分に洗い、硬化油脂の溶解した液を回収する。回収したクロロホルム溶液をロータリーエバポレーター(液温度70℃)で十分に乾固し、回収した固形分重量を測定する。試験に供した硬化油脂粉末に対する回収した固形分の割合(y%)を求める。固形分をクロロホルムに溶解し、イアトロスキャン「商品名;MK−5」(イアトロン社製)を用いて(展開液;ヘキサン/エーテル(80/20))、総面積に対するトリアシルグリセロールの面積比を求め、上記y%を乗じて、トリアシルグリセロールの純度を求める。
(Purity of hardened oil and fat)
About 1 g of hardened oil and fat powder is accurately weighed, dissolved in 30 mL of chloroform, and filtered. Wash the filter paper thoroughly with chloroform and collect the liquid in which the hardened fats and oils are dissolved. The collected chloroform solution is sufficiently dried by a rotary evaporator (liquid temperature 70 ° C.), and the weight of the collected solid content is measured. The ratio (y%) of the collected solid content to the hardened oil / fat powder subjected to the test is determined. The solid content was dissolved in chloroform, and the area ratio of triacylglycerol to the total area was measured using Iatroscan “trade name; MK-5” (manufactured by Iatron) (developing solution: hexane / ether (80/20)). Is multiplied by y% to determine the purity of triacylglycerol.

(19°/21°強度比)
X線回折測定は、(株)リガク製「商品名:RINT−Ultima」で測定を行った。管電圧:20kV、管電流:40mA、開始角度3°、終了角度30°、スキャンスピード:2°/分、試料サンプルをサンプルホルダーに充填し、測定を行った。硬化油脂の結晶多形の同定には、前記のとおり、2θ=16〜27°のピーク強度、特に19°/21°強度比を算出することができる。
(19 ° / 21 ° intensity ratio)
The X-ray diffraction measurement was performed by “trade name: RINT-Utima” manufactured by Rigaku Corporation. Tube voltage: 20 kV, tube current: 40 mA, start angle 3 °, end angle 30 °, scan speed: 2 ° / min, a sample sample was filled in a sample holder, and measurement was performed. As described above, the peak intensity of 2θ = 16 to 27 °, particularly the 19 ° / 21 ° intensity ratio can be calculated for identification of the crystal polymorph of the hardened fat.

(平均粒径)
粉末の平均粒径は、レーザー乾式粒度分布測定機(商品名:SALD−2100、(株)島津製作所製)を用いて測定した。内蔵するプログラム「Wing−1」により、データ処理された値にて評価した。
(Average particle size)
The average particle size of the powder was measured using a laser dry particle size distribution analyzer (trade name: SALD-2100, manufactured by Shimadzu Corporation). Evaluation was performed using data-processed values by the built-in program “Wing-1”.

(舌触り)
約50mgを舌に乗せ、○:ざらつきが少ない、△:ややざらついている、×ざらざらとしている、の3段階で評価した。
(Feeling of the tongue)
About 50 mg was placed on the tongue, and the evaluation was made in three stages: ○: little roughness, Δ: slightly rough, and × rough.

(呈味強度)
約50mgを舌に乗せ、20秒間そのまま口中に含んだあとに飲み込む。このときに感じる呈味の強度を、1:感じない、2:ほとんど感じない、3:やや感じる、4:感じる、5:強く感じる、の5段階で評価した。
(Taste strength)
Put about 50mg on your tongue and swallow it after putting it in your mouth for 20 seconds. The intensity of the taste felt at this time was evaluated in five stages: 1: not felt, 2: hardly felt, 3: slightly felt, 4: felt, 5: felt strongly.

(保存安定性)
製造後1ヶ月(常温保管)の2重被覆粉末の状態を目視検査した。
(Storage stability)
The state of the double-coated powder one month after production (room temperature storage) was visually inspected.

(打錠性)
実施例、比較例により得られた粉末300g、乳糖(旭化成ケミカルズ(株)製、商品名:SUPER TAB)200g、及びショ糖脂肪酸エステル(三菱化学フーズ(株)製、商品名:シュガーエステルB−370F)10gを混合し、ロータリー式打錠機を用いて打錠した。錠剤重量を400mgとし、杵種を10mm径、R=8.5mm、打錠圧を10000Nの条件で打錠品を作製した。これらの打錠品から無作為に200錠を取り出し、スティッキングの有無を調べた。
(Tabletability)
300 g of powder obtained by Examples and Comparative Examples, 200 g of lactose (manufactured by Asahi Kasei Chemicals Co., Ltd., trade name: SUPER TAB), and sucrose fatty acid ester (manufactured by Mitsubishi Chemical Foods Co., Ltd., trade name: Sugar Ester B- (370F) 10 g was mixed and tableted using a rotary tableting machine. A tableted product was prepared under the conditions of a tablet weight of 400 mg, a grape seed of 10 mm diameter, R = 8.5 mm, and a tableting pressure of 10,000 N. 200 tablets were randomly taken out from these tableted products and examined for the presence of sticking.

