JP5044901B2 - Method for producing water-soluble polysaccharide - Google Patents
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本発明は植物素材から、食品工業で有用な水溶性の多糖類を製造する方法に関するものである。詳しくは植物素材の懸濁液を高温・高圧の水蒸気を導入するという加熱をすることにより水溶性の多糖類を抽出・製造する方法に関し、さらには酸性蛋白の安定化機能等食品分野での機能性に優れた有用な水溶性多糖類を効率的に抽出する方法に関する。 The present invention relates to a method for producing water-soluble polysaccharides useful in the food industry from plant materials. Specifically, it relates to a method for extracting and producing water-soluble polysaccharides by heating a suspension of plant material by introducing high-temperature and high-pressure steam, and further functions in the food field such as the stabilization function of acidic proteins. The present invention relates to a method for efficiently extracting a useful water-soluble polysaccharide having excellent properties.
植物由来の水溶性多糖類は食物繊維として利用されているのを始め、食品工業においての機能剤として幅広く利用されている。これら多糖類の植物性繊維質原料として、果実類、穀類、イモ類、豆類、油糧種子植物等が知られている。 Plant-derived water-soluble polysaccharides are widely used as functional agents in the food industry, including those used as dietary fiber. Fruits, cereals, potatoes, beans, oilseed plants and the like are known as plant fiber raw materials for these polysaccharides.
植物性原料から水溶性多糖類を抽出、製造する技術として従来より、原料に加水しこれを酸性、または中性、或いはアルカリ性において加熱する方法が知られている。例えば、タンパク質の等電点付近のpHで130℃以下の条件で、水溶性多糖類を抽出する方法がある(特許文献1)が、この方法では抽出時間が通常60分以上の長時間を要し、さらに短時間で効率的な抽出法が望まれている。 As a technique for extracting and producing a water-soluble polysaccharide from a plant raw material, a method of adding water to the raw material and heating it in an acidic, neutral, or alkaline manner has been known. For example, there is a method of extracting water-soluble polysaccharides at a pH of about 130 ° C. or less at a pH near the isoelectric point of protein (Patent Document 1), but this method usually requires a long time of 60 minutes or more. In addition, an efficient extraction method is desired in a shorter time.
また、穀類や豆類の外皮を130℃から160℃に加熱し、水溶性のヘミセルロースを得る方法(特許文献2)も知られているが、この方法では、温度を上げていって歩留を上げようとすると、着色や低分子化が進んでくるため問題がある。 Also known is a method for obtaining water-soluble hemicellulose by heating the cereal and bean hulls from 130 ° C. to 160 ° C. In this method, the temperature is raised to increase the yield. If it tries to do so, there is a problem because coloring and low molecular weight progress.
また抽出剤として、ヘキサメタリン酸を使用して80℃以上で、水溶性多糖類を抽出する方法(特許文献3)、が開示されているが、このような抽出剤を使用すること自体食品への利用には問題がある。 Moreover, although the method (patent document 3) which extracts a water-soluble polysaccharide at 80 degreeC or more using hexametaphosphoric acid as an extractant is disclosed, using such an extractant itself to foodstuffs is disclosed. There is a problem in use.
さらに、高温・高圧水に接触させることにより短時間で抽出を行う方法(特許文献4,5)も知られているが、非常に高圧のため、設備が大掛かりになることと、所望の品質や機能を有する多糖類を得るためには抽出条件の制御が困難となるという問題がある。 Furthermore, a method of performing extraction in a short time by contacting with high temperature / high pressure water (Patent Documents 4 and 5) is also known. However, because the pressure is very high, the equipment becomes large and the desired quality and In order to obtain a polysaccharide having a function, there is a problem that it is difficult to control extraction conditions.
本発明は、植物繊維質原料から、簡便な方法で、短時間で効率よく、分解反応が過剰に進むことなく、食品工業で有用な機能を有する品質の良い、水溶性多糖類を製造する方法を提供することである。なお食品工業で有用な機能の主な例としては、酸性蛋白食品の安定化機能が上げられる。 The present invention is a method for producing a high-quality, water-soluble polysaccharide having a useful function in the food industry from a plant fiber raw material by a simple method, efficiently in a short time, and without causing excessive decomposition reaction. Is to provide. A main example of a function useful in the food industry is a function for stabilizing acidic protein foods.
