JP3746064B2 - β-maltose hydrous crystal-containing powder, its production method and use - Google Patents

β-maltose hydrous crystal-containing powder, its production method and use Download PDF

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JP3746064B2
JP3746064B2 JP2005097350A JP2005097350A JP3746064B2 JP 3746064 B2 JP3746064 B2 JP 3746064B2 JP 2005097350 A JP2005097350 A JP 2005097350A JP 2005097350 A JP2005097350 A JP 2005097350A JP 3746064 B2 JP3746064 B2 JP 3746064B2
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孝 渋谷
利行 杉本
俊雄 三宅
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Hayashibara Seibutsu Kagaku Kenkyujo KK
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本発明は、β−マルトース含水結晶含有粉末とその製造方法並びに用途に関し、更に詳細には、噴霧方式で粉末化され、水系媒体への溶解性に優れ、取扱い容易なβ−マルトース含水結晶含有粉末とその製造方法並びに当該粉末を水系媒体に溶解、含有せしめた飲食物、化粧品、医薬品など各種組成物への用途に関する。   The present invention relates to a β-maltose hydrous crystal-containing powder and a method for producing the same, and more specifically, and more specifically, β-maltose hydrous crystal-containing powder that is powdered by a spray method, has excellent solubility in an aqueous medium, and is easy to handle. Further, the present invention relates to a method for producing the same and a use thereof for various compositions such as foods, drinks, cosmetics and pharmaceuticals in which the powder is dissolved and contained in an aqueous medium.

従来、甘味料として砂糖が大量に消費されてきた。しかしながら、砂糖は甘味が強すぎることから最近の嗜好に合わず、また、虫歯の主な誘発物質であるなどの欠点を有している。   Conventionally, a large amount of sugar has been consumed as a sweetener. However, since sugar is too sweet, it does not meet recent tastes, and has the disadvantage that it is the main inducer of caries.

近年、砂糖の欠点を解消するために、各種糖質を利用することが提案され、とりわけ、澱粉から製造されるマルトースについては、砂糖と比較して甘味が低い、虫歯誘発の懸念が少ない、風味が良好である、などの特徴を有しており、現在では、食品級のβ−マルトース含水結晶含有粉末が、（株）林原商事から登録商標「サンマルト」及び「サンマルトＳ」として市販され、その消費量の更なる拡大が期待できる。   In recent years, it has been proposed to use various sugars in order to eliminate the disadvantages of sugar. Especially, maltose produced from starch has lower sweetness compared to sugar, less concern about induction of tooth decay, and flavor. Currently, food-grade β-maltose hydrous crystal-containing powders are commercially available from Hayashibara Corporation as registered trademarks “San Mart” and “San Mart S”. Further expansion of consumption can be expected.

β−マルトース含水結晶含有粉末は、通常、マルトース含有溶液を原料として、分蜜方式、切削方式又は噴霧方式により製造されている。   The β-maltose hydrous crystal-containing powder is usually produced by a honey method, a cutting method, or a spray method using a maltose-containing solution as a raw material.

これらのうち、分蜜方式は、原料のマルトース含有溶液を濃縮し、β−マルトース含水結晶が種晶として共存する状態下で、撹拌しつつ徐冷してβ−マルトース含水結晶を晶出させたマスキットとし、これを遠心分離などにより、結晶と蜜とに分離し、結晶部分を採取、乾燥する粉末の製造方法である。この方式は、きわめて高純度の結晶粉末が得られるものの、蜜を副生する分、β−マルトース含水結晶粉末の収率が低い欠点がある。   Among these, the honey-concentration method concentrated the raw material maltose-containing solution and gradually cooled it with stirring under the condition that β-maltose hydrous crystals coexisted as seed crystals to crystallize β-maltose hydrous crystals. This is a method for producing a powder in which a mass kit is obtained, which is separated into crystals and nectar by centrifugation or the like, and the crystal portion is collected and dried. This method has a disadvantage that the yield of β-maltose hydrous crystal powder is low due to the fact that nectar is by-produced, although extremely high purity crystal powder can be obtained.

これに対して、切削方式や噴霧方式は、通常、原料のマルトース含有溶液を濃縮し、これをマスキットにした後、切削方式においては全量を固化、熟成させて切削、乾燥して粉末を採取するか、噴霧方式においてはマスキットを噴霧乾燥させたものを熟成し採取する、粉末の製造方法である。これらの方式は、マルトースの純度を高めることはできないものの全量を粉末化でき、蜜を副生することもなく、工業的に有利である。   On the other hand, in the cutting method and the spraying method, normally, the raw material maltose-containing solution is concentrated and made into a mass kit. Then, in the cutting method, the whole amount is solidified and aged, then cut and dried to collect the powder. Alternatively, the spray method is a powder production method in which a mass kit spray-dried is aged and collected. Although these methods cannot increase the purity of maltose, they can be pulverized in total, and do not produce nectar as a byproduct, which is industrially advantageous.

詳細には、切削方式については、通常、マルトース含有溶液を濃縮し、種晶としてβ−マルトース含水結晶を加えてβ−マルトース含水結晶を部分的に晶出させマスキットとしたのち、全量をブロック状に固化、熟成させて、これを切削、乾燥、篩別して、安定なβ−マルトース含水結晶含有粉末を製造するものであるが、この切削方式によって工業的に生産された製品は、（株）林原商事より商標登録「サンマルト」として販売されている。この切削方式によれば、原料マルトースの全量を粉末化することができ、工業的に有利であるものの、この切削方式には、マスキットをブロック状に固化、熟成させるのに５乃至１５日間もの長い期間を要するのみならず、その後の切削、乾燥、篩別に繁雑な工程を必要とする欠点がある。   Specifically, for the cutting method, normally, a maltose-containing solution is concentrated, β-maltose hydrated crystals are added as seed crystals, and β-maltose hydrated crystals are partially crystallized to form a mass kit, and then the entire amount is blocked. This product is solidified and aged, and is then cut, dried and sieved to produce a stable β-maltose hydrous crystal-containing powder. The product produced industrially by this cutting method is Hayashibara Corporation. It is sold as a registered trademark "San Mart" by Shoji. According to this cutting method, the entire amount of raw material maltose can be pulverized, which is industrially advantageous. However, this cutting method requires 5 to 15 days to solidify and age the mass kit in blocks. Not only does it require a period of time, it also has the disadvantage of requiring complicated processes for subsequent cutting, drying and sieving.

一方、噴霧方式については、従来、マルトース含有溶液を濃縮し、種晶としてβ−マルトース含水結晶を加えてβ−マルトース含水結晶を部分的に晶出させマスキットとしたのち、これを噴霧乾燥して粉末化し、熟成させて、β−マルトース含水結晶含有粉末を製造する方法が知られていた（特許文献１、特許文献２）。この噴霧方式は、マスキットを固化、熟成させる長い期間を必要とせず工業的には最も有利であるものの、それでも、その製造に３乃至４日間もの期間を要し、噴霧方式でスムーズに連続的に粉末を製造することが困難であった。   On the other hand, for the spraying method, conventionally, a maltose-containing solution is concentrated, β-maltose hydrated crystals are added as seed crystals to partially crystallize β-maltose hydrated crystals to form a mass kit, which is then spray-dried. There has been known a method of producing a powder containing β-maltose hydrous crystals by pulverization and aging (Patent Document 1, Patent Document 2). This spray method is industrially most advantageous because it does not require a long period for solidifying and aging the mass kit, but it still takes 3 to 4 days for its production, and it is smoothly and continuously produced by the spray method. It was difficult to produce a powder.

その後、これを改善するために、マルトース以外の糖質、具体的には、グルコース、マルトトリオース及びグルコース重合度４以上のオリゴ糖などの含量をできる限り低減させて、無水物換算で、マルトース含量約９５質量％（以下、本明細書では、特段の断りがない限り、質量％を単に％と略称する。）以上とした極めて高純度のマルトース含有溶液を用いることにより、噴霧方式でβ−マルトース含水結晶含有粉末を比較的短時間で製造する方法が確立され、（株）林原商事より登録商標「サンマルトＳ」として販売されるに至った。しかしながら、本発明者等が初めて見いだした知見によれば、この噴霧方式によって得られるβ−マルトース含水結晶含有粉末は、意外にも、水系媒体への溶解性が必ずしも満足できるものでなく、この溶解性を更に向上させる必要性のあることが判明した。   Thereafter, in order to improve this, the content of carbohydrates other than maltose, specifically, glucose, maltotriose and oligosaccharides having a glucose polymerization degree of 4 or more are reduced as much as possible to reduce maltose in terms of anhydride. By using an extremely high-purity maltose-containing solution having a content of about 95% by mass (hereinafter, unless otherwise specified, mass% is simply abbreviated as%), β- A method for producing maltose hydrous crystal-containing powder in a relatively short time was established, and it was sold by Hayashibara Shoji Co., Ltd. under the registered trademark “Sanmalto S”. However, according to the knowledge found by the present inventors for the first time, the β-maltose hydrous crystal-containing powder obtained by this spraying method is surprisingly not necessarily satisfactory in solubility in an aqueous medium. It has been found that there is a need to further improve the performance.

特公昭５４−３９３７号公報Japanese Patent Publication No.54-3937 特公昭５４−２７３２５号公報Japanese Patent Publication No.54-27325

本発明は、本発明者等が新たに見いだした上記噴霧方式の欠点を解決するためになされたもので、工業的に有利で、且つ安価に実施できる噴霧方式を採用し、水系媒体への溶解性に優れ、取扱い容易なβ−マルトース含水結晶含有粉末とその製造方法並びに用途を提供することを課題とするものである。   The present invention has been made in order to solve the disadvantages of the above-mentioned spraying method newly found by the present inventors, and employs a spraying method that is industrially advantageous and can be carried out at low cost, and is dissolved in an aqueous medium. It is an object of the present invention to provide a β-maltose hydrous crystal-containing powder that is excellent in properties and easy to handle, a method for producing the same, and an application.