実施例1
グルコサミン粉末(焼津水産化学工業(株)製、商品名:ナチュラルグルコサミン、平均粒径108μm)500gを転動流動層装置((株)ダルトン製、商品名:ニューマルメライザーNQ−160)に仕込み、ゼイン(小林香料(株)製、商品名:小林ツェインDP)58.8gを含水エタノール(精製水/エタノール=30/70(v/v))530gに溶解したコーティング液を噴霧した。運転条件は、給気温度:75℃、給気風量:1m/min、ローター回転数:300rpm、噴霧液速度:15g/minで行った。平均粒径が125μmのゼイン被覆粉末を503g得た。
得られたゼイン被覆粉末450gと、菜種極度硬化油(融点67℃、19°/21°ピーク強度比0.35、ヨウ素価1.1、トリアシルグリセロール純度100%、平均粒径12μm)50gを高速攪拌機((株)パウレック製、商品名:VG−05)に仕込み、ブレード回転数500rpm、クロススクリュー回転数2000rpm、ジャケット温度25℃にて40分間混合した。これを45℃の恒温槽にいれ、5時間静置し、平均粒径が121μmの油脂被覆粉末を490g得た。得られた油脂被覆粉末について、舌触り、呈味強度、保存安定性試験を行った。試験の結果を表1に示す。
Example 1
500 g of glucosamine powder (manufactured by Yaizu Suisan Kagaku Kogyo Co., Ltd., trade name: natural glucosamine, average particle size 108 μm) is charged into a rolling fluidized bed apparatus (manufactured by Dalton Co., Ltd., trade name: Numeralizer NQ-160). A coating solution in which 58.8 g of zein (manufactured by Kobayashi Fragrance Co., Ltd., trade name: Kobayashi Zein DP) was dissolved in 530 g of hydrous ethanol (purified water / ethanol = 30/70 (v / v)) was sprayed. The operating conditions were as follows: supply air temperature: 75 ° C., supply air volume: 1 m 3 / min, rotor rotation speed: 300 rpm, spray liquid speed: 15 g / min. 503 g of zein-coated powder having an average particle size of 125 μm was obtained.
450 g of the obtained zein-coated powder and 50 g of rapeseed extremely hardened oil (melting point 67 ° C., 19 ° / 21 ° peak intensity ratio 0.35, iodine value 1.1, triacylglycerol purity 100%, average particle size 12 μm) The mixture was charged into a high-speed stirrer (trade name: VG-05, manufactured by POWREC Co., Ltd.), and mixed for 40 minutes at a blade rotation speed of 500 rpm, a cross screw rotation speed of 2000 rpm, and a jacket temperature of 25 ° C. This was put into a 45 degreeC thermostat, and left still for 5 hours, and 490g of oil-fat coating powder with an average particle diameter of 121 micrometers was obtained. About the obtained oil-and-fat coating powder, the touch, taste strength, and storage stability test were done. The test results are shown in Table 1.

実施例2
実施例1の製造方法において、コーティング液として、ゼイン(小林香料(株)製、商品名:小林ツェインDP)を53g、中鎖トリグリセライド(日本油脂(株)製、商品名:パナセート810)5.9gを含水エタノール(精製水/エタノール=30/70(v/v))530gに溶解したものを使用し、同様に行った。
Example 2
In the production method of Example 1, 53 g of zein (manufactured by Kobayashi Fragrance Co., Ltd., trade name: Kobayashi Zein DP) and medium chain triglyceride (manufactured by Nippon Oil & Fats Co., Ltd., trade name: Panacet 810) are used as the coating liquid. 9 g was dissolved in 530 g of hydrous ethanol (purified water / ethanol = 30/70 (v / v)), and the same procedure was performed.