本発明者らは、如上の点に鑑み鋭意研究した結果、植物繊維質原料を含む懸濁液に高温・高圧の水蒸気を吹き込み加熱することにより、水溶性多糖類の抽出を容易ならしめる、という知見を得、本発明を完成するに至った。これは蒸気の導入時の物理的なシェアにより、植物繊維質原料の細胞壁を効率的に破壊され、水溶性多糖類の抽出を容易ならしめる、という効果を生じていると考えられる。また、水蒸気導入による加熱を複数回行うこと、及び加熱の後にこの原料懸濁液を瞬間的に減圧して冷却する操作を行うことにより爆砕効果が得られ、さらに効率的な水溶性多糖類の抽出が行えるという知見を得、発明を発展させることが出来た。なお減圧の操作は通常大気圧まで開放する方法が用いられる。 As a result of intensive studies in view of the above points, the present inventors have made it easy to extract water-soluble polysaccharides by blowing high-temperature and high-pressure steam into a suspension containing plant fiber raw material and heating it. Knowledge has been obtained and the present invention has been completed. This is thought to be due to the fact that the cell wall of the plant fiber raw material is efficiently destroyed and the extraction of water-soluble polysaccharides is facilitated by the physical share at the time of introduction of steam. Further, by performing heating by introducing water vapor a plurality of times, and performing an operation of instantaneously reducing the pressure of the raw material suspension and cooling after the heating, a blasting effect can be obtained, and more efficient water-soluble polysaccharides can be obtained. The knowledge that extraction can be performed was acquired, and the invention was able to be developed. In general, a method of releasing the pressure up to atmospheric pressure is used for the decompression operation.
すなわち本発明は、植物繊維質原料の懸濁液に高温・高圧の水蒸気を導入して加熱する工程を含むことを特徴とする水溶性多糖類の製造方法である。また高温・高圧の水蒸気を導入するという加熱を複数回行う水溶性多糖類の製造方法であり、本発明はまた、植物繊維質原料として大豆を用いる水溶性多糖類の製造方法である。 That is, the present invention is a method for producing a water-soluble polysaccharide, comprising a step of introducing high-temperature and high-pressure steam into a suspension of plant fiber raw material and heating it. The present invention also relates to a method for producing a water-soluble polysaccharide in which high-temperature and high-pressure steam is introduced several times, and the present invention is also a method for producing a water-soluble polysaccharide using soybean as a plant fiber raw material.
本発明はさらに植物繊維質原料の加熱時のpHを3〜7とし、かつ加熱温度を140℃以上とする上記記載の水溶性多糖類の製造方法であり、導入する水蒸気の圧力が6Kg/cm2以上である、水溶性多糖類の製造方法である。 The present invention further relates to the method for producing a water-soluble polysaccharide as described above, wherein the plant fiber raw material has a pH of 3 to 7 and a heating temperature of 140 ° C. or higher. The water vapor pressure to be introduced is 6 kg / cm 2. This is the method for producing a water-soluble polysaccharide as described above.
さらに本発明は植物繊維質原料を複数回の加熱を行う際に、複数回の加熱の合計加熱時間が30分以内で行う水溶性多糖類の製造方法であり、複数回の加熱におけるいずれかの加熱の後に瞬間的に該原料懸濁液を減圧する工程を経ることを特徴とする水溶性多糖類の製造方法である。 Furthermore, the present invention is a method for producing a water-soluble polysaccharide in which a total heating time of a plurality of heatings is performed within 30 minutes when the plant fiber raw material is heated a plurality of times. It is a method for producing a water-soluble polysaccharide characterized by passing through a step of depressurizing the raw material suspension instantaneously after heating.
本発明により、簡便な方法で、短時間で、酸性下での乳蛋白安定能等、高機能を持つ水溶性大豆ヘミセルロースを効率よく製造することが可能となる。 According to the present invention, it is possible to efficiently produce water-soluble soybean hemicellulose having high functions such as stability of milk protein under acidic conditions in a short time by a simple method.
以下に本発明について詳細に説明する。 The present invention is described in detail below.
本発明において、原料として使用される植物素材は、りんごや柑橘類の果実皮、穀類や芋類、豆類、さらに菜種、パーム等油糧種子の搾油粕等も用いられる。中でも大豆原料で、特に大豆の子葉部分が好適であり、これを多く含む脱脂大豆やおからが特に適している。 In the present invention, plant materials used as raw materials include apples and citrus fruit peels, cereals and strawberries, beans, and oilseed sesame seeds such as rapeseed and palm. Of these, soybean raw materials, particularly the cotyledon portion of soybeans, are particularly suitable, and defatted soybeans and okara containing a large amount thereof are particularly suitable.
本発明では原料の懸濁液を加熱するため高圧の水蒸気を導入する。水蒸気導入の方法は特に限定されないが、加熱は出来るだけ短時間で効率的に行うことが望ましく、蒸気インジェクターを使用して原料の懸濁液に、高圧の水蒸気を連続的に吹き込んで加熱する方法が、目的温度まで瞬時に昇温できるので好ましい方式である。 In the present invention, high-pressure steam is introduced to heat the raw material suspension. The method for introducing water vapor is not particularly limited, but it is desirable that heating be performed efficiently in as short a time as possible. A method in which high-pressure water vapor is continuously blown into a raw material suspension using a steam injector and heated. However, this is a preferable method because the temperature can be instantaneously increased to the target temperature.