本発明者等は、上記の課題を解決するために、噴霧方式で粉末化されるβ−マルトース含水結晶含有粉末の各種物性について研究し、とりわけ、原料のマルトース含有溶液の糖組成と得られる粉末の各種物性との関係に着目して、鋭意研究を重ねた。即ち、各種糖組成のマルトース含有溶液から調製したマスキットを、噴霧方式で粉末とし、まず、比較的低湿度で高温の雰囲気に保ち、次いで、比較的高湿度で低温の雰囲気に保って得られるβ−マルトース含水結晶含有粉末を採取し、この粉末の吸湿性、固着性、溶解性、α−アノマー含量、結晶化度などの諸性質について詳細に調べた。   In order to solve the above problems, the present inventors have studied various physical properties of β-maltose hydrous crystal-containing powders that are pulverized by a spray method, and in particular, the sugar composition of the raw material maltose-containing solution and the resulting powder Focusing on the relationship with various physical properties, we conducted extensive research. That is, a mass kit prepared from a maltose-containing solution of various sugar compositions is powdered by a spray method, first kept in a relatively high humidity and low temperature atmosphere, and then kept in a relatively high humidity and low temperature atmosphere. -Maltose hydrous crystal-containing powder was collected, and various properties such as hygroscopicity, adhesiveness, solubility, α-anomer content, crystallinity, etc. of this powder were examined in detail.

その結果、（１）、噴霧方式で粉末化され、無水物換算で、マルトース８６％以上９３％未満およびグルコース２％以上含有し、結晶化度が６２％以上７２％未満であるβ−マルトース含水結晶含有粉末が、水系媒体への溶解性に優れ、且つ、取扱い容易な粉末であることを見いだし、当該粉末の製造方法として、（２）、無水物換算で、マルトース８６％以上９３％未満およびグルコース２％以上を含有している溶液を、β−マルトース含水結晶を晶出させたマスキットとし、次いで噴霧方式で粉末とし、更に、比較的低湿度で高温の雰囲気に保って、マルトース中のα−アノマー高含有粉末とし、その後、比較的高湿度で低温の雰囲気に保って、噴霧された粉末のマルトース中のα−アノマー含量を７％以上１４％未満に低減せしめ、得られる結晶化度が６２％以上７２％未満の粉末を採取することを特徴とするβ−マルトース含水結晶含有粉末の製造方法を確立し、併せて、（３）、前記の（１）、又は（２）の製造方法で得られるβ−マルトース含水結晶含有粉末を水系媒体に溶解、含有せしめた組成物を確立して本発明を完成した。   As a result, (1) β-maltose hydrous powder which is powdered by a spray method, contains 86% to 93% maltose and 2% or more glucose in terms of anhydride, and has a crystallinity of 62% to less than 72%. The crystal-containing powder was found to be a powder having excellent solubility in an aqueous medium and easy to handle. As a method for producing the powder, (2) maltose 86% to less than 93% in terms of anhydride and A solution containing 2% or more of glucose is used as a mass kit in which β-maltose hydrous crystals are crystallized, then powdered by a spray method, and further maintained in a relatively low humidity and high temperature atmosphere to maintain α in maltose. A powder containing a high amount of anomer, and then kept in a relatively high humidity and low temperature atmosphere to reduce the α-anomer content in the maltose of the sprayed powder to 7% or more and less than 14%; A method for producing a β-maltose hydrous crystal-containing powder characterized by collecting a powder having a crystallinity of 62% or more and less than 72%. (3), (1) or ( The present invention was completed by establishing a composition in which β-maltose hydrous crystal-containing powder obtained by the production method 2) was dissolved and contained in an aqueous medium.

本発明によれば、水系媒体への溶解性に優れたβ−マルトース含水結晶含有粉末を容易に、低コストで製造できる。   According to the present invention, a β-maltose hydrous crystal-containing powder excellent in solubility in an aqueous medium can be easily produced at low cost.

本発明のβ−マルトース含水結晶含有粉末の原料に用いるマルトース含有溶液としては、噴霧方式で粉末化され、無水物換算で、マルトース８６％以上９３％未満およびグルコース２％以上を含有し、結晶化度が６２％以上７２％未満であるβ−マルトース含水結晶含有粉末ができるものであればよく、そのようなマルトース含有溶液の製造方法としては、例えば、特公昭５４−３９３７号公報、特公昭５６−２８１５３号公報、特公昭５７−３３５６号公報、特許第２５１８６４６号公報などに開示されるように、各種の澱粉を加熱、糊化したのちにα−アミラーゼ（ＥＣ．３．２．１．１）を作用させるか、酸または機械力により、できるだけ低い加水分解率に液化し、次いで、β−アミラーゼ（ＥＣ．３．２．１．２）と澱粉枝切り酵素（プルラナーゼＥＣ．３．２．１．４１またはイソアミラーゼＥＣ．３．２．１．６８のいずれか）を作用させて糖化して製造する方法がある。   The maltose-containing solution used as a raw material for the β-maltose hydrous crystal-containing powder of the present invention is pulverized by a spray method and contains 86% to less than 93% maltose and 2% or more glucose in terms of anhydride. Any β-maltose hydrous crystal-containing powder having a degree of 62% or more and less than 72% can be used. Examples of methods for producing such a maltose-containing solution include Japanese Patent Publication No. 54-3937 and Japanese Patent Publication No. 56. As disclosed in Japanese Patent No. 28153, Japanese Patent Publication No. 57-3356, Japanese Patent No. 2518646, and the like, various starches are heated and gelatinized and then α-amylase (EC 3.2.1.1.1). ) Or by acid or mechanical force to liquefy to the lowest possible hydrolysis rate, and then β-amylase (EC 3.2.1.2) and starch debranching enzyme By the action of one) of the pullulanase EC.3.2.1.41 or isoamylase EC.3.2.1.68 there is a method for producing and saccharified.

本発明でいう、無水物換算で、マルトース８６％以上９３％未満及びグルコース２％以上を含有する溶液は、前述のように澱粉から製造され、通常、他の糖質としてマルトトリオース及びグルコース重合度４以上のオリゴ糖などを含有している。このマルトトリオース及びグルコース重合度４以上のオリゴ糖は、マルトース含有溶液からβ−マルトース含水結晶の晶出を阻害し易いのでできるだけこの含量を低減させることが望ましく、とりわけ、マルトトリオースについては、その含量を、無水物換算で、２％未満にするのが好適である。   The solution containing maltose 86% or more and less than 93% and glucose 2% or more, as referred to in the present invention, is produced from starch as described above, and usually maltotriose and glucose polymerization as other carbohydrates. Contains oligosaccharides with a degree of 4 or more. Since this maltotriose and oligosaccharide having a glucose polymerization degree of 4 or more are liable to inhibit crystallization of β-maltose hydrous crystals from a maltose-containing solution, it is desirable to reduce this content as much as possible. Especially, for maltotriose, The content is preferably less than 2% in terms of anhydride.

マルトトリオース及びグルコース重合度４以上のオリゴ糖の含量を低減させる方法としては、例えば、特公昭５６−２８１５４号公報、特許第２６９６５３０号公報などに開示されているように、マルトトリオースまたはグルコース重合度４以上のオリゴ糖に比較的よく作用し、それらを分解してグルコースやマルトースなどを生成する酵素を作用させることで、マルトトリオースまたはグルコース重合度４以上のオリゴ糖の含量を減少させるとともにマルトースの含量を増加させることができる。また、ＵＦ膜や逆浸透膜、活性炭などを用いてマルトトリオースまたはグルコース重合度４以上のオリゴ糖を分離、除去することも、更に、特公昭６２−５１１２０号公報、特公平５−７９３１６号公報などに開示されているように、イオン交換樹脂を用いるクロマト分離法を用いてマルトトリオースまたはそれ以上のオリゴ糖を分離、除去することもできる。   As a method for reducing the content of maltotriose and oligosaccharide having a glucose polymerization degree of 4 or more, for example, as disclosed in Japanese Patent Publication No. 56-28154, Japanese Patent No. 2696530, etc., maltotriose or glucose Reducing the content of maltotriose or oligosaccharides having a polymerization degree of glucose of 4 or more by acting on enzymes having a polymerization degree of 4 or more and acting on enzymes that decompose them to produce glucose or maltose. At the same time, the maltose content can be increased. In addition, it is also possible to separate and remove maltotriose or oligosaccharide having a glucose polymerization degree of 4 or more using a UF membrane, reverse osmosis membrane, activated carbon, or the like, as described in JP-B-62-51120 and JP-B-5-79316. As disclosed in publications and the like, maltotriose or higher oligosaccharides can also be separated and removed using a chromatographic separation method using an ion exchange resin.

本発明の特徴の一つは、次に述べる各工程を組み合わせる一連の製造方法を採用し、マルトースの晶出速度を高めることにより、無水物換算で、マルトース含量が８６％以上９３％未満、換言すれば、グルコース、マルトトリオース及びグルコース重合度４以上のオリゴ糖などのマルトース以外の糖質を７％以上１４％未満と比較的多量共存含有しているにもかかわらず、噴霧方式で、溶解性に優れ、且つ、取扱いの容易なβ−マルトース含水結晶含有粉末が容易に、比較的短時間に製造できることである。   One of the features of the present invention is that a maltose content is 86% or more and less than 93% in terms of anhydride by adopting a series of production methods combining the following steps and increasing the crystallization rate of maltose. In this case, it is dissolved in a spray method despite the fact that carbohydrates other than maltose, such as glucose, maltotriose and oligosaccharides with a glucose polymerization degree of 4 or higher, are present in a relatively large amount of 7% to less than 14%. A β-maltose hydrous crystal-containing powder that is excellent in properties and easy to handle can be easily produced in a relatively short time.

