JP4446126B2 - Method for producing fast-dissolving konjac mannan - Google Patents

Method for producing fast-dissolving konjac mannan Download PDF

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JP4446126B2
JP4446126B2 JP2007043381A JP2007043381A JP4446126B2 JP 4446126 B2 JP4446126 B2 JP 4446126B2 JP 2007043381 A JP2007043381 A JP 2007043381A JP 2007043381 A JP2007043381 A JP 2007043381A JP 4446126 B2 JP4446126 B2 JP 4446126B2
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konjac mannan
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寿夫 清水
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Description

本発明は、速溶性、すなわち水に膨潤(溶解)する時のピーク粘度に達する時間が短縮されたコンニャクマンナンの製造法に関する。   The present invention relates to a method for producing konjac mannan having a fast solubility, that is, a time required to reach a peak viscosity when swollen (dissolved) in water.

コンニャクマンナンの主成分のグルコマンナンは、その水溶液にアルカリを加え加熱することにより熱不可逆性の弾性ゲルを形成するなどの独特の化学的、物理的性質を有し、これを利用して古来からこんにゃく製造の原料に使用されて来た。こんにゃくの製造には、こんにゃく芋と呼ばれるサトイモ科の植物の塊茎をスライスし、乾燥、粉砕した後風力選別によりデンプン、繊維質などの不純物を除去して得られるこんにゃく精粉が使用される。   Glucomannan, the main component of konjac mannan, has unique chemical and physical properties such as the formation of elastic irreversible elastic gels by adding alkali to the aqueous solution and heating it. It has been used as a raw material for konjac production. For the production of konjac, konjac fine powder obtained by slicing tubers of a plant of the taro family called konjac koji, drying, pulverizing, and removing impurities such as starch and fiber by wind sorting is used.

グルコマンナンには低濃度で高い増粘作用、ゲル化作用、結着作用などがあり、低カロリーの食物繊維として生理作用を有することから、こんにゃく以外の食品の品質を改良するために使用される。しかしながらこんにゃく精粉の平均粒子径は約300μm以上と大きく、かつ表面が硬いサックで覆われているため水に膨潤(溶解)するまでの時間が長く、常温で約3〜4時間以上を要する。このためこんにゃく精粉を微粒子化して比表面積を大きくすることによって水に対する膨潤(溶解)時間を短縮する試みがなされてきた。ところがこんにゃく精粉に代表されるグルコマンナン含量50%以上のコンニャクマンナンは10%程度の水分を含有し、ゴムのように弾力性に富むので単なる機械的粉砕によって微粉化するのは困難である。そのため液体窒素等で超低温へ冷却し脆くなった状態で粉砕する方法もあるが、工業的スケールでの生産には適さない。   Glucomannan has high thickening, gelling, binding, etc. at low concentrations, and has physiological effects as low-calorie dietary fiber, so it is used to improve the quality of foods other than konjac . However, the average particle diameter of konjac fine powder is as large as about 300 μm or more, and since the surface is covered with a hard sack, it takes a long time to swell (dissolve) in water, and requires about 3 to 4 hours or more at room temperature. For this reason, attempts have been made to shorten the swelling (dissolution) time with respect to water by making konjac fine powder fine particles to increase the specific surface area. However, konjac mannan having a glucomannan content of 50% or more, which is represented by konjac fine powder, contains about 10% of water and is elastic like rubber, so that it is difficult to pulverize by mere mechanical grinding. For this reason, there is a method of pulverizing in a state of being brittle after cooling to ultra-low temperature with liquid nitrogen or the like, but it is not suitable for production on an industrial scale.