本発明では加熱の条件として、原料の植物材料を含む懸濁液に、高圧の水蒸気を吹き込み140℃以上で加熱する。この加熱操作は複数回行うことがより好ましい。本発明の場合、静置状態の反応容器を加熱していく方法に比べ、高圧の水蒸気を原料懸濁液に吹き込むので、急激なシェア(攪拌)がかかる。この現象により、植物細胞壁成分の物理的破壊が起こり、水溶性多糖類が溶出しやすくなり、抽出効果を高めることができる。従って、加熱を複数回行うことは抽出をより効率的に行う効果が期待できる。高圧の水蒸気について言えば、高温を得ることと、物理的なシェアの効果から水蒸気の圧力としてゲージ圧で6kg/cm2以上のものを用いるのが良い。圧力が低すぎると高温が得られないし、蒸気導入時のシェアが弱くなる。またあまりな高圧は装置的なコストが大きくなるし、抽出の制御も難しくなる。 In the present invention, as a heating condition, high-pressure steam is blown into a suspension containing a raw material plant material and heated at 140 ° C. or higher. It is more preferable to perform this heating operation a plurality of times. In the case of this invention, compared with the method of heating the reaction container in a stationary state, since high-pressure steam is blown into the raw material suspension, a rapid share (stirring) is applied. By this phenomenon, the physical destruction of the plant cell wall component occurs, the water-soluble polysaccharide is easily eluted, and the extraction effect can be enhanced. Therefore, the effect of performing extraction more efficiently can be expected by performing heating a plurality of times. Speaking of high-pressure water vapor, it is preferable to use a water vapor pressure of 6 kg / cm 2 or more as a water vapor pressure from the viewpoint of obtaining a high temperature and a physical share. If the pressure is too low, a high temperature cannot be obtained, and the share at the time of introducing the steam becomes weak. An excessively high pressure increases the cost of the apparatus and makes it difficult to control the extraction.
加熱後は冷却を行うが、この冷却方法については、本発明においては少なくとも一度は加熱後、瞬間的な減圧、特に瞬間的に大気圧まで減圧して冷却することが好ましい。本発明の140℃以上の加熱では、抽出装置内の圧力は、ほぼその温度における飽和蒸気圧程度の圧力になっており、この圧力から瞬間的な減圧、(通常大気圧まで減圧)することで爆砕効果による、植物細胞壁成分の物理的破壊が起こり、水溶性多糖類の抽出効果をより高めることができる。このように、大気圧まで減圧して冷却する操作は瞬間的に行うが、この瞬間的とは通常1秒もかからない程度である。本発明のような加熱操作を行えば背圧弁を通過した瞬間に圧力が開放され、大気圧まで減圧されるので1秒を超えるような時間にはならない。一方、一般的なプレートによる冷却では急激な圧力降下は起こらず、爆砕効果による水溶性多糖類の抽出効率を上げることはできない。 Although cooling is performed after heating, in the present invention, it is preferable to cool at an instantaneous pressure reduction, particularly instantaneously reduced to atmospheric pressure after heating at least once in the present invention. In the heating at 140 ° C. or higher according to the present invention, the pressure in the extraction device is about the saturated vapor pressure at that temperature, and instantaneous pressure reduction (normally pressure reduction to atmospheric pressure) is performed from this pressure. Physical destruction of plant cell wall components occurs due to the blasting effect, and the extraction effect of the water-soluble polysaccharide can be further enhanced. As described above, the operation of reducing the pressure to the atmospheric pressure and cooling it is performed instantaneously, but this momentary time is usually about 1 second. If the heating operation as in the present invention is performed, the pressure is released at the moment of passing through the back pressure valve, and the pressure is reduced to atmospheric pressure, so that it does not take more than 1 second. On the other hand, cooling with a general plate does not cause a rapid pressure drop, and the extraction efficiency of water-soluble polysaccharides due to the blasting effect cannot be increased.