即ち、一連の製造方法は、（ａ）、本発明に用いる糖組成のマルトース含有溶液をマスキットとし、次いで、（ｂ）、噴霧方式、望ましくは、高圧ノズルや回転円盤を用いた噴霧乾燥法により粉末とし、望ましくは、水分１０％未満、更に望ましくは、約５乃至９％の粉末とし、更に、これに含まれるマルトースの晶出速度を高めるために、（ｃ）、これを比較的低湿度で高温の雰囲気、望ましくは、相対湿度（ＲＨ）４０％未満、更に望ましくは２０％未満で、望ましくは、７５℃を越え、更に望ましくは８０乃至１１０℃の雰囲気に１乃至４時間程度保って、マルトース異性体であるα−アノマーの高含有粉末、望ましくは、マルトース中のα−アノマー含量が３５％以上の粉末とし、その後、（ｄ）、比較的高湿度で低温の雰囲気、望ましくは、相対湿度（ＲＨ）７０％を越え、更に望ましくは８０％以上で、望ましくは、５０℃未満、更に望ましくは２０乃至４５℃の雰囲気に５乃至１０時間程度保って、そのマルトース中のα−アノマー含量を７％以上１４％未満に低減せしめ、（ｅ）、得られる結晶化度が６２％以上７２％未満のβ−マルトース含水結晶含有粉末を採取することにより達成される。   That is, a series of production methods are (a) using a maltose-containing solution of the sugar composition used in the present invention as a mass kit, and then (b) spraying, preferably by a spray drying method using a high-pressure nozzle or a rotating disk. In order to increase the crystallization rate of maltose contained in the powder, preferably (c), which has a relatively low humidity, the powder is preferably less than 10% moisture, more preferably about 5-9%. At a high temperature atmosphere, preferably less than 40% relative humidity (RH), more preferably less than 20%, preferably above 75 ° C., more preferably 80-110 ° C. for about 1 to 4 hours. , A powder containing a high content of α-anomer which is a maltose isomer, preferably a powder having a content of α-anomer in maltose of 35% or more, and (d) a relatively high humidity and low temperature atmosphere, desired Alternatively, the relative humidity (RH) exceeds 70%, more preferably 80% or more, preferably less than 50 ° C., more preferably 20 to 45 ° C. for about 5 to 10 hours. The α-anomer content is reduced to 7% or more and less than 14%, and (e) is achieved by collecting β-maltose hydrous crystal-containing powder having a crystallinity of 62% or more and less than 72%.

以下、前記各工程について、更に詳細に説明する。前記工程（ａ）においては、マルトース含有溶液を濃縮し、望ましくは、水分１５乃至３０％の濃縮液とし、これに種晶としてβ−マルトース含水結晶の適量、通常は０．１乃至５％程度を共存させて徐冷、攪拌しつつマスキットを製造する。この際、β−マルトース含水結晶の晶出率（以下、本明細書では、特段の断りがない限り、晶出率とは、マスキットを結晶と蜜とに分別し、（結晶無水物重量／マスキットの無水物重量）×１００の値をいう。）が高くなればなる程、マスキットの粘度が上昇する。   Hereafter, each said process is demonstrated in detail. In the step (a), the maltose-containing solution is concentrated, desirably a concentrated solution having a water content of 15 to 30%, and an appropriate amount of β-maltose hydrous crystal as a seed crystal, usually about 0.1 to 5%. A mass kit is produced while gradually cooling and stirring together. At this time, the crystallization rate of β-maltose hydrous crystals (hereinafter, unless otherwise specified, the crystallization rate means that the mass kit is divided into crystals and nectar, and (crystal anhydride weight / mass kit). The weight of the anhydride)) x 100.) The higher the value of), the higher the viscosity of the mass kit.

また、前記工程（ｂ）においては、本発明者等は、β−マルトース含水結晶を含む高粘度のマスキットを実質的に晶出率を低下させない範囲内で加熱、昇温させてその粘度を低下させることにより、噴霧方式でβ−マルトース含水結晶含有粉末が容易に製造できるという知見を得た。すなわち、本発明者等は、マスキットを加熱、昇温すると、粘度は温度の上昇とともに直ちに低下するものの、生成した結晶は多少温度が上昇しても短時間では溶解することはなく、晶出率の低下は殆ど見られないことを見出し、実質的に晶出率を低下させることなく、マスキットを昇温することでマスキットの粘度を、望ましくは、５０，０００ｃｐ（以下、本明細書では、特段の断りがない限り、粘度ｃｐとはＢＨ型回転粘度計を使用し、Ｎｏ．７のローターを用い、４ｒｐｍで回転させて測定したときの値をいう。）以下にすれば、噴霧処理の操作が容易となり、しかも、その乾燥効率を良くできることが明らかとなった。   In the step (b), the present inventors reduced the viscosity by heating and raising the temperature of the high-viscosity mass kit containing β-maltose hydrous crystals within a range that does not substantially reduce the crystallization rate. As a result, it was found that a β-maltose hydrous crystal-containing powder can be easily produced by a spray method. That is, the inventors of the present invention, when the mass kit is heated and heated, the viscosity immediately decreases as the temperature increases, but the generated crystals do not dissolve in a short time even if the temperature rises somewhat, and the crystallization rate The viscosity of the mass kit is desirably increased by raising the temperature of the mass kit without substantially reducing the crystallization rate, and desirably the viscosity of the mass kit is 50,000 cp (hereinafter referred to as “special” in the present specification). Unless otherwise indicated, the viscosity cp means a value measured by rotating at 4 rpm using a No. 7 rotor using a BH rotational viscometer. It has become clear that the drying efficiency can be improved.

昇温の方法は特に限定されない。例えば、マスキットが入った助晶機のジャケットに温水を流す、助晶機内に直接蒸気を加える、助晶機から送液ポンプの間で熱交換機を使用して加温するなど公知の方式が適宜採用できる。昇温の程度は、マスキットの粘度が噴霧できる程度、具体的には、５０，０００ｃｐ以下、望ましくは、４０，０００ｃｐ以下となればよく、通常、２乃至１５℃、望ましくは、２乃至１０℃の範囲で晶出率の低下を起こさない程度になるべく短時間に行うのが好適である。   The method for raising the temperature is not particularly limited. For example, known methods such as flowing warm water through a jacket of a crystallizer containing a mass kit, adding steam directly into the crystallizer, and heating using a heat exchanger between the crystallizer and the liquid feed pump are appropriately used. Can be adopted. The degree of temperature rise is such that the viscosity of the mass kit can be sprayed, specifically, 50,000 cp or less, preferably 40,000 cp or less, usually 2 to 15 ° C., preferably 2 to 10 ° C. It is preferable to carry out in as short a time as possible without causing a decrease in the crystallization rate.

前記工程（ｃ）においては、粉末をα−マルトース無水結晶の少量と接触させてマルトース中のα−アノマーへの異性化を促進する方法を採用することも有利に実施できる。マルトース異性体としては、α−アノマーとβ−アノマーが存在する。結晶の形態としては、α−マルトース無水結晶、β−マルトース含水結晶、β−マルトース無水結晶並びにα−マルトースとβ−マルトースが一定の割合で共存するα、βコンプレックス結晶が知られている。   In the step (c), it is also possible to advantageously employ a method in which the powder is brought into contact with a small amount of anhydrous α-maltose crystals to promote isomerization to α-anomer in maltose. As maltose isomers, there are α-anomer and β-anomer. Known crystal forms include anhydrous α-maltose crystals, hydrous β-maltose crystals, anhydrous β-maltose crystals, and α and β complex crystals in which α-maltose and β-maltose coexist at a certain ratio.

マルトース中のα−アノマーを７％以上１４％未満含有するとは、マルトース中のα−アノマーの含量を意味し、その形態が非晶質であるか結晶質であるかは問わない。一般的に、マルトース中のα−アノマーの含量が１４％以上の場合は、非晶質のマルトースが多いか、又は、α−マルトース無水結晶を含有していることを意味し、逆に、マルトース中のα−アノマーの含量が７％未満の場合は、残りはβ−マルトースであるのでβ−マルトース含水又は無水結晶の含量が高いことを意味している。   The content of α-anomer in maltose of 7% or more and less than 14% means the content of α-anomer in maltose, regardless of whether the form is amorphous or crystalline. In general, when the content of α-anomer in maltose is 14% or more, it means that there is a lot of amorphous maltose or α-maltose anhydrous crystals, and conversely, maltose. When the content of α-anomer is less than 7%, the rest is β-maltose, which means that the content of water containing β-maltose or anhydrous crystals is high.

更に、前記工程（ｄ）においては、５乃至１０時間程度保ってマルトース中のα−アノマー含量を７％以上１４％未満に低減せしめた後、必要ならば、更に乾燥工程を加えることも有利に実施できる。   Further, in the step (d), after the α-anomer content in the maltose is reduced to 7% or more and less than 14% by keeping it for about 5 to 10 hours, it is advantageous to add a drying step if necessary. Can be implemented.

前記工程（ｅ）においては、得られるβ−マルトース含水結晶含有粉末が、粒度分布試験（澱粉糖関連工業分析法、１９９１年発行、（株）食品化学新聞社発売に１１８頁記載の粒度分布の測定方法に準じて、ＪＩＳ・Ｚ８８０１のふるいを用い、試料５０ｇを１５分間篩って測定した）において、比較的粒度の大きな粉末を多量含有しており、通常、１０６μｍを越す粉末を６０％以上含んでおり、多くの場合、１５０μｍを越え３００μｍ以下の粉末を４０％以上含んでいる。また、この１５０μｍを越え３００μｍ以下の粉末は、しばしば噴霧乾燥機内を落下する途中、または熟成から乾燥終了に至る工程で、複数個の粒子が付着、凝集して生成した凝集物を含んでいる。   In the step (e), the obtained β-maltose hydrous crystal-containing powder is subjected to a particle size distribution test (starch sugar related industrial analysis method, published in 1991, released by Food Chemical Newspaper Co., Ltd. on page 118). According to the measurement method, a sample of 50 g was measured for 15 minutes using a JIS / Z8801 sieve) and contained a large amount of powder having a relatively large particle size, and usually more than 60% of the powder exceeding 106 μm In many cases, it contains 40% or more of powders exceeding 150 μm and not more than 300 μm. In addition, the powder of more than 150 μm and less than 300 μm often contains agglomerates produced by adhering and agglomerating a plurality of particles in the course of dropping in the spray dryer or in the process from aging to completion of drying.