他の方法として、本出願人の特公平6−97960号に開示された方法がある。この方法はこんにゃく精粉にその乾燥重量の3〜20倍の水を加えて膨潤させてゾルとなし、ゾルにエタノールを加えて生成したゲルを湿式粉砕後乾燥することよりなる。膨潤させてゾルにすることによりサックが破れ、エタノールで沈殿化させることにより粉砕が容易となる。   As another method, there is a method disclosed in Japanese Patent Publication No. 6-97960 of the present applicant. This method consists in adding 3 to 20 times the dry weight of water to a konjac flour to swell it to form a sol, and adding the ethanol to the sol to wet-grind and dry. The sack is broken by swelling to a sol, and pulverization is facilitated by precipitation with ethanol.

この方法により、平均粒子径約100μmまで微粉化でき、粘度がピークに達する水に対する膨潤(溶解)時間が約2時間程度まで短縮される。しかしながら水に対する膨潤(溶解)時間をさらに短縮し、例えば粘度ピーク時間を1時間以内、より好ましくは約30分間程度まで短縮できるようにさらに微粒子化することが望ましい。   By this method, it is possible to finely pulverize to an average particle size of about 100 μm, and the swelling (dissolution) time for water at which the viscosity reaches a peak is shortened to about 2 hours. However, it is desirable to further reduce the swelling (dissolution) time in water, for example, so that the viscosity peak time can be shortened to within 1 hour, more preferably to about 30 minutes.

こんにゃく精粉にはトリメチルアミンや亜硫酸塩などの多くの不純物が残留し、特異な刺激臭を有する。そのため微粒子化の過程でこれら不純物が除去されることが望ましい。   Many impurities such as trimethylamine and sulfite remain in the konjac fine powder and have a unique irritating odor. Therefore, it is desirable to remove these impurities in the process of making fine particles.

これらの要望は本発明によって満たされる。本発明は、グルコマンナン含量50%以上のコンニャクマンナン、典型的にはこんにゃく精粉を水で膨潤するのでなく、逆に原料に含まれる水分を脱水性のある有機溶媒に接触させることにより脱水し、弾力性をなくした状態で微粒子化することを原理とする。このためコンニャクマンナンを脱水性溶媒のスラリーの状態で高速攪拌機中において攪拌することによって微粒子化することが可能になる。   These needs are met by the present invention. The present invention does not swell the konjac mannan having a glucomannan content of 50% or more, typically konjac flour, with water, but conversely, the water contained in the raw material is brought into contact with a dehydrating organic solvent for dehydration. The principle is to make fine particles in a state where elasticity is lost. For this reason, konjac mannan can be made into fine particles by stirring in a high-speed stirrer in the form of a slurry of a dehydrating solvent.

従って本発明は、グルコマンナン含量50%以上のコンニャクマンナンを50%以上95%以下の含水エタノールに分散したスラリーの状態で高速回転する攪拌翼を備える攪拌機中で平均粒子径が50μm以下になるまで攪拌し、固液分離後乾燥することを特徴とする易溶性コンニャクマンナンの製造方法を提供する。   Therefore, in the present invention, the average particle size is reduced to 50 μm or less in a stirrer equipped with a stirring blade rotating at high speed in a slurry state in which konjac mannan having a glucomannan content of 50% or more is dispersed in water-containing ethanol having a content of 50% or more and 95% or less. Provided is a method for producing a readily soluble konjac mannan characterized by stirring and drying after solid-liquid separation.

好ましくは、含水エタノールによる脱水処理は繰り返して実施することができる。このため原料コンニャクマンナンを前記含水エタノールに分散し、ゆっくり攪拌した後固液分離した後、再度含水エタノールに分散してスラリーとし、高速攪拌機中で攪拌して微粒子化する。   Preferably, the dehydration treatment with hydrous ethanol can be performed repeatedly. For this reason, the raw material konjac mannan is dispersed in the water-containing ethanol, slowly stirred and then solid-liquid separated, and then dispersed again in water-containing ethanol to form a slurry, which is stirred in a high-speed stirrer to form fine particles.

含水エタノールとの接触の繰り返しにより脱水の程度が均一に高まり、微粒子化が容易になる。   Repeated contact with hydrous ethanol increases the degree of dehydration uniformly and facilitates the formation of fine particles.