このように、本発明では、水溶性多糖類をより効果的に抽出するために、加熱は複数回することがより有効であり、また、加熱後の冷却方法として、瞬間的に大気圧まで減圧する方法が特に有効である。この加熱と冷却の方法については、1回加熱する毎に冷却し、これを複数回行う方法、充分な冷却を経ずに複数回の加熱を行った上冷却し、再度加熱後冷却する方法、複数回加熱後、最後に冷却する方法がある。このように、加熱時の冷却のタイミングについては制限されないが、加熱後の少なくとも1回、瞬間的に大気圧まで減圧して冷却操作を行うことで大きな効果が得られる。また、複数回の加熱における加熱温度は同じ温度であってもよいし、段階的に温度を変えてもよい。上述の方法は、どれも水溶性多糖類の抽出効率を高めることができる手段であるが、中でも、1回加熱する毎に、瞬間的に大気圧まで減圧して冷却し、これを複数回行う方法が最も有効な手段である。 As described above, in the present invention, in order to extract the water-soluble polysaccharide more effectively, it is more effective to perform the heating a plurality of times, and as a cooling method after heating, the pressure is instantaneously reduced to atmospheric pressure. This method is particularly effective. About this heating and cooling method, it is cooled every time it is heated, a method of performing this a plurality of times, a method of cooling after performing a plurality of times of heating without sufficient cooling, a method of cooling after heating again, There is a method of cooling at the end after heating a plurality of times. Thus, although the timing of cooling at the time of heating is not limited, a great effect can be obtained by performing a cooling operation by instantaneously reducing the pressure to atmospheric pressure at least once after heating. Moreover, the same temperature may be sufficient as the heating temperature in several times of heating, and you may change temperature in steps. Any of the above-mentioned methods is a means that can increase the extraction efficiency of the water-soluble polysaccharide, but among them, every time heating is performed, the pressure is instantaneously reduced to atmospheric pressure, and this is performed a plurality of times. The method is the most effective means.
加熱の温度は140℃以上で行われるが、好ましくは150℃以上、より好ましくは160℃以上で行うのが良い。加熱温度が140℃未満だと、抽出効果が低下し、短時間で目的の水溶性多糖類を効率的に抽出することはできない。また、加熱時の上限温度については特に限定されないが、加熱温度を上げていくと、分解反応が進みやすく、過剰な分解を抑制し、目的とする機能を有する多糖類を得る為には反応時間制御が厳しくなる。加熱温度が190℃を超えると水溶性多糖類の分解が進みすぎることがあり、これ以上の温度での加熱は好ましくない。 The heating temperature is 140 ° C. or higher, preferably 150 ° C. or higher, more preferably 160 ° C. or higher. When the heating temperature is less than 140 ° C., the extraction effect is reduced, and the target water-soluble polysaccharide cannot be efficiently extracted in a short time. Further, the upper limit temperature during heating is not particularly limited, but as the heating temperature is raised, the decomposition reaction tends to proceed, the reaction time is reduced in order to suppress excessive decomposition and obtain a polysaccharide having the desired function. Control becomes stricter. When the heating temperature exceeds 190 ° C., decomposition of the water-soluble polysaccharide may proceed excessively, and heating at a temperature higher than this is not preferable.
加熱回数については特に限定しないが、通常3〜4回までで十分である。これ以上加熱回数を増やしても工程を増やすだけで、水溶性多糖類の抽出率を高める効果は低い。 Although it does not specifically limit about the frequency | count of a heating, Usually, 3 to 4 times is enough. Even if the number of heating is further increased, the effect of increasing the extraction rate of the water-soluble polysaccharide is low only by increasing the number of steps.
大気圧まで瞬間的に減圧して冷却する回数の上限については特に限定しないが、通常2〜3回までで十分である。 The upper limit of the number of times of instantaneous pressure reduction to atmospheric pressure and cooling is not particularly limited, but usually 2 to 3 times is sufficient.
抽出時のpHは3〜7で行われる。好ましくは4〜6である。抽出時のpHが3未満になると、酸による加水分解を受け易く、抽出される多糖類が低分子化して、高機能を有する水溶性多糖類を得ることが難しくなる。また、pHが7を超えると、原料素材に蛋白質が共存している場合、この蛋白質が分解して水溶性多糖類と一緒に溶出してしまい、多糖類純度が低下し、多糖類の溶液が白濁したり、分解されて生じた糖とアミノ酸とが反応して黒褐色に褐変してしまい品質が悪くなりがちである。 The pH at the time of extraction is 3-7. Preferably it is 4-6. When the pH at the time of extraction is less than 3, it is susceptible to hydrolysis by an acid, and the extracted polysaccharide is reduced in molecular weight, making it difficult to obtain a water-soluble polysaccharide having a high function. On the other hand, when the pH exceeds 7, when the protein coexists in the raw material, the protein is decomposed and eluted together with the water-soluble polysaccharide, the purity of the polysaccharide is lowered, and the polysaccharide solution is reduced. The sugar tends to become cloudy or decomposed, and the amino acid reacts to turn brownish brown and tends to deteriorate the quality.