この様にして得られる本発明のβ−マルトース含水結晶含有粉末は、水系媒体への溶解性に優れ、しかも、保存安定性、流動性良好で、取扱い容易な粉末である。   The β-maltose hydrous crystal-containing powder of the present invention thus obtained is a powder that is excellent in solubility in an aqueous medium, has good storage stability and fluidity, and is easy to handle.

本発明でいう水系媒体とは、β−マルトース含水結晶含有粉末を溶解、含有させることのできる水または水分を多く含む液状、ペースト状、半固状物又は固状物を意味する。とりわけ、粘性を有する水系媒体としては、例えば、糖類、澱粉、脂肪、蛋白質、ポリフェノール及び乳化剤などを含むものであって、具体的には、例えば、求肥、餅菓子などに用いられる糊化澱粉、小麦粉から調製された生地、ドウ、麺などや、生あん、魚肉、畜肉などの擂潰食肉、液卵、乳クリーム、発酵乳、ピーナッツペースト、果実パルプ、野菜パルプ、糖類シロップ、抽出液濃縮物などがある。   The aqueous medium referred to in the present invention means a liquid, paste, semi-solid or solid containing a large amount of water or water that can dissolve and contain the β-maltose hydrous crystal-containing powder. In particular, the aqueous medium having viscosity includes, for example, sugars, starches, fats, proteins, polyphenols, emulsifiers, and the like. Specifically, for example, gelatinized starch used for fertilization, rice cake confectionery, etc. Dough, dough, noodles, etc. prepared from wheat flour, crushed meat such as raw bean paste, fish meat, livestock meat, liquid egg, milk cream, fermented milk, peanut paste, fruit pulp, vegetable pulp, sugar syrup, extract concentrate and so on.

本発明のβ−マルトース含水結晶含有粉末は、前述の粘性を持つ水系媒体への溶解性に優れ、これに利用されることはもとより、粘度の低い水系媒体への用途にも有利に利用できる。また、良質で上品な甘味を有すると共に、虫歯の原因の一つであるデキストランの生成を阻害する作用を有しており、虫歯を起こしにくい甘味料としても好適に利用される。   The β-maltose hydrous crystal-containing powder of the present invention is excellent in solubility in an aqueous medium having the above-mentioned viscosity, and can be advantageously used not only for this purpose but also for use in an aqueous medium having a low viscosity. In addition, it has good quality and elegant sweetness and has an action of inhibiting the production of dextran, which is one of the causes of dental caries, and is also suitably used as a sweetener that hardly causes caries.

また、本発明のβ−マルトース含水結晶含有粉末は、プルラン、ヒドロキシエチルスターチ、ポリビニルピロリドンなどの公知の結合剤と併用して、錠剤の糖衣剤としても有利に用いることができる。更に、本発明のβ−マルトース含水結晶含有粉末は、浸透圧調節性、賦形性、照り付与性、保湿性、粘性、糖質晶出防止性、糊化澱粉の老化防止性などの有用な性質をも兼備している。   Moreover, the β-maltose hydrous crystal-containing powder of the present invention can be advantageously used as a sugar coating for tablets in combination with known binders such as pullulan, hydroxyethyl starch, and polyvinylpyrrolidone. Furthermore, the β-maltose hydrous crystal-containing powder of the present invention is useful for osmotic pressure controllability, shaping, irradiating properties, moisture retention, viscosity, sugar crystallization prevention properties, anti-aging properties of gelatinized starch, etc. It also has properties.

従って、本発明のβ−マルトース含水結晶含有粉末は、甘味料、呈味改良剤、風味改良剤、品質改良剤、安定剤、賦形剤などとして、食品、飼料、餌料、化粧品、医薬品、嗜好品などの各種組成物に有利に用いることができる。   Accordingly, the β-maltose hydrous crystal-containing powder of the present invention is used as a sweetener, a taste improver, a flavor improver, a quality improver, a stabilizer, an excipient, etc. as food, feed, feed, cosmetics, pharmaceuticals, tastes, etc. It can be advantageously used in various compositions such as products.

本発明のβ−マルトース含水結晶含有粉末の具体的な用途としては、各種物品の甘味付けのための調味料としても用いることができる。必要に応じて、例えば、粉飴、ブドウ糖、フラクトース、ラクトスクロース、蔗糖、トレハロース、異性化糖、蜂蜜、メープルシュガー、イソマルトオリゴ糖、ガラクトオリゴ糖、フラクトオリゴ糖、ソルビトール、マルチトール、ラクチトール、ジヒドロカルコン、ステビオシド、α−グリコシルステビオシド、レバウディオシド、グリチルリチン、Ｌ−アスパルチル−Ｌ−フェニルアラニンメチルエステル、スクラロース、アセスルファムＫ、サッカリン、グリシン、アラニンなどのような他の甘味料の１種又は２種以上と併用することも、必要ならば、デキストリン、澱粉、砂糖、乳糖などの増量剤の１種又は２種以上と併用することも随意である。   As a specific use of the β-maltose hydrous crystal-containing powder of the present invention, it can be used as a seasoning for sweetening various articles. As necessary, for example, powdered sugar, glucose, fructose, lactosucrose, sucrose, trehalose, isomerized sugar, honey, maple sugar, isomaltoligosaccharide, galactooligosaccharide, fructooligosaccharide, sorbitol, maltitol, lactitol, dihydrochalcone, Use in combination with one or more of other sweeteners such as stevioside, α-glycosyl stevioside, rebaudioside, glycyrrhizin, L-aspartyl-L-phenylalanine methyl ester, sucralose, acesulfame K, saccharin, glycine, alanine, etc. If necessary, it is also optional to use in combination with one or more fillers such as dextrin, starch, sugar and lactose.

又、本発明のβ−マルトース含水結晶含有粉末は、そのままで、又は必要に応じて、適宜の増量剤、賦形剤、結合剤、甘味料などの１種又は２種以上と併用して、顆粒、球状、短棒状、板状、立方体状、錠剤状、フィルム状又はシート状などの各種形状に成型して用いることも随意である。   Further, the β-maltose hydrous crystal-containing powder of the present invention is used as it is or in combination with one or more of appropriate fillers, excipients, binders, sweeteners, etc. It is also optional to use in various shapes such as granules, spheres, short bars, plates, cubes, tablets, films or sheets.

更に、本発明のβ−マルトース含水結晶含有粉末の甘味は、酸味、塩から味、渋味、旨味、苦味などの他の呈味を有する各種物質とよく調和し、各種飲食物の甘味付け、呈味改良に、又品質改良を目的として用いることができる。具体的には、例えば、アミノ酸、ペプチド類、醤油、粉末醤油、味噌、粉末味噌、もろみ、ひしお、ふりかけ、マヨネーズ、ドレッシング、食酢、三杯酢、粉末すし酢、中華の素、天つゆ、麺つゆ、ソース、ケチャップ、焼肉のタレ、カレールウ、シチューの素、スープの素、ダシの素、核酸系調味料、複合調味料、みりん、新みりん、テーブルシュガー、コーヒーシュガーなど各種調味料として有利に利用できる。又、例えば、せんべい、あられ、おこし、餅類、まんじゅう、ういろう、あん類、羊羮、水羊羮、錦玉、ゼリー、カステラ、飴玉などの各種和菓子、パン、ビスケット、クラッカー、クッキー、パイ、プリン、バタークリーム、カスタードクリーム、シュークリーム、ワッフル、スポンジケーキ、ドーナツ、チョコレート、チューインガム、キャラメル、キャンディーなどの洋菓子、アイスクリーム、シャーベットなどの氷菓、果実のシロップ漬、氷蜜などのシロップ類、フラワーペースト、ピーナッツペースト、フルーツペースト、スプレッドなどのペースト類、ジャム、マーマレード、シロップ漬、糖果などの果実、野菜の加工食品類、福神漬、べったら漬、千枚漬、らっきょう漬などの漬物類、たくあん漬の素、白菜漬の素などの漬物の素類、ハム、ソーセージなどの畜肉製品類、魚肉ハム、魚肉ソーセージ、かまぼこ、ちくわ、天ぷらなどの魚肉製品、ウニ、イカの塩辛、酢こんぶ、さきするめ、ふぐみりん干しなどの各種珍味類、のり、山菜、するめ、小魚、貝などで製造されるつくだ煮類、煮豆、ポテトサラダ、こんぶ巻などの惣菜食品、ヨーグルト、チーズなどの乳製品、魚肉、畜肉、果実、野菜のビン詰、缶詰類、清酒、合成酒、リキュール、洋酒などの酒類、コーヒー、紅茶、ココア、ジュース、炭酸飲料、乳酸飲料、乳酸菌飲料などの清涼飲料水、プリンミックス、ホットケーキミックス、即席しるこ、即席スープなどの即席食品、更には、離乳食、治療食、ドリンク剤、ペプチド食品、冷凍食品、健康食品などの各種飲食物に有利に利用できる。   Furthermore, the sweetness of the β-maltose hydrous crystal-containing powder of the present invention is well harmonized with various substances having other tastes such as acidity, salt to taste, astringency, umami, bitterness, sweetening various foods, It can be used for improving taste and improving quality. Specifically, for example, amino acids, peptides, soy sauce, powdered soy sauce, miso, powdered miso, moromi, hashio, sprinkle, mayonnaise, dressing, vinegar, three cups of vinegar, powdered sushi vinegar, Chinese food, tentsuyu, noodle soup, sauce , Ketchup, grilled meat sauce, curry roux, stew element, soup element, dashi element, nucleic acid seasoning, compound seasoning, mirin, new mirin, table sugar, coffee sugar, etc. Also, for example, various Japanese sweets such as rice crackers, hail, rice cakes, rice cakes, manju, eel wax, bean jam, water sheep cake, brocade, jelly, castella, rice cake, bread, biscuits, crackers, cookies, pie , Pudding, butter cream, custard cream, cream puff, waffle, sponge cake, donut, chocolate, chewing gum, caramel, candy and other Western confectionery, ice cream, sorbet and other ice confectionery, fruit syrup pickled, syrup such as ice honey, flower Paste such as paste, peanut paste, fruit paste, spread, fruit such as jam, marmalade, syrup pickles, sugar cane, processed foods of vegetables, pickles such as Fukujin pickles, bedara pickles, thousand pieces pickles, pickled pickles, takan pickles, Pickled Chinese cabbage Raw meat products such as ham, sausage, fish meat ham, fish sausage, fish products such as kamaboko, chikuwa, tempura, sea urchin, salted squid, vinegared konbu, suki-sume, dried fugurin, and paste , Wild vegetables such as wild vegetables, sushi, small fish, shellfish, boiled beans, potato salad, side dish foods such as kombu rolls, dairy products such as yogurt and cheese, fish meat, livestock meat, fruits, bottled vegetables, canned foods , Sake, synthetic sake, liqueur, liquor such as Western liquor, coffee, tea, cocoa, juice, carbonated beverages, lactic acid beverages, lactic acid beverages, lactic acid bacteria beverages and other soft drinks, pudding mix, hot cake mix, instant sushi, instant soup, etc. It can be advantageously used in foods, and various foods such as baby foods, therapeutic foods, drinks, peptide foods, frozen foods, and health foods.