本発明では分散媒であるエタノールを固液分離して回収するので、刺激臭のある不純物が含水エタノールに溶出され、一般食品に使用することが可能になる。また回収した含水エタノールは再蒸留して再使用することができる。   In the present invention, ethanol, which is a dispersion medium, is recovered by solid-liquid separation, so that impurities with an irritating odor are eluted in hydrous ethanol and can be used for general foods. The recovered water-containing ethanol can be reused by re-distilling.

コンニャクマンナン粒子は水で膨潤し、逐にはサックが破れてゾルすなわちコロイド溶液を形成する。しかしながら無水アルコールには全く膨潤しないし、含水エタノールにもエタノール分が高くなると膨潤しない。むしろコンニャクマンナンに含まれている水分がエタノール側に拡散し、脱水される。脱水性能を有する溶媒は他にもヘキサン、アセトンなどがあるが、食品用途に対しては50%以上95%以下、好ましくは70%以上95%以下の含水エタノールが適している。   The konjac mannan particles swell with water, and the sac is broken and forms a sol or colloidal solution. However, it does not swell at all in absolute alcohol, and does not swell in ethanol containing water as the ethanol content increases. Rather, water contained in konjac mannan diffuses to the ethanol side and is dehydrated. Other solvents having dehydration performance include hexane and acetone, but water-containing ethanol of 50% to 95%, preferably 70% to 95% is suitable for food applications.

脱水の程度はコンニャクマンナンに対する含水エタノールの量比および接触時間による。50%以上の含水エタノールの場合、コンニャクマンナンと含水エタノールの比(wt/vol)が少なくとも1:5、好ましくは1:10であり、含水エタノールとの接触時間は合計して30分以上で充分である。この接触時間には含水エタノール中の前処理および攪拌機中の高速攪拌時間が含まれる。従って異なるまたは同じ攪拌機を使用し、原料コンニャクマンナンを最初は含水エタノール中でゆっくり攪拌しながら接触させ、固液分離後ケーキを再び含水エタノールに分散し、高速攪拌しても良く、または最初の含水エタノールとの接触を省き、高速攪拌と同時に必要な接触時間を確保しても良い。微粒子化を伴なわないコンニャクマンナンと含水エタノールとの接触、次いで固液分離したケーキを含水エタノールに再分散し、微粒子化を伴う高速攪拌にかけるのが好ましい。均一な脱水と、不純物の溶出除去が同時に達成される。   The degree of dehydration depends on the ratio of water-containing ethanol to konjac mannan and the contact time. In the case of 50% or more hydrous ethanol, the ratio of konjac mannan to hydrous ethanol (wt / vol) is at least 1: 5, preferably 1:10, and the total contact time with hydrous ethanol is 30 minutes or more. It is. This contact time includes pretreatment in water-containing ethanol and high-speed stirring time in a stirrer. Therefore, using a different or the same stirrer, the raw material konjac mannan is first brought into contact with water-containing ethanol while stirring slowly, and after solid-liquid separation, the cake may be dispersed again in water-containing ethanol and stirred at high speed, or the first water-containing Contact with ethanol may be omitted, and necessary contact time may be secured simultaneously with high-speed stirring. It is preferable to contact konjac mannan without pulverization and hydrous ethanol, then re-disperse the solid-liquid separated cake in hydrous ethanol and subject to high-speed stirring accompanied by pulverization. Uniform dehydration and elution removal of impurities are achieved at the same time.