加熱時間の合計は、30分以内で充分であるが、工業的に効率的な生産を行うためには20分以内、より好ましくは10分以内で行うと良い。時間が長くなれば、分解率が高くなり水溶性多糖類の抽出効率は向上するが、低分子化が進み、機能が低下するので好ましくない。当反応では、最低時間については特に限定しないが、水溶性多糖類の抽出量を充分得るためには、通常1分程度は必要である。 The total heating time is sufficient within 30 minutes. However, in order to carry out industrially efficient production, it is preferably within 20 minutes, more preferably within 10 minutes. If the time is longer, the decomposition rate becomes higher and the extraction efficiency of the water-soluble polysaccharide is improved, but it is not preferable because the molecular weight is lowered and the function is lowered. In this reaction, the minimum time is not particularly limited, but usually about 1 minute is necessary to obtain a sufficient amount of water-soluble polysaccharide extract.
水溶性多糖類の分子量については、どのような分子量であっても、ある程度の機能は得られるが、分子量が大き過ぎると粘度が高くなり、取り扱いが困難になるという欠点が出てくる。また分子量が小さ過ぎると、安定化機能が弱くなってしまう。分子量としては通常数千〜数百万のものが適切であり、好ましくは1万〜100万の範囲である。 With regard to the molecular weight of the water-soluble polysaccharide, a certain degree of function can be obtained regardless of the molecular weight, but if the molecular weight is too large, the viscosity becomes high and handling becomes difficult. On the other hand, if the molecular weight is too small, the stabilizing function is weakened. The molecular weight is usually from several thousand to several million, and preferably in the range from 10,000 to 1,000,000.
以下、実施例により本発明の実施態様を説明するが、これは例示であって本願発明の精神がこれらの例示によって制限されるものではない。なお、例中、部および%は何れも重量基準を意味する。 Hereinafter, the embodiments of the present invention will be described by way of examples. However, these are merely examples, and the spirit of the present invention is not limited by these examples. In the examples, both parts and% mean weight basis.
図1に示す反応装置において、原料タンク1中に、脱脂された乾燥おから1部に水14部を加え、塩酸でpHを5.0に調整した。このおからの懸濁液をポンプ7で、ホールディング管へ送液し、蒸気インジェクター11を使用して、圧力が7Kg/cm2の水蒸気を導入し、155℃まで瞬間的に加熱し、2.5分間ホールド後、再び蒸気インジェクター12を使用して、圧力が7Kg/cm2の水蒸気を導入し、165℃まで瞬間的に加熱し、2.5分間ホールド後冷却装置6で100℃以下に冷却し、反応液受入器5にスラリーを受入れた。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。 In the reaction apparatus shown in FIG. 1, 14 parts of water was added to 1 part of degreased dried okara in the raw material tank 1, and the pH was adjusted to 5.0 with hydrochloric acid. The suspension from this okara is sent to the holding tube by the pump 7, steam using the steam injector 11 is introduced into the steam, the pressure is 7 kg / cm 2, and the water is heated instantaneously to 155 ° C., 2.5 After holding for a minute, the steam injector 12 is used again to introduce water vapor with a pressure of 7 Kg / cm 2, and the water is instantaneously heated to 165 ° C., held for 2.5 minutes and then cooled to 100 ° C. or lower with the cooling device 6, The slurry was received in the reaction solution receiver 5. The obtained slurry was separated by centrifugation, the supernatant was subjected to ethanol precipitation, and the precipitate was dried to obtain a water-soluble polysaccharide.
図1に示す反応装置において原料タンク1中に、脱脂された乾燥おから1部に水14部を加え、塩酸でpHを5.0に調整した。このおからの懸濁液をポンプ7でホールディング管に送液し、蒸気インジェクター11を使用して、圧力が7Kg/cm2の水蒸気を導入し、155℃まで瞬間的に加熱し、2.5分間ホールド後、再び蒸気インジェクター12を使用して、圧力が7.0Kg/cm2の水蒸気を導入し、165℃まで瞬間的に加熱し、2.5分間ホールド後、瞬間的に大気圧まで減圧して冷却し、スラリーをタンク2で受け、ポンプ8により反応液受入器5にスラリーを受入れた。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。 In the reaction apparatus shown in FIG. 1, 14 parts of water was added to 1 part of degreased dried okara in the raw material tank 1, and the pH was adjusted to 5.0 with hydrochloric acid. This suspension from okara is sent to the holding tube by the pump 7, and steam of a pressure of 7 kg / cm 2 is introduced using the steam injector 11 and heated instantaneously to 155 ° C. for 2.5 minutes. After the hold, use steam injector 12 again to introduce water vapor with a pressure of 7.0 Kg / cm 2, heat to 165 ° C momentarily, hold for 2.5 minutes, then instantaneously reduce to atmospheric pressure and cool Then, the slurry was received in the tank 2, and the slurry was received in the reaction liquid receiver 5 by the pump 8. The obtained slurry was separated by centrifugation, the supernatant was subjected to ethanol precipitation, and the precipitate was dried to obtain a water-soluble polysaccharide.