更に、家畜、家禽、その他蜜蜂、蚕、魚などの飼育動物用の飼料、餌料などの嗜好性を向上させる目的で使用することもできる。その他、タバコ、練歯磨、口紅、リップクリーム、内服液、錠剤、トローチ、肝油ドロップ、口中清涼剤、口中香剤、うがい剤などの各種固形物用甘味剤として、又はそれらの呈味改良剤、矯味剤、品質改良剤、安定剤などとして有利に利用できる。   Furthermore, it can also be used for the purpose of improving the palatability of feed, feed, etc. for domestic animals, poultry, other bees, rabbits, fish and other domestic animals. In addition, as a sweetener for various solids such as tobacco, toothpaste, lipstick, lip balm, oral solution, tablet, troche, liver oil drop, mouth freshener, mouth fragrance, gargle, etc., or a taste improver thereof, It can be advantageously used as a corrigent, quality improver, stabilizer and the like.

本発明のβ−マルトース含水結晶含有粉末は、品質改良剤及び／又は安定剤として、有効成分、活性成分又は生理活性物質を含む健康食品、医薬品などに配合することにより、安定で高品質の液状、ペースト状又は固状の健康食品や医薬品を得ることができる。前記有効成分や生理活性物質としては、例えば、インターフェロン−α、インターフェロン−β、インターフェロン−γ、ＴＮＦ−α、ＴＮＦ−β、マクロファージ遊走阻止因子、コロニー刺激因子、トランスファーファクター、インターロイキンなどのリンホカイン、インシュリン、成長ホルモン、プロラクチン、エリトロポエチン、卵細胞刺激ホルモンなどのホルモン、ＢＣＧワクチン、日本脳炎ワクチン、はしかワクチン、ポリオ生ワクチン、痘苗、破傷風トキソイド、ハブ抗毒素、ヒト免疫グロブリンなどの生物製剤、ペニシリン、エリスロマイシン、クロラムフェニコール、テトラサイクリン、スプレプトマイシン、硫酸カナマイシンなどの抗生物質、チアミン、リボフラビン、Ｌ−アスコルビン酸、α−グリコシルアスコルビン酸、肝油、カロチノイド、エルゴステロール、トコフェロール、ルチン、α−グリコシルルチン、ナリンジン、α−グリコシルナリンジン、ヘスペリジン、α−グリコシルヘスペリジンなどのビタミン類、リパーゼ、エラスターゼ、ウロキナーゼ、プロテアーゼ、β−アミラーゼ、イソアミラーゼ、グルカナーゼ、ラクターゼなどの酵素、薬用人参エキス、笹エキス、梅エキス、松エキス、スッポンエキス、クロレラエキス、アロエエキス、プロポリスエキスなどのエキス類、ウイルス、乳酸菌、酵母などの生菌、ローヤルゼリーなどを例示することができる。   The β-maltose hydrous crystal-containing powder of the present invention is a stable, high-quality liquid by blending it into health foods, pharmaceuticals, etc. containing active ingredients, active ingredients or bioactive substances as quality improvers and / or stabilizers. A paste-like or solid health food or medicine can be obtained. Examples of the active ingredient and physiologically active substance include interferon-α, interferon-β, interferon-γ, TNF-α, TNF-β, macrophage migration inhibitory factor, colony stimulating factor, transfer factor, lymphokine such as interleukin, Hormones such as insulin, growth hormone, prolactin, erythropoietin, egg cell stimulating hormone, BCG vaccine, Japanese encephalitis vaccine, measles vaccine, polio vaccine, seedling, tetanus toxoid, hub antitoxin, human immunoglobulin and other biologics, penicillin, erythromycin Antibiotics such as chloramphenicol, tetracycline, sprepomycin, kanamycin sulfate, thiamine, riboflavin, L-ascorbic acid, α-glycosyl ascorbic acid, Oils, carotenoids, ergosterol, tocopherol, rutin, α-glycosylrutin, naringin, α-glycosylnarindine, hesperidin, α-glycosylhesperidin and other vitamins, lipase, elastase, urokinase, protease, β-amylase, isoamylase, glucanase , Enzymes such as lactase, ginseng extract, potato extract, plum extract, pine extract, suppon extract, chlorella extract, aloe extract, propolis extract, etc., live bacteria such as viruses, lactic acid bacteria, yeast, royal jelly, etc. be able to.

以上述べた各種組成物に、本発明のβ−マルトース含水結晶含有粉末を含有させる方法は、これらの組成物が完成するまでの工程で含有させればよく、例えば、混和、溶解、融解、浸漬、浸透、散布、塗布、被覆、噴霧、注入、晶出、固化など公知の方法が適宜選ばれる。その量は、通常、前記組成物重量当たり、１％以上、好ましくは、２％以上、より好ましくは、５乃至９９％配合するのが好適である。   The above-described method for adding the β-maltose hydrous crystal-containing powder of the present invention to the various compositions may be included in the process until these compositions are completed, for example, mixing, dissolution, melting, and immersion. Well-known methods such as permeation, spraying, coating, coating, spraying, pouring, crystallization and solidification are appropriately selected. The amount is usually 1% or more, preferably 2% or more, more preferably 5 to 99%, based on the weight of the composition.

以下、本発明を具体的な実験を用いて詳しく説明する。   Hereinafter, the present invention will be described in detail using specific experiments.

〈実験：各種β−マルトース結晶含有粉末の物性に及ぼす原料糖組成の影響〉
噴霧方式による、各種β−マルトース結晶含有粉末の物性に及ぼす原料糖組成の影響を調べた。試験用粉末は、糖組成の異なる各種の原料マルトース含有溶液を調製し、これを噴霧方式でβ−マルトース含水結晶含有粉末としたものを用いた。マルトース含有溶液は、市販の精製マルトース（（株）林原商事販売 登録商標「サンマルトＳ」）、又は、この精製マルトースにグルコース（和光純薬（株）販売 試薬特級）、マルトトリオース、マルトテトラオース及び／又はマルトペンタオース（いずれも（株）林原生物化学研究所製造 試薬）を加えて各種組成のマルトース含有溶液を調製した。 <Experiment: Effect of raw sugar composition on physical properties of various β-maltose crystal-containing powders>
The effect of the raw sugar composition on the physical properties of various β-maltose crystal-containing powders by the spray method was investigated. As the test powder, various raw material maltose-containing solutions having different sugar compositions were prepared and used as a powder containing β-maltose hydrous crystals by a spray method. Maltose-containing solutions are commercially available purified maltose (registered trademark “Sanmalto S”, sold by Hayashibara Shoji Co., Ltd.), or glucose (reagent grade sold by Wako Pure Chemical Industries, Ltd.), maltotriose, maltotetraose. And / or maltopentaose (all are reagents manufactured by Hayashibara Biochemical Laboratories Co., Ltd.) to prepare maltose-containing solutions of various compositions.

噴霧方式によるβ−マルトース含水結晶含有粉末の調製は次の通り行った。即ち、原料のマルトース含有溶液を水分２５％に濃縮したのち助晶機に移し、種晶としてβ−マルトース含水結晶を１％加え、ゆっくり攪拌しながら、温度を徐々に３０℃まで低下させ、１２乃至１８時間かけてβ−マルトース含水結晶を部分的に晶出させ、マスキットを得た。マスキットの晶出率は３６乃至４３％であった。助晶を終了した後、マスキットの粘度が５０，０００ｃｐを超えるものについては、高圧ポンプで送液する前に加温し、晶出率を実質的に低減させることなく約４５，０００ｃｐに粘度を下げるとともに、加圧ノズルを用いて噴霧した。噴霧時の乾燥用熱風の温度は７５℃、熱風の送風方式は噴霧乾燥機内で垂直下降流、送風空気量は噴霧乾燥機内から取出した時の乾燥粉末の水分が約８．５％となるように調節した。   Preparation of the β-maltose hydrous crystal-containing powder by a spraying method was performed as follows. That is, after concentrating the raw material maltose-containing solution to a water content of 25%, it was transferred to an auxiliary crystal machine, and 1% of β-maltose water-containing crystal was added as a seed crystal, and the temperature was gradually lowered to 30 ° C. while slowly stirring. Β-maltose hydrous crystals were partially crystallized over a period of 18 hours to obtain a mass kit. The crystallization rate of the mass kit was 36 to 43%. After the auxiliary crystal is finished, if the viscosity of the mass kit exceeds 50,000 cp, heat it before sending it with a high-pressure pump, and increase the viscosity to about 45,000 cp without substantially reducing the crystallization rate. While lowering, spraying was performed using a pressure nozzle. The temperature of the hot air for drying at the time of spraying is 75 ° C, the hot air blowing method is a vertical downward flow in the spray dryer, and the amount of blown air is such that the moisture of the dry powder when taken out from the spray dryer is about 8.5% Adjusted.