実施例3
実施例1の製造方法において、油脂被覆材として、菜種極度硬化油(融点67℃、19°/21°ピーク強度比0.55、ヨウ素価1.1、トリアシルグリセロール純度100%、平均粒径12μm)を使用し、同様に行った。
Example 3
In the production method of Example 1, rapeseed extremely hardened oil (melting point 67 ° C., 19 ° / 21 ° peak intensity ratio 0.55, iodine number 1.1, triacylglycerol purity 100%, average particle diameter as fat coating material) 12 μm) was used in the same manner.

実施例4
実施例1の製造方法において、油脂被覆材として、菜種極度硬化油(融点62℃、19°/21°ピーク強度比0.31、ヨウ素価3.2、トリアシルグリセロール純度100%、平均粒径12μm)を使用し、同様に行った。
Example 4
In the production method of Example 1, rapeseed extremely hardened oil (melting point 62 ° C., 19 ° / 21 ° peak intensity ratio 0.31, iodine value 3.2, triacylglycerol purity 100%, average particle size as fat coating material 12 μm) was used in the same manner.

実施例5及び6
実施例1の製造方法において、テンパリング温度及び時間を、実施例5では37℃で5時間、実施例6では55℃3時間とし、同様に行った。
Examples 5 and 6
In the production method of Example 1, the tempering temperature and time were set to 37 ° C. for 5 hours in Example 5, and 55 ° C. for 3 hours in Example 6, and the same procedure was performed.

実施例7
L−ロイシン粉末(協和発酵工業(株)製、商品名:L−ロイシン、平均粒径127μm)500g、ゼイン(小林香料(株)製、商品名:小林ツェインDP)115.4gを含水エタノール(精製水/エタノール=30/70(v/v))654gを用いて、実施例1と同様に製造した。平均粒径が138μmのゼイン被覆粉末を520g得た。
得られたゼイン被覆粉末400gと実施例1の菜種極度硬化油100gを使用し、実施例1と同様に製造した。
得られた2重被覆粉末について、舌触り、呈味強度、打錠試験、保存安定性試験を行った。試験の結果を表1に示す。
Example 7
L-leucine powder (manufactured by Kyowa Hakko Kogyo Co., Ltd., trade name: L-leucine, average particle size 127 μm) 500 g, zein (manufactured by Kobayashi Fragrance Co., Ltd., trade name: Kobayashi Zein DP) 115.4 g of water-containing ethanol ( It was produced in the same manner as in Example 1 using 654 g of purified water / ethanol = 30/70 (v / v)). 520 g of zein-coated powder having an average particle size of 138 μm was obtained.
400 g of the obtained zein-coated powder and 100 g of rapeseed extremely hardened oil of Example 1 were used and produced in the same manner as in Example 1.
The resulting double-coated powder was subjected to touch, taste strength, tableting test, and storage stability test. The test results are shown in Table 1.

Figure 2009084157
Figure 2009084157

比較例1
グルコサミン粉末(焼津水産化学工業(株)製、商品名:ナチュラルグルコサミン、平均粒径108μm)500gを転動流動層装置((株)ダルトン製、商品名:ニューマルメライザーNQ−160)に仕込み、ゼイン(小林香料(株)製「小林ツェインDP」)88.2gを含水エタノール(精製水/エタノール=30/70(v/v))500gに溶解したコーティング液を噴霧した。運転条件は、実施例1と同様に行った。平均粒径が125μmのゼイン被覆粉末を510g得た。
得られたゼイン被覆粉末について、舌触り、呈味強度、保存安定性試験を行った。試験の結果を表2に示す。
Comparative Example 1
500 g of glucosamine powder (manufactured by Yaizu Suisan Kagaku Kogyo Co., Ltd., trade name: natural glucosamine, average particle size 108 μm) is charged into a rolling fluidized bed apparatus (manufactured by Dalton Co., Ltd., trade name: Numeralizer NQ-160). A coating solution in which 88.2 g of zein (“Kobayashi Zein DP” manufactured by Kobayashi Fragrance Co., Ltd.) was dissolved in 500 g of hydrous ethanol (purified water / ethanol = 30/70 (v / v)) was sprayed. The operating conditions were the same as in Example 1. 510 g of zein-coated powder having an average particle size of 125 μm was obtained.
The resulting zein-coated powder was tested for touch, taste strength, and storage stability. The test results are shown in Table 2.