図1に示す反応装置において原料タンク1中に、脱脂された乾燥おから1部に水14部を加え、塩酸にてpHを5に調整した。このおからの懸濁液をポンプ7でホールディング管に送液し、蒸気インジェクター11を使用して、圧力が7Kg/cm2の水蒸気を導入し、155℃まで瞬間的に加熱し、2.5分間ホールド後、瞬間的に大気圧まで減圧して冷却し、スラリーをタンク3で受けた。スラリーをポンプ9によりホールディング管に送液し、蒸気インジェクター13を使用して、圧力が7Kg/cm2の水蒸気を導入し、165℃まで瞬間的に加熱し、2.5分間ホールド後、瞬間的に大気圧まで減圧して冷却し、スラリーをタンク4で受け、ポンプ10により、反応液受入器5にスラリーを受入れた。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。
In the reaction apparatus shown in FIG. 1, 14 parts of water was added to 1 part of degreased dried okara in the raw material tank 1, and the pH was adjusted to 5 with hydrochloric acid. This suspension from okara is sent to the holding tube by the pump 7, steam is introduced into the holding tube using the steam injector 11, the pressure is instantaneously heated to 155 ° C, and held for 2.5 minutes. Then, the pressure was instantaneously reduced to atmospheric pressure to cool, and the slurry was received in the tank 3. The slurry is fed to the holding tube by the pump 9, and steam using the steam injector 13 is introduced into the steam at a pressure of 7 kg / cm 2, heated instantaneously to 165 ° C., held for 2.5 minutes, and then momentarily. The pressure was reduced to atmospheric pressure, the slurry was cooled, the slurry was received in the tank 4, and the slurry was received in the reaction liquid receiver 5 by the
〈比較例1〉
脱脂された乾燥おから1部に水14部を加え、塩酸にてpHを5に調整した。このおからの懸濁液をオートクレーブに入れ、165℃に加熱し、5分間ホールド後自然冷却した。得られたスラリーを再び、オートクレーブに入れ、165℃に加熱し、5分間ホールド後自然冷却した。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。
<Comparative example 1>
14 parts of water was added to 1 part of degreased dried okara and the pH was adjusted to 5 with hydrochloric acid. This okara suspension was placed in an autoclave, heated to 165 ° C., held for 5 minutes, and then naturally cooled. The obtained slurry was again placed in an autoclave, heated to 165 ° C., held for 5 minutes, and then naturally cooled. The obtained slurry was separated by centrifugation, the supernatant was subjected to ethanol precipitation, and the precipitate was dried to obtain a water-soluble polysaccharide.
〈比較例2〉
図1に示す反応装置において原料タンク1中に、脱脂された乾燥おから1部に水14部を加え、塩酸にてpHを5に調整した。このおからの懸濁液をポンプ7でホールディング管に送液し、蒸気インジェクター11を使用して、圧力が7Kg/cm2の水蒸気を導入し、130℃まで瞬間的に加熱し、10分間ホールド後、瞬間的に大気圧まで減圧して冷却し、スラリーをタンク3で受けた。スラリーをポンプ9によりホールディング管に送液し、蒸気インジェクター13を使用して、圧力が7Kg/cm2の水蒸気を導入し、130℃まで瞬間的に加熱し、10分間ホールド後、瞬間的に大気圧まで減圧して冷却し、スラリーをタンク4で受けた。この操作をさらにもう一度行い、反応液受入器5にスラリーを受入れた。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。
<Comparative example 2>
In the reaction apparatus shown in FIG. 1, 14 parts of water was added to 1 part of degreased dried okara in the raw material tank 1, and the pH was adjusted to 5 with hydrochloric acid. This suspension from okara is sent to the holding tube by the pump 7, steam is introduced at a pressure of 7 Kg / cm 2 using the steam injector 11, heated instantaneously to 130 ° C., and held for 10 minutes. Then, the pressure was instantaneously reduced to atmospheric pressure to cool, and the slurry was received in the tank 3. The slurry is fed to the holding tube by the pump 9, and steam using the steam injector 13 is introduced into the steam at a pressure of 7 kg / cm 2, heated instantaneously to 130 ° C., held for 10 minutes, and then instantaneously atmospheric pressure. The pressure was reduced to a low temperature and the slurry was received. This operation was performed once more, and the slurry was received in the reaction solution receiver 5. The obtained slurry was separated by centrifugation, the supernatant was subjected to ethanol precipitation, and the precipitate was dried to obtain a water-soluble polysaccharide.