微粒子化を伴う高速攪拌は高速回転する攪拌翼を備える攪拌機を使用して実施される。このタイプの攪拌機は、本来固体と液体、または互いに混じり合わない液体同士を混合するための装置である。機内の液流の方向により放射流型と軸流型に分類され、そのいずれでも良いが、剪断力により微粒子化を行うので、攪拌翼の回転数は5,000RPM以上である必要がある。具体的な回転数は採用する特定の攪拌機によって変動するが、例えば実施例で使用した特殊機化(株)製のHOMOMIXER MARK IIの場合、10,000RPMで行った。   High-speed agitation accompanied by atomization is performed using a stirrer equipped with a stirring blade that rotates at high speed. This type of stirrer is an apparatus for mixing solids and liquids or liquids that do not mix with each other. Depending on the direction of the liquid flow in the machine, it may be classified into a radial flow type and an axial flow type, and either of them may be used. The specific number of rotations varies depending on the particular stirrer employed. For example, in the case of HOMOMIXER MARK II manufactured by Tokushu Kika Co., Ltd. used in the examples, it was performed at 10,000 RPM.

高速攪拌の継続時間は、微粒化されたコンニャクマンナンの乾燥後の平均粒子径が50μm以下、好ましくは30μm以下に達するのに十分でなければならない。具体的な攪拌時間は含水エタノールによる予備処理の有無、使用する機種、回転数などによって変動するが、一般に20分で十分であろう。   The duration of the high-speed stirring should be sufficient for the atomized konjac mannan to reach an average particle size after drying of 50 μm or less, preferably 30 μm or less. The specific stirring time varies depending on the presence / absence of pretreatment with water-containing ethanol, the model to be used, the rotational speed, etc., but generally 20 minutes will be sufficient.

高速攪拌による微粒子化の後、スラリーを濾過して固液分離し、ウエットケーキを100℃以下の温度で乾燥し、粉砕する。得られる微粒子化コンニャクマンナンは従来の易溶性グルコマンナンよりも平均粒子径において半分以下であり、粘度ピーク到達時間において約1/4に短縮され、約15分で粘度ピークの約95%が発現される。   After micronization by high-speed stirring, the slurry is filtered for solid-liquid separation, and the wet cake is dried at a temperature of 100 ° C. or less and pulverized. The resulting finely divided konjac mannan is less than half the average particle size compared to conventional readily soluble glucomannan, shortened to about 1/4 in the time to reach the viscosity peak, and about 95% of the viscosity peak is expressed in about 15 minutes. The

以下の実施例において、重量部および容量部は、g:mlの関係にある。   In the following examples, parts by weight and parts by volume are in a relationship of g: ml.

実施例1
グルコマンナン含量75%のコンニャクマンナン(こんにゃく精粉)10重量部を95%含水エタノール100容量部に加え、均一に分散するようにゆっくり30分間攪拌した。その後分散液を一旦濾過し、濾過ケーキを80%含水エタノール100容量部に再分散し、分散液を特殊機化(株)製T.K.HOMOMIXER MARK II中で回転速度10,000RPMにて20分間攪拌した。
Example 1
10 parts by weight of konjac mannan (konjac fine powder) having a glucomannan content of 75% was added to 100 parts by volume of 95% water-containing ethanol, and slowly stirred for 30 minutes so as to be uniformly dispersed. Thereafter, the dispersion was once filtered, and the filter cake was redispersed in 100 parts by volume of 80% water-containing ethanol. K. The mixture was stirred for 20 minutes in a HOMOMIXER MARK II at a rotation speed of 10,000 RPM.

攪拌終了後分散液を濾過して固液分離し、ケーキを90℃で24時間乾燥し、粉砕した。   After the stirring, the dispersion was filtered to separate into solid and liquid, and the cake was dried at 90 ° C. for 24 hours and pulverized.

実施例2
グルコマンナン含量80%のコンニャクマンナン(こんにゃく精粉)10重量部を70%含水エタノール100容量部に加え、均一に分散するようにゆっくり約60分間攪拌した。その後分散液を一旦濾過し、濾過ケーキを80%含水エタノール100容量部に再分散し、実施例1で使用した高速攪拌機を使用して回転速度10,000RPMにて20分間攪拌した。その後分散液を濾過して固液分離し、ケーキを90℃で24時間攪拌、粉砕した。
Example 2
10 parts by weight of konjac mannan (konjac fine powder) having a glucomannan content of 80% was added to 100 parts by volume of 70% hydrous ethanol, and the mixture was slowly stirred for about 60 minutes so as to disperse uniformly. Thereafter, the dispersion was filtered once, and the filter cake was redispersed in 100 parts by volume of 80% water-containing ethanol, and stirred at a rotational speed of 10,000 RPM for 20 minutes using the high-speed stirrer used in Example 1. Thereafter, the dispersion was filtered for solid-liquid separation, and the cake was stirred and pulverized at 90 ° C. for 24 hours.