得られた粉末は、直ちに、種晶としてα−マルトース無水結晶０．２％と混合接触せしめ、温度９０℃、相対湿度（ＲＨ）２０％の恒温恒湿機内で２時間保存し、次いで、３０℃、相対湿度（ＲＨ）８０％の恒温恒湿機内で５時間保持し、熟成を行ってβ−マルトース含水結晶含有粉末を得た。この粉末を、次に述べる各種物性試験に供した。   The obtained powder was immediately mixed and contacted with 0.2% anhydrous α-maltose crystals as seed crystals, stored for 2 hours in a constant temperature and humidity machine at a temperature of 90 ° C. and a relative humidity (RH) of 20%, and then 30 It was kept for 5 hours in a constant temperature and humidity machine at 80 ° C. and a relative humidity (RH) and aged to obtain a β-maltose hydrous crystal-containing powder. This powder was subjected to various physical property tests described below.

物性試験には、対照として、精製マルトース（（株）林原商事販売 登録商標「サンマルトＳ」）、試薬β−マルトース含水結晶（（株）林原生物化学研究所製造 商品名「マルトースＨＨＨ」）及びα−マルトース無水結晶（（株）林原商事販売 登録商標「ファイントース」）を用いた。   In the physical property test, purified maltose (registered trademark “Sanmalto S”, traded by Hayashibara Corporation), hydrated reagent β-maltose crystal (manufactured by Hayashibara Biochemical Laboratories, Inc., trade name “Maltose HHH”) and α were used as controls. -Anhydrous maltose crystal (registered trademark "Fine Tose" sold by Hayashibara Shoji Co., Ltd.) was used.

物性試験は次のような方法で行った。
Ａ．糖組成分析は、ＫＳ−８０１カラム（昭和電工製）またはＣＨ０４ＳＳカラム（ＭＣＩ製）を用いた液体クロマトグラフィーを行い、クロマトグラムの面積比より糖組成を求めた。 The physical property test was conducted by the following method.
A. In the sugar composition analysis, liquid chromatography using a KS-801 column (manufactured by Showa Denko) or a CH04SS column (manufactured by MCI) was performed, and the sugar composition was determined from the area ratio of the chromatogram.

Ｂ．吸湿性試験は、アルミカップに入れた試料の蓋をしないで、ＲＨ７５．２％（飽和塩化ナトリウム水溶液で平衡化）に調整したデシケーター内に入れ、２５℃で３日間放置したのち、重量変化を測定し、元のサンプル対する重量増加の割合（％）を求め、吸湿性とした。   B. In the hygroscopicity test, the sample placed in the aluminum cup is not covered, placed in a desiccator adjusted to 75.2% RH (equilibrated with a saturated sodium chloride aqueous solution), and left at 25 ° C. for 3 days. Measurement was made to determine the rate of weight increase (%) with respect to the original sample, and it was defined as hygroscopicity.

Ｃ．固着性は、吸湿性試験で３日間放置後取り出したアルミカップ内の試料の状態を肉眼観察し、試料が試験前と比べて吸湿したことにより固まっておれば、固着性有りとした。   C. The sticking property was determined to be sticky if the sample in the aluminum cup taken out after being left for 3 days in the hygroscopic test was visually observed and solidified as a result of the sample absorbing moisture compared to before the test.

Ｄ．溶解性試験は、（ｉ）水に対する溶解性試験としては、２５℃の脱イオン水５ｍｌをプラスチック製試験管に入れ、これに各種糖組成のマルトース結晶含有粉末１ｇを一度に加え、粉末が完全に水中に沈んだ状態で密栓し、これを５０℃の恒温槽中で保持し、粉末の溶解状態を２０分毎に肉眼観察した。評価は、粉末が完全溶解し、透明になるまでに要する時間（分）を求めた。評価の基準は、粉末が溶けて見えなくなるまでの時間が短いものほど溶解性に優れると判断した。   D. The solubility test is as follows: (i) As a solubility test in water, 5 ml of deionized water at 25 ° C. is put in a plastic test tube, and 1 g of maltose crystal-containing powder having various sugar compositions is added to the solution at a time. The tube was sealed in a state of being submerged in water, held in a thermostatic bath at 50 ° C., and the dissolved state of the powder was visually observed every 20 minutes. In the evaluation, the time (minutes) required until the powder was completely dissolved and became transparent was determined. As a criterion for evaluation, it was judged that the shorter the time until the powder disappears, the better the solubility.

（ｉｉ）デキストリン含有溶液に対する溶解性試験としては、粘性を有する濃度１７％のデキストリン（（株）松谷化学工業製造 商品名「パインデックス＃１」）水溶液５ｍｌをプラスチック製試験管に入れ、これに各種糖組成のマルトース結晶含有粉末１ｇを前記（ｉ）の水に対する溶解性試験の場合と同様に加え、粉末が完全に水中に沈んだ状態で密栓し、これを５０℃の恒温槽中で保持し、粉末の状態を肉眼観察した。評価の基準は前記（ｉ）の水に対する溶解性試験の場合と同様とした。   (Ii) As a solubility test for a dextrin-containing solution, 5 ml of a dextrin having a viscosity of 17% (manufactured by Matsutani Chemical Industry Co., Ltd., “Paindex # 1”) in an aqueous solution is placed in a plastic test tube. Add 1 g of maltose crystal-containing powder with various sugar compositions in the same manner as in the water solubility test of (i) above, seal the powder completely in water, and hold it in a thermostat at 50 ° C. Then, the state of the powder was visually observed. The standard of evaluation was the same as in the case of the solubility test in water of (i) above.

Ｅ．マルトース異性体の分析は、試料を無水ピリジンに溶解後、ＴＭＳ化処理を行って、２％ＯＶ−１７ クロモソルブＷ（ＡＷ−ＤＭＣＳ）を用いたガスクロマトグラフィーを行い、クロマトグラムの面積比よりα、β−アノマー比を求めた。   E. For analysis of maltose isomers, the sample was dissolved in anhydrous pyridine, TMS-treated, gas chromatography using 2% OV-17 chromosolve W (AW-DMCS) was performed, and α was determined from the area ratio of the chromatogram. , Β-anomeric ratio was determined.

Ｆ．粉末の結晶化度の測定は、Ｘ線回折装置ガイガーフレックスＲＤＡ−ＩＩＢ（Ｃｕ、Ｋα線使用）（理学電気（株）製）を用いて、粉末Ｘ線回折図形に基づくルーランド（Ｒｕｌａｎｄ）の方法（アクタ クリスクログラフィカ：Ａｃｔａ Ｃｒｙｓｔａｌｌｏｇｒａｐｈｉｃａ、第１４巻、第１１８０頁、１９６１年）により求めた。測定した粉末のうち、代表的な粉末Ｘ線回折図形を図１乃至図５に示した。   F. The measurement of the crystallinity of the powder was carried out using the X-ray diffractometer Geiger Flex RDA-IIB (using Cu and Kα rays) (manufactured by Rigaku Denki Co., Ltd.). (Acta Crystallographica: Acta Crystallographica, Vol. 14, page 1180, 1961). Among the measured powders, typical powder X-ray diffraction patterns are shown in FIGS.

原料のマルトース含有溶液の糖組成及び得られた各粉末の吸湿性、固着性、溶解性、α−アノマー含量、結晶化度についての試験結果は、各種マルトース結晶含有粉末の物性として表１にまとめた。   The sugar composition of the raw material maltose-containing solution and the test results on the hygroscopicity, stickiness, solubility, α-anomer content, and crystallinity of each powder obtained are summarized in Table 1 as the physical properties of various maltose crystal-containing powders. It was.

Figure 0003746064
Figure 0003746064

表１から明らかなように、試験Ｎｏ．３乃至６の噴霧方式で得られた、無水物換算で、マルトース８６％以上９３％未満及びグルコース２％以上を含有し、他の糖質として、マルトトリオース及びグルコース重合度４以上のオリゴ糖を含有し、マルトース異性体としてマルトース中のα−アノマーを７％以上１４％未満含有する結晶化度が６２％以上７２％未満のβ−マルトース含水結晶含有粉末は、吸湿性が低く、固着性が見られず保存安定性良好、取扱い容易で、しかも、水及び粘性を有するデキストリン含有溶液などの水系媒体への溶解性に優れていることが判明した。これに対して、試験Ｎｏ．１及び２のマルトース含量が８２．４％及び８４．２％と低く、マルトース異性体としてマルトース中のα−アノマー含量が１４％を越える結晶化度が６２％未満の噴霧方式で得られたβ−マルトース含水結晶含有粉末は、水系媒体への溶解性に優れているものの吸湿性が高く、固着性を示し、保存安定性に劣る不安定な粉末であった。   As is apparent from Table 1, test no. Oligosaccharides containing maltotriose 86% or more and less than 93% and glucose 2% or more obtained by spraying method 3 to 6 as malt triose and glucose polymerization degree 4 or more as other saccharides The β-maltose hydrous crystal-containing powder having a crystallinity of 62% or more and less than 72% containing 7% or more and less than 14% of the α-anomer in the maltose as a maltose isomer has low hygroscopicity and adhesion. No storage was observed, it was found that the storage stability was good, the handling was easy, and the solubility in an aqueous medium such as a dextrin-containing solution having water and viscosity was excellent. In contrast, test no. 1 and 2 having a maltose content as low as 82.4% and 84.2%, and β obtained by a spray system in which the α-anomer content in maltose as maltose isomer exceeds 14% and the crystallinity is less than 62%. -The maltose hydrous crystal-containing powder was an unstable powder that was excellent in solubility in an aqueous medium but had high hygroscopicity, high stickiness, and poor storage stability.