〈比較例3〉
図1に示す反応装置において原料タンク1中に、脱脂された乾燥おから1部に水14部を加え、塩酸でpHを2.5に調整した。このおからの懸濁液をポンプ7でホールディング管に送液し、蒸気インジェクター11を使用して、圧力が7Kg/cm2の水蒸気を導入し、155℃まで瞬間的に加熱し、2.5分間ホールド後、蒸気インジェクター12を使用して、圧力が7Kg/cm2の水蒸気を導入し、165℃まで瞬間的に加熱し、2.5分間ホールド後冷却装置6で100℃以下に冷却し、反応液受入器5にスラリーを受入れた。得られたスラリーを遠心分離により分離し、上清液をエタノール沈殿処理後、沈殿物を乾燥し、水溶性多糖類を得た。
<Comparative Example 3>
In the reactor shown in FIG. 1, 14 parts of water was added to 1 part of degreased dried okara in the raw material tank 1, and the pH was adjusted to 2.5 with hydrochloric acid. This suspension from okara is sent to the holding tube by the pump 7, and steam of a pressure of 7 kg / cm 2 is introduced using the steam injector 11 and heated instantaneously to 155 ° C. for 2.5 minutes. After the hold, steam of a pressure of 7 kg / cm 2 is introduced using the steam injector 12 and heated instantaneously to 165 ° C., held for 2.5 minutes and then cooled to 100 ° C. or lower with the cooling device 6, and the reaction solution The slurry was received in the receiver 5. The obtained slurry was separated by centrifugation, the supernatant was subjected to ethanol precipitation, and the precipitate was dried to obtain a water-soluble polysaccharide.
結果を比較して以下に示す。
〔(1)水溶性多糖類の歩留〕
水溶性多糖類の歩留は、原料の固形量に対して得られた水溶性多糖類量により算出した。尚、表中のゲージ圧とは圧力計が示す圧力で、圧力計は大気圧を0MPaとした圧力表示になっている。
The results are compared and shown below.
[(1) Water-soluble polysaccharide yield]
The yield of the water-soluble polysaccharide was calculated from the amount of the water-soluble polysaccharide obtained with respect to the solid amount of the raw material. In the table, the gauge pressure is a pressure indicated by a pressure gauge, and the pressure gauge displays a pressure with the atmospheric pressure set to 0 MPa.
実施例1のように、複数回の加熱を短時間で行うことにより、原料の固形量に対する水溶性多糖類の歩留は26%と、高歩留で得られた。また、実施例2、3のように、加熱後瞬間的に大気圧まで減圧して冷却することにより、さらに高歩留の水溶性多糖類が得られた。この実施例の操作は、圧力のデータが示すように、飽和蒸気圧より若干高い、極めて飽和蒸気圧に近い圧力で行う方法であることがわかる。圧力があまり高くなく、抽出条件としては温和な条件で、設備としても大掛かりなものにはならないので、簡便な方法である。さらに、実施例の方法から得られた水溶性大豆ヘミセルロースの分子量分布を分析したところ、従来の抽出方法と同様の分子量パターンであることが確認できた。一方、比較例1のようなオートクレーブ式の加熱方法では、加熱時間を延ばしたとしても、歩留は低くなった。比較例2のように、加熱温度が130℃と低い場合、本発明の加熱・冷却方法を用いても歩留はかなり低くなった。比較例3では、歩留は上がるが、分子量パターンを分析した結果、高分子の画分が分解し、かなり低分子化が進んでいることがわかった。 As in Example 1, by performing heating a plurality of times in a short time, the yield of the water-soluble polysaccharide relative to the solid content of the raw material was 26%, which was obtained at a high yield. Further, as in Examples 2 and 3, a water-soluble polysaccharide having a higher yield was obtained by reducing the pressure to atmospheric pressure instantaneously after heating and cooling. As can be seen from the pressure data, the operation of this example is performed at a pressure slightly higher than the saturated vapor pressure and very close to the saturated vapor pressure. Since the pressure is not so high, the extraction conditions are mild, and the equipment is not too large, it is a simple method. Furthermore, when the molecular weight distribution of the water-soluble soybean hemicellulose obtained from the method of Example was analyzed, it was confirmed that the molecular weight pattern was the same as that of the conventional extraction method. On the other hand, in the autoclave heating method as in Comparative Example 1, the yield was low even if the heating time was extended. As in Comparative Example 2, when the heating temperature was as low as 130 ° C., the yield was considerably low even when the heating / cooling method of the present invention was used. In Comparative Example 3, although the yield increased, as a result of analyzing the molecular weight pattern, it was found that the polymer fraction was decomposed and the molecular weight was considerably lowered.