比較例2
グルコサミン粉末(焼津水産化学工業(株)製、商品名:ナチュラルグルコサミン、平均粒径108μm)425gと、菜種極度硬化油75gを、高速攪拌機((株)パウレック製、商品名:VG−05)に仕込み、実施例1と同様に混合した。これを45℃の恒温槽にいれ、12時間静置し、平均粒径が125μmの油脂被覆粉末を490g得た。得られた粉末について、舌触り、呈味強度、保存安定性試験を行った。試験の結果を表2に示す。
Comparative Example 2
425 g of glucosamine powder (made by Yaizu Suisan Chemical Co., Ltd., trade name: natural glucosamine, average particle size 108 μm) and 75 g of rapeseed extremely hardened oil are added to a high-speed stirrer (trade name: VG-05, manufactured by POWREC Co., Ltd.). Preparation and mixing as in Example 1. This was put into a 45 degreeC thermostat, and left still for 12 hours, and 490g of oil-fat coating powder whose average particle diameter is 125 micrometers was obtained. About the obtained powder, the touch, taste strength, and storage stability test were done. The test results are shown in Table 2.

比較例3
実施例1の製造方法において、油脂被覆材として、菜種極度硬化油(融点67℃、19°/21°ピーク強度比2.52、ヨウ素価1.2、トリアシルグリセロール純度100%、平均粒径12μm)を使用し、同様に行った。
Comparative Example 3
In the production method of Example 1, rapeseed extremely hardened oil (melting point: 67 ° C., 19 ° / 21 ° peak intensity ratio: 2.52, iodine number: 1.2, triacylglycerol purity: 100%, average particle size as fat coating material. 12 μm) was used in the same manner.

比較例4〜6
実施例1の製造方法において、テンパリング温度及び時間を、比較例4ではテンパリング処理を行わず、比較例5では30℃で12時間、比較例6では70℃3時間とし、同様に行った。
Comparative Examples 4-6
In the manufacturing method of Example 1, the tempering temperature and time were the same as in Comparative Example 4 except that tempering treatment was not performed, Comparative Example 5 was 30 ° C. for 12 hours, and Comparative Example 6 was 70 ° C. for 3 hours.

比較例7
L−ロイシン粉末(協和発酵工業(株)製、商品名:L−ロイシン、平均粒径127μm)500gに、ゼラチン(新田ゼラチン(株)製「新田ゼラチンGBL−200」)115.4gを精製水2000gに溶解したコーティング液を噴霧した。運転条件は、給気温度:85℃、給気風量:1m3/min、ローター回転数:300rpm、噴霧液速度:12g/minで行った。平均粒径が238μmのゼイン被覆粉末を508g得た。
得られたゼラチン被覆粉末400gと実施例1の菜種極度硬化油100gを使用し、実施例1と同様に製造した。但し、テンパリング処理は行わなかった。
得られた油脂被覆粉末について、舌触り、呈味強度、打錠試験、保存安定性試験を行った。試験の結果を表2に示す。
Comparative Example 7
115.4 g of gelatin (“Nitta Gelatin GBL-200”, manufactured by Nitta Gelatin Co., Ltd.) is added to 500 g of L-leucine powder (manufactured by Kyowa Hakko Kogyo Co., Ltd., trade name: L-leucine, average particle size 127 μm). A coating solution dissolved in 2000 g of purified water was sprayed. The operating conditions were as follows: supply air temperature: 85 ° C., supply air volume: 1 m 3 / min, rotor rotation speed: 300 rpm, spray liquid speed: 12 g / min. 508 g of zein-coated powder having an average particle size of 238 μm was obtained.
Using the obtained gelatin-coated powder 400 g and the rapeseed extremely hardened oil 100 g of Example 1, it was produced in the same manner as in Example 1. However, the tempering process was not performed.
About the obtained oil-and-fat coating powder, the touch, taste strength, tableting test, and storage stability test were performed. The test results are shown in Table 2.

比較例8
比較例7と同様に油脂被覆粉末を調製し、45℃で5時間テンパリング処理を行った。
Comparative Example 8
An oil-coated powder was prepared in the same manner as in Comparative Example 7 and tempered at 45 ° C. for 5 hours.