一方、試験Ｎｏ．１のマルトース含量が９４．１％と高く、マルトース異性体としてマルトース中のα−アノマー含量が７％以下と少なく、結晶化度が７２％を越える噴霧方式で得られたβ−マルトース含水結晶含有粉末は、吸湿性が少なく、固着性がないものの、水系媒体への溶解性に劣る粉末であった。   On the other hand, test no. The maltose content of 1 is as high as 94.1%, the α-anomer content in maltose is as low as 7% or less as maltose isomers, and β-maltose hydrous crystals are obtained by spraying with a crystallinity exceeding 72%. The powder was poor in solubility in an aqueous medium, although it had little hygroscopicity and no stickiness.

なお、対照として用いた試験Ｎｏ．８の「サンマルトＳ」は、噴霧方式で得られた粉末である。しかしながら、マルトース純度が９５．０％、結晶化度７４．５％といずれも高く、吸湿性がほとんどなく、固着性も全くないものの、水系媒体への溶解性に劣るものであった。また、試験Ｎｏ．９の「マルトースＨＨＨ」は、マスキットを分蜜して得られた結晶粉末である。本粉末はきわめて高純度のマルトースであって、マルトース純度が９９．６％、結晶化度も８２．６％と高く、吸湿性がほとんどなく、固着性も全く示さないものの、水系媒体への溶解性に劣るものであった。更に、試験Ｎｏ．１０の「ファイントース」は、他の試料と異なって、α−マルトース無水結晶粉末である。本粉末はマルトース中のα−アノマー含量が高く、粉末が示す性質はβ−マルトース含水結晶を主とする他の粉末とは大きく異なっており、結晶化度の違いにかかわらず、吸湿性が高く、固着性も激しく、保存安定性に劣る不安定な粉末であり、その上、水系媒体への溶解性に劣るものであった。   In addition, test No. used as a control. “Sanmalto S” of 8 is a powder obtained by a spray method. However, the maltose purity was 95.0% and the crystallinity was 74.5%, both of which had little hygroscopicity and no sticking property, but were poor in solubility in aqueous media. In addition, Test No. No. 9 “Maltose HHH” is a crystalline powder obtained by honeying a mass kit. This powder is a very high-purity maltose, having a high maltose purity of 99.6% and a crystallinity of 82.6%, almost no hygroscopicity and no stickiness, but soluble in an aqueous medium. It was inferior in nature. Furthermore, test no. No. 10 “Fine Tose” is an α-maltose anhydrous crystal powder, unlike the other samples. This powder has a high α-anomer content in maltose, and the properties of the powder are significantly different from other powders mainly composed of β-maltose hydrous crystals, and it has high hygroscopicity regardless of the crystallinity. Further, the powder is unstable and has an inferior storage stability, and also has poor solubility in an aqueous medium.

以上の結果から、噴霧方式によるβ−マルトース結晶含有粉末の製造においては、無水物換算で、マルトース８６％以上９３％未満及びグルコース２％以上を含有している溶液を原料とし、本発明の一連の製造方法に従って製造すると、水系媒体への溶解性に優れ、取扱いの容易なβ−マルトース結晶含有粉末を得ることができることが判明した。   From the above results, in the production of the β-maltose crystal-containing powder by the spray method, a solution containing maltose 86% or more and less than 93% and glucose 2% or more in terms of anhydride is used as a raw material. It was found that a β-maltose crystal-containing powder having excellent solubility in an aqueous medium and easy to handle can be obtained by the production according to this production method.

従って、本発明を採用することにより得られる、無水物換算で、マルトース８６％以上９３％未満及びグルコース２％以上を含有し、結晶化度が６２％以上７２％未満であるβ−マルトース結晶含有粉末は、水系媒体への溶解性に優れ、取扱い容易で、しかも高収率に製造できるのに加え、これまでと比較して、水系媒体に溶解して使用するときの作業時間を大幅に短縮することができ、産業上もきわめて価値の高いものといえる。   Therefore, containing β-maltose crystals containing maltose of 86% or more and less than 93% and glucose of 2% or more and having a crystallinity of 62% or more and less than 72% in terms of anhydride, obtained by employing the present invention. Powders have excellent solubility in aqueous media, are easy to handle, and can be manufactured in high yields. In addition, compared to conventional powders, the work time when dissolved in aqueous media is greatly reduced. It can be said that it is extremely valuable industrially.

以下に、具体的な実施例を挙げて本発明をさらに詳しく説明するが、本発明はこれらの実施例によって限定されるものではない。   Hereinafter, the present invention will be described in more detail with reference to specific examples, but the present invention is not limited to these examples.

＜マルトース含有溶液の調製＞
馬鈴薯澱粉１質量部と水４質量部との懸濁液に市販の細菌液化型α−アミラーゼ（スピターゼＨＳ 長瀬産業（株）製）を加え９０℃に昇温し、加熱糊化したのち、直ちに１３０℃に加熱して酵素反応を止め、ＤＥ１．８の液化液を得た。この澱粉液化液を５５℃まで急冷し、澱粉枝切り酵素（シュードモナス菌を培養して調製したイソアミラーゼ）を澱粉１ｇ当たり１００単位および大豆由来のβアミラーゼ（商品名＃１５００ 長瀬産業（株）製）を澱粉１ｇ当たり５０単位、更に、マルトゲナーゼ（ノボ ノルディスク（株）製）を糖質１ｇ当たり１０単位加え加えｐＨ５．０に保って４０時間糖化した。これを、常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行って精製し、減圧濃縮してマルトース含有溶液を得た。マルトース含有溶液の糖組成は、グルコース３．８％、マルトース９２．５％、マルトトリオース１．１％、マルトテトラオース以上２．６％であった。 <Preparation of maltose-containing solution>
Immediately after adding a commercially available bacterial liquefied α-amylase (Spytase HS manufactured by Nagase Sangyo Co., Ltd.) to a suspension of 1 part by weight of potato starch and 4 parts by weight of water, heating to 90 ° C. The enzyme reaction was stopped by heating to 130 ° C. to obtain a liquefied liquid of DE1.8. This starch liquefied liquid is rapidly cooled to 55 ° C., and starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacteria) is 100 units per 1 g of starch and soybean-derived β-amylase (trade name # 1500, manufactured by Nagase Sangyo Co., Ltd.) ) Was added at 50 units per gram of starch, and 10 units of maltogenase (manufactured by Novo Nordisk Co., Ltd.) per gram of saccharide was added to maintain the pH at 5.0 and saccharified for 40 hours. This was purified by decolorization by activated carbon treatment and desalting by ion exchange resin treatment according to conventional methods, and concentrated under reduced pressure to obtain a maltose-containing solution. The sugar composition of the maltose-containing solution was 3.8% glucose, 92.5% maltose, 1.1% maltotriose, and 2.6% maltotetraose or higher.

＜β−マルトース含水結晶含有粉末の調製＞
実施例１で得られたマルトース含有溶液を水分２９％に濃縮したのち助晶缶に移し、種晶としてβ−マルトース含水結晶を１％加え、ゆっくり攪拌しながら、マスキットの温度を徐々に２９℃まで低下させ、１２時間かけてβ−マルトース含水結晶を部分的に晶出させた。マスキットの晶出率は３７％となった。助晶終了後のマスキットを高圧ポンプで送液し、回転円盤を用いて噴霧乾燥機内に噴霧した。このときの乾燥用熱風の温度は７０℃、熱風の送風は噴霧乾燥機内で垂直下降並流、送風空気量は噴霧乾燥機内から取出し時の乾燥粉末の水分が７．５％となるように調節した。 <Preparation of β-maltose hydrous crystal-containing powder>
The maltose-containing solution obtained in Example 1 was concentrated to a moisture content of 29% and transferred to an auxiliary crystal can. 1% of β-maltose hydrous crystals were added as seed crystals, and the temperature of the mass kit was gradually increased to 29 ° C. while stirring slowly. The hydrated β-maltose crystal was partially crystallized over 12 hours. The crystallization rate of Muskit was 37%. After completion of the auxiliary crystal, the mass kit was fed with a high-pressure pump and sprayed into a spray dryer using a rotating disk. At this time, the temperature of the hot air for drying is 70 ° C., the blowing of the hot air is adjusted in the vertical descent in the spray dryer, and the amount of blown air is adjusted so that the moisture content of the dry powder when taken out from the spray dryer is 7.5%. did.

この粉末を直ちにα−マルトース無水結晶０．２％と混合接触させ、温度８５℃、相対湿度（ＲＨ）２０％で３時間保持し、次いで、３０℃、相対湿度（ＲＨ）８０％で５時間保持し熟成を行って、結晶化度が７１．４％、水分６．１％のβ−マルトース含水結晶含有粉末を、原料の馬鈴薯澱粉に対し、無水物換算で、収率９６％で得た。本粉末は、無水物換算で、マルトース９２．５％とともに、グルコース３．８％、マルトトリオース１．１％及びグルコース重合度４以上のオリゴ糖２．６％を含有し、しかも、マルトース異性体としてマルトース中のα−アノマーを７．８％含有しているもので、水系媒体への溶解性に優れていた。しかも、２５℃、相対湿度（ＲＨ）７５．２％の条件下で保存してもほとんど吸湿性を示さず、保存安定性に優れ、流動性良好で、取扱い容易な粉末であった。また、本粉末の粒度分布を測定した結果、粒子中に微粒子が凝集した粉末を含み、１５０μｍ以上３００μｍ以下の粒子が４１％含まれていた。   This powder was immediately mixed and contacted with 0.2% anhydrous α-maltose crystals, held at a temperature of 85 ° C. and a relative humidity (RH) of 20% for 3 hours, and then at 30 ° C. and a relative humidity (RH) of 80% for 5 hours. Holding and ripening, a β-maltose hydrous crystal-containing powder having a crystallinity of 71.4% and a moisture content of 6.1% was obtained with a yield of 96% in terms of anhydride relative to the raw material potato starch. . This powder contains, in terms of anhydride, 92.5% maltose, 3.8% glucose, 1.1% maltotriose, and 2.6% oligosaccharide having a glucose polymerization degree of 4 or more, and maltose isomerism. It contained 7.8% α-anomer in maltose as a body and was excellent in solubility in an aqueous medium. Moreover, even when stored under the conditions of 25 ° C. and relative humidity (RH) 75.2%, it hardly showed hygroscopicity, had excellent storage stability, good fluidity, and was easy to handle. Further, as a result of measuring the particle size distribution of the present powder, it was found that 41% of particles having a particle size of 150 μm or more and 300 μm or less were included, including a powder in which fine particles aggregated.