1.微粒子化コンニャクマンナンの粒度分布
実施例1および実施例において製造した微粒子化コンニャクマンナンの粒度分布を、(株)島津製作所製レーザ回折式粒度分布測定装置、モデルSALD−3000Sにより測定した。比較のため、使用した原料コンニャクマンナン(こんにゃく精粉)、および従来の易溶性グルコマンナン(清水化学(株)レオレックスRS)の粒度分布も同様に測定した。
1. Particle size distribution of micronized konjac mannan The particle size distribution of micronized konjac mannan produced in Example 1 and Examples was measured by a laser diffraction particle size distribution measuring apparatus, model SALD-3000S, manufactured by Shimadzu Corporation. For comparison, the particle size distributions of the raw material konjac mannan (konnyaku fine powder) used and the conventional readily soluble glucomannan (Shimizu Chemical Co., Ltd., ROLEX RS) were also measured.

図1は、実施例1で製造した微粒子化コンニャクマンナンの粒度分布曲線であり、図2は実施例2で製造した微粒子化コンニャクマンナンの粒度分布曲線である。図1および図2のグラフは原料コンニャクマンナンの平均径は323μmおよび315μmであり、従来の易溶性グルコマンナンの平均粒子径は91μmであるのに対し、本発明方法によって製造したグルコマンナンの平均粒子径は26μmであることを示している。   FIG. 1 is a particle size distribution curve of the finely divided konjac mannan produced in Example 1, and FIG. 2 is a particle size distribution curve of the finely divided konjac mannan produced in Example 2. The graphs of FIGS. 1 and 2 show that the average diameter of the raw material konjac mannan is 323 μm and 315 μm, and the average particle diameter of the conventional readily soluble glucomannan is 91 μm, whereas the average particle of glucomannan produced by the method of the present invention The diameter is 26 μm.

2.微粒子化コンニャクマンナンの溶解性
代表として実施例1で製造した微粒子化コンニャクマンナンを選び、その1%水溶液の粘度の経時的変化を25℃±1℃においてB形粘度計を用いて測定した。比較のため原料こんにゃく精粉、従来の易溶性グルコマンナン(清水化学(株)製レオレックスRS)、および高純度グルコマンナン(清水化学(株)製プロポールA)の粘度の経時的変化を同じ条件で測定した。結果を図3のグラフに示す。
2. Solubility of micronized konjac mannan As a representative, micronized konjac mannan produced in Example 1 was selected, and the change over time in the viscosity of a 1% aqueous solution was measured at 25 ° C. ± 1 ° C. using a B-type viscometer. For comparison, the same time-dependent changes in the viscosity of raw material konjac fine powder, conventional readily soluble glucomannan (Rolex RS manufactured by Shimizu Chemical Co., Ltd.), and high purity glucomannan (Propol A manufactured by Shimizu Chemical Co., Ltd.) are the same. Measured under conditions. The results are shown in the graph of FIG.