比較例9
グルコサミン粉末(焼津水産化学工業(株)製、商品名:ナチュラルグルコサミン、平均粒径108μm)500gを流動層造粒装置(フロイント産業(株)製、商品名:フローコーターミニ)に仕込み、実施例1と同様にしてゼイン溶液を噴霧した。スプレーはトップスプレー式を用いた。運転条件は、給気温度:75℃、給気風量:1m/min、噴霧液速度:30g/minで行い、平均粒径399μmの造粒されたゼイン被覆粉末を490g得た。これを用いて、実施例1と同様にして、硬化油脂被覆、テンパリング処理を行った。
Comparative Example 9
Example: 500 g of glucosamine powder (manufactured by Yaizu Suisan Kagaku Kogyo Co., Ltd., trade name: natural glucosamine, average particle size 108 μm) was charged into a fluidized bed granulator (manufactured by Freund Sangyo Co., Ltd., trade name: Flow Coater Mini). The zein solution was sprayed in the same manner as in 1. The spray used the top spray type. The operating conditions were an air supply temperature: 75 ° C., an air supply amount: 1 m 3 / min, and a spray liquid speed: 30 g / min, and 490 g of granulated zein-coated powder having an average particle size of 399 μm was obtained. Using this, cured oil and fat coating and tempering treatment were performed in the same manner as in Example 1.

Figure 2009084157
Figure 2009084157

実施例1及び2と比較例1及び2より、ゼイン及び硬化油脂の被覆粉末が味のマスキング効果が高いことがわかる。比較例3より、結晶多形がβ型である硬化油脂粉末を使用すると、味のマスキング効果が弱い。比較例4〜7では、C工程において、適切なテンパリング処理をしないと、味のマスキング効果、保存安定性、打錠性が低いことがわかる。比較例8と実施例7を比較すると、ゼインを使用することにより、良好な硬化油脂被膜が形成され、味のマスキング効果、打錠性、保存安定性を向上させることがわかる。また、比較例9より、造粒され平均粒径が300μmを超えると、舌触りが悪くなることがわかる。   From Examples 1 and 2 and Comparative Examples 1 and 2, it can be seen that the coating powder of zein and hardened oil has a high taste masking effect. From the comparative example 3, when the hardened oil and fat powder whose crystal polymorph is β type is used, the taste masking effect is weak. In Comparative Examples 4 to 7, it can be seen that the taste masking effect, storage stability, and tableting properties are low unless an appropriate tempering treatment is performed in Step C. Comparing Comparative Example 8 and Example 7, it can be seen that by using zein, a good hardened oil / fat film is formed, and the taste masking effect, tableting property, and storage stability are improved. Further, it can be seen from Comparative Example 9 that when granulated and the average particle size exceeds 300 μm, the touch of the tongue is deteriorated.

Claims (2)

下記の(A)〜(C)工程を含み、呈味成分を含有する油脂被覆粉末の製造方法。
(A)呈味成分を含有する粉末にゼインを被覆する工程。
(B)前記(A)工程で得られたゼイン被覆粉末に、平均粒径1〜50μm、融点50〜80℃であり、光源としてCuKα線を用いたX線回折測定における2θ(19°)のピーク強度と2θ(21°)のピーク強度比(19°/21°強度比)が0.6以下である硬化油脂粉末を、粉体温度が45℃以下となる条件で衝突させ、被覆粉末を得る工程。
(C)前記工程(B)で得られた被覆粉末を、35〜60℃において、1時間〜200時間テンパリングする工程。
The manufacturing method of the fat-and-oil coating powder containing the following (A)-(C) process and containing a taste component.
(A) The process of coat | covering zein on the powder containing a taste component.
(B) The zein-coated powder obtained in the step (A) has an average particle diameter of 1 to 50 μm, a melting point of 50 to 80 ° C., and 2θ (19 °) in X-ray diffraction measurement using CuKα rays as a light source. Hardened oil and fat powder having a peak intensity ratio (19 ° / 21 ° intensity ratio) of peak intensity and 2θ (21 °) of 0.6 or less is collided under a condition that the powder temperature is 45 ° C. or less. Obtaining step.
(C) A step of tempering the coating powder obtained in the step (B) at 35 to 60 ° C. for 1 hour to 200 hours.
請求項1の製造方法により得られた、平均粒径が100〜300μmである油脂被覆粉末。   An oil-coated powder having an average particle size of 100 to 300 µm obtained by the production method of claim 1.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012012308A (en) * 2010-06-29 2012-01-19 House Foods Corp Complex and method for producing the same
JP2013184888A (en) * 2012-03-05 2013-09-19 Nof Corp Covered particle
JP2019059680A (en) * 2017-09-25 2019-04-18 株式会社イムダイン Hydrogen adsorption composition

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012012308A (en) * 2010-06-29 2012-01-19 House Foods Corp Complex and method for producing the same
JP2013184888A (en) * 2012-03-05 2013-09-19 Nof Corp Covered particle
JP2019059680A (en) * 2017-09-25 2019-04-18 株式会社イムダイン Hydrogen adsorption composition

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