〔(2)酸性下での乳蛋白安定性評価〕
酸性下での乳蛋白安定性評価は、特開平5-262802号に示される方法で行った。方法は以下の通りである。
[(2) Milk protein stability evaluation under acidic conditions]
Evaluation of milk protein stability under acidic conditions was carried out by the method disclosed in JP-A-5-262802. The method is as follows.
(ヨーグルトの調製)
水に脱脂粉乳を加え(21%)、加熱攪拌し、95℃で殺菌後冷却し、スターターとして市販のプレーンヨーグルトを接種し、38℃の恒温器中で醗酵させた。醗酵したヨーグルトを攪拌機を用いてカードを均質化した。その後、10〜15℃に冷却した。
(Preparation of yogurt)
Nonfat dry milk was added to water (21%), heated and stirred, sterilized at 95 ° C, cooled, inoculated with commercially available plain yogurt as a starter, and fermented in a 38 ° C incubator. The fermented yogurt was homogenized using a stirrer. Then, it cooled to 10-15 degreeC.
(安定剤溶液の調製)
水溶性ヘミセルロース2%溶液を加熱攪拌し(80℃、10分間攪拌)、その後25℃に冷却した。
(Preparation of stabilizer solution)
The water-soluble hemicellulose 2% solution was heated and stirred (stirred at 80 ° C. for 10 minutes) and then cooled to 25 ° C.
(酸性乳飲料の調製)
水に砂糖を加え、次いで上記のヨーグルトを加え、乳酸、クエン酸ナトリウム水溶液でpHを調整した。その後、ホモゲナイザー(150Kg/cm2)で均質化し、瓶詰め後冷蔵庫内で1週間保存した。それぞれの配合は、安定剤溶液、ヨーグルト、砂糖、及び水をそれぞれ、20、40、7、及び33%であった。結果を表2に示す。
(Preparation of acidic milk beverage)
Sugar was added to water, then the above yogurt was added, and the pH was adjusted with lactic acid and an aqueous sodium citrate solution. Thereafter, the mixture was homogenized with a homogenizer (150 Kg / cm 2), stored in a refrigerator for 1 week after bottling. Each formulation was 20, 40, 7, and 33% stabilizer solution, yogurt, sugar, and water, respectively. The results are shown in Table 2.
(表2)
No. 7日後の状態
――――――――――――――――――――――
実施例1 (−)
実施例2 (−)
実施例3 (−)
比較例3 (+)
―――――――――――――――――――――――
*酸性乳飲料の保存後の状態評価
(−): 分離せず安定。(+): 二層に分離
(Table 2)
No. State after 7 days ――――――――――――――――――――――
Example 1 (-)
Example 2 (-)
Example 3 (-)
Comparative Example 3 (+)
―――――――――――――――――――――――
* Assessment of acid milk beverage after storage (-): Stable without separation. (+): Separated into two layers
実施例の方法で得られた水溶性多糖類は、酸性下での乳蛋白安定化能があり、高機能を持つことが確認された。
一方、比較例3のように低pHで抽出して得られた水溶性多糖類は低分子化が進み、酸性乳飲料の安定化能はなく、歩留は高くても、高機能を有する水溶性多糖類を得ることはできない。
It was confirmed that the water-soluble polysaccharide obtained by the method of the example has a milk protein stabilizing ability under acidic conditions and has a high function.
On the other hand, the water-soluble polysaccharide obtained by extraction at a low pH as in Comparative Example 3 has a low molecular weight, has no ability to stabilize acidic milk beverages, and has a high function even if the yield is high. Sexual polysaccharides cannot be obtained.
本発明は、水溶性多糖類の効率的な製造方法であり、特に食品産業での有益な機能が優れている水溶性多糖類の工業的に有利な製法を提供するものである。本発明により食品工業で有用な水溶性多糖類が効率よく得ることができる。 The present invention is an efficient method for producing water-soluble polysaccharides, and provides an industrially advantageous method for producing water-soluble polysaccharides that are particularly excellent in useful functions in the food industry. According to the present invention, water-soluble polysaccharides useful in the food industry can be obtained efficiently.
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| JPH0314802A (en) * | 1989-06-13 | 1991-01-23 | Kyushu Biseibutsu Kenkyusho:Kk | Method and apparatus for extracting hemicellulose from okara |
| JPH074188B2 (en) * | 1990-01-12 | 1995-01-25 | 不二製油株式会社 | Okara sterilization method |
| JP2883911B2 (en) * | 1990-11-15 | 1999-04-19 | ダイセル化学工業株式会社 | Water-soluble cellulose acetate and method for producing the same |
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