本発明方法によって製造した速溶性コンニャクマンナンは、約30分で約35,000mPa・sのピーク粘度に達し、約15分で粘度ピーク時の約95%の粘度を発現した。これに対し、従来の易溶性グルコマンナンではピーク粘度約35,000Pa・sに達するまでに約2時間を要し、15分では粘度ピーク時の約50%粘度しか発現しない。勿論約30分の短い粘度ピーク時間は、原料こんにゃく精粉および高純度グルコマンナンでは得られない。   The fast-dissolving konjac mannan produced by the method of the present invention reached a peak viscosity of about 35,000 mPa · s in about 30 minutes, and developed a viscosity of about 95% at the viscosity peak in about 15 minutes. On the other hand, in the conventional easily soluble glucomannan, it takes about 2 hours to reach the peak viscosity of about 35,000 Pa · s, and in about 15 minutes, only about 50% viscosity at the viscosity peak is developed. Of course, a short viscosity peak time of about 30 minutes cannot be obtained with raw material konjac refined powder and high-purity glucomannan.

実施例1で製造した微粒子化コンニャクマンナンの粒度分布曲線のグラフ。2 is a graph of a particle size distribution curve of finely divided konjac mannan produced in Example 1. FIG. 実施例で製造した微粒子化コンニャクマンナンの粒度分布曲線グラフ。The particle size distribution curve graph of micronized konjac mannan manufactured in the Example. 本発明方法によって製造した微粒子化コンニャクマンナンの経時的粘度変化のグラフ。The graph of the viscosity change with time of micronized konjac mannan produced by the method of the present invention.

Claims (2)

グルコマンナン含量50%以上のコンニャクマンナンを、70%以上95%以下の含水エタノールに、少なくとも1:5のコンニャクマンナン対含水エタノールの比(wt/vol)において分散し、スラリーの状態で高速回転する攪拌翼を備える攪拌機で平均粒子径が50μm以下になるまで攪拌し、この時攪拌時間を含めコンニャクマンナンを含水エタノールと少なくとも30分以上接触させ、固液分離後乾燥することを特徴とする速溶性コンニャクマンナンの製造方法。 Konjac mannan having a glucomannan content of 50% or more is dispersed in hydrous ethanol having a content of 70% or more and 95% or less at a ratio of konjac mannan to hydrous ethanol of at least 1: 5 (wt / vol), and is rotated at high speed in a slurry state. Stirring with a stirrer equipped with a stirring blade until the average particle size is 50 μm or less, including at this time the konjac mannan is brought into contact with water-containing ethanol for at least 30 minutes, solid-liquid separation and then drying. Manufacturing method of konjac mannan. 含水エタノール中のスラリーの状態でコンニャクマンナンを前記攪拌機中で攪拌する前に、コンニャクマンナンを70%以上95%以下の含水エタノールに少なくとも1:5のコンニャクマンナン対含水エタノールの比(wt/vol)において分散した状態に保ち、固液分離する前処理ステップを含み、その際前処理ステップと前記攪拌機中の攪拌ステップにおけるコンニャクマンナンと含水エタノールとの合計接触時間を少なくとも30分以上に保つ請求項1の方法。
Before stirring the konjac mannan in the slurry in the water-containing ethanol in the stirrer, the ratio of the konjac mannan to the water-containing ethanol of 70% to 95% water-containing ethanol at least 1: 5 (wt / vol) 2. A pretreatment step for maintaining a dispersed state in which the solid-liquid separation is performed, wherein the total contact time of konjac mannan and hydrous ethanol in the pretreatment step and the stirring step in the stirrer is kept at least 30 minutes or more. the method of.
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Publication number Priority date Publication date Assignee Title
EP2826464A1 (en) 2013-07-19 2015-01-21 Shimizu Chemical Corporation Sustained release solid dosage preparations
US9114091B2 (en) 2013-07-05 2015-08-25 Shimizu Chemical Corporation Sustained release solid dosage preparations

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JP5903250B2 (en) * 2011-11-16 2016-04-13 清水化学株式会社 Sustained release composition
CN111518854A (en) * 2020-04-01 2020-08-11 陕西理工大学 Multi-enzyme zymolyte of konjac fine powder and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9114091B2 (en) 2013-07-05 2015-08-25 Shimizu Chemical Corporation Sustained release solid dosage preparations
EP2826464A1 (en) 2013-07-19 2015-01-21 Shimizu Chemical Corporation Sustained release solid dosage preparations

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