また、本粉末は、甘味料、呈味改良剤、品質改良剤、安定剤、変色防止剤、増量剤、賦形剤、結合剤などとして、とりわけ、水系媒体への溶解性に優れているので、例えば、水のみならず、ペースト状、半固状物などに溶解、含有せしめて、飲食物、嗜好物、飼料、餌料、化粧品、医薬品などの各種組成物に有利に利用できる。更に、そのままで、または必要に応じて、増量剤、賦形剤、結合剤などと混合して、顆粒、球状、短棒状、板状、立方体、錠剤など各種形状に成形して使用することも随意である。   In addition, the powder is excellent in solubility in an aqueous medium, especially as a sweetener, taste improver, quality improver, stabilizer, anti-discoloring agent, extender, excipient, binder, etc. For example, it can be dissolved and contained not only in water but also in a paste or semi-solid material, and can be advantageously used in various compositions such as foods and drinks, foods, feeds, foods, cosmetics, and pharmaceuticals. Further, it can be used as it is or mixed with a bulking agent, excipient, binder, etc., and shaped into various shapes such as granules, spheres, short bars, plates, cubes, tablets, etc. Is voluntary.

＜マルトース含有溶液の調製＞
コーンスターチ１質量部と水３質量部との懸濁液に市販の細菌液化型α−アミラーゼ（スピターゼＨＳ 長瀬産業（株）製）を加え９０℃に昇温し、加熱糊化したのち直ちに１３０℃に加熱して酵素反応を止め、ＤＥ２．５の液化液を得た。この澱粉液化液を５５℃まで急冷し、澱粉枝切り酵素（シュードモナス菌を培養して調製したイソアミラーゼ）を澱粉１ｇ当たり５０単位および大豆由来のβアミラーゼ（商品名＃１５００ 長瀬産業（株）製）を同じく２０単位加えｐＨ５．０に保って４０時間糖化し、マルトース含量が固形物当たり８４．６％の高純度マルトース含有糖化液を得た。マルトース含有糖化液の糖組成は、グルコース３．５％、マルトース８４．６％、マルトトリオース８．２％、マルトテトラオース以上３．７％であった。 <Preparation of maltose-containing solution>
A commercially available bacterial liquefied α-amylase (Spytase HS manufactured by Nagase Sangyo Co., Ltd.) was added to a suspension of 1 part by weight of corn starch and 3 parts by weight of water, the temperature was raised to 90 ° C, and gelatinized by heating to 130 ° C immediately. The enzyme reaction was stopped by heating to a DE2.5 liquefied solution. This starch liquefied liquid is rapidly cooled to 55 ° C., and starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacteria) is 50 units per 1 g of starch and β-amylase derived from soybean (trade name # 1500, manufactured by Nagase Sangyo Co., Ltd.) ) Was added in the same manner, and saccharified for 40 hours while maintaining the pH at 5.0 to obtain a high-purity maltose-containing saccharified solution having a maltose content of 84.6% per solid. The sugar composition of the maltose-containing saccharified solution was 3.5% glucose, 84.6% maltose, 8.2% maltotriose, and 3.7% or more maltotetraose.

この糖化液に、更に、タカアミラーゼＡを糖質１ｇ当たり５０単位加えｐＨ５．５に保って、更に２０時間、酵素反応を進めた。これを常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行い精製し、減圧濃縮してマルトース含有溶液を得た。マルトース含有溶液の糖組成は、グルコース５．６％、マルトース９１．２％、マルトトリオース１．３％、マルトテトラオース以上１．９％であった。   To this saccharified solution, takaamylase A was further added at 50 units per gram of sugar, and the pH was kept at 5.5, and the enzyme reaction was further continued for 20 hours. This was purified by decolorization by activated carbon treatment and desalting by ion exchange resin treatment in accordance with conventional methods, and concentrated under reduced pressure to obtain a maltose-containing solution. The sugar composition of the maltose-containing solution was 5.6% glucose, 91.2% maltose, 1.3% maltotriose, and 1.9% maltotetraose or higher.

＜β−マルトース含水結晶含有粉末の調製＞
実施例３で得られたマルトース含有溶液を水分２６％に濃縮したのち助晶機に移し、種晶としてβ−マルトース含水結晶を１％加え、ゆっくり攪拌しながら、マスキットの温度を徐々に３０℃まで低下させ、１４時間かけてβ−マルトース含水結晶を部分的に晶出させた。マスキットの晶出率は４１％であった。助晶終了後のマスキットを高圧ポンプで送液し、回転円盤を用いて噴霧乾燥機内に噴霧した。乾燥用の熱風の温度は７５℃、熱風の送風は噴霧乾燥機内で垂直下降並流、送風空気量は噴霧乾燥機内から取出し時の乾燥粉末の水分が８．５％となるように調節した。 <Preparation of β-maltose hydrous crystal-containing powder>
After concentrating the maltose-containing solution obtained in Example 3 to a moisture content of 26%, it was transferred to an auxiliary crystallizer, and 1% of a β-maltose hydrous crystal was added as a seed crystal, and the temperature of the mass kit was gradually increased to 30 ° C. while stirring slowly. The hydrated β-maltose crystal was partially crystallized over 14 hours. The crystallization rate of the mass kit was 41%. After completion of the auxiliary crystal, the mass kit was fed with a high-pressure pump and sprayed into a spray dryer using a rotating disk. The temperature of the hot air for drying was 75 ° C., the blowing of the hot air was adjusted in the vertical descent in the spray dryer, and the amount of blown air was adjusted so that the water content of the dry powder when taken out from the spray dryer was 8.5%.

この粉末を直ちにα−マルトース無水結晶０．２％と混合接触させ、温度９０℃、相対湿度（ＲＨ）２５％で２時間保持し、次いで、３０℃、相対湿度（ＲＨ）８０％で５時間保持し熟成を行って、結晶化度７０．４％、水分６．１％のβ−マルトース含水結晶含有粉末を、原料のコーンスターチに対し、無水物換算で、収率９５％で得た。本粉末は、無水物換算で、マルトース９１．２％とともに、グルコース５．６％、マルトトリオース１．３％及びグルコース重合度４以上のオリゴ糖１．９％を含有し、しかも、マルトース異性体としてマルトース中のα−アノマーを９．２％含有しているもので、水系媒体への溶解性に優れていた。しかも、２５℃、相対湿度（ＲＨ）７５．２％の条件下で保存してもほとんど吸湿性を示さず、保存安定性に優れ、流動性良好で、取扱い容易な粉末であった。また、本粉末の粒度分布を測定した結果、粒子中に微粒子が凝集した粉末を含み、１５０μｍ以上３００μｍ以下の粒子が４７％含まれていた。   This powder was immediately mixed and contacted with 0.2% α-maltose anhydrous crystals, kept at a temperature of 90 ° C. and a relative humidity (RH) of 25% for 2 hours, and then at 30 ° C. and a relative humidity (RH) of 80% for 5 hours. This was retained and aged to obtain a β-maltose hydrous crystal-containing powder having a crystallinity of 70.4% and a water content of 6.1% with respect to the raw material corn starch in a yield of 95% in terms of anhydride. This powder contains, in terms of anhydride, 91.2% maltose, 5.6% glucose, 1.3% maltotriose, and 1.9% oligosaccharides having a glucose polymerization degree of 4 or more, and maltose isomerism. It contained 9.2% α-anomer in maltose as a body and was excellent in solubility in an aqueous medium. Moreover, even when stored under the conditions of 25 ° C. and relative humidity (RH) 75.2%, it hardly showed hygroscopicity, had excellent storage stability, good fluidity, and was easy to handle. Further, as a result of measuring the particle size distribution of the present powder, 47% of particles having a particle size of 150 μm or more and 300 μm or less were included, including a powder in which fine particles were aggregated.

また、本粉末は、甘味料、呈味改良剤、品質改良剤、安定剤、変色防止剤、増量剤、賦形剤、結合剤などとして、とりわけ、水系媒体への溶解性に優れているので、例えば、水のみならず、ペースト状、半固状物などに溶解、含有せしめて、飲食物、嗜好物、飼料、餌料、化粧品、医薬品などの各種組成物に有利に利用できる。更に、そのままで、または必要に応じて、増量剤、賦形剤、結合剤などと混合して、顆粒、球状、短棒状、板状、立方体、錠剤など各種形状に成形して使用することも随意である。   In addition, the powder is excellent in solubility in an aqueous medium, especially as a sweetener, taste improver, quality improver, stabilizer, anti-discoloring agent, extender, excipient, binder, etc. For example, it can be dissolved and contained not only in water but also in a paste or semi-solid material, and can be advantageously used in various compositions such as foods and drinks, foods, feeds, foods, cosmetics, and pharmaceuticals. Further, it can be used as it is or mixed with a bulking agent, excipient, binder, etc., and shaped into various shapes such as granules, spheres, short bars, plates, cubes, tablets, etc. Is voluntary.

＜マルトース含有溶液の調製＞
コーンスターチ３質量部と水７質量部との懸濁液に市販の細菌液化型α−アミラーゼ（スピターゼＨＳ 長瀬産業（株）製）を加え９０℃に昇温し、加熱糊化したのち直ちに１３０℃に加熱して酵素反応を止め、ＤＥ４．３の液化液を得た。この澱粉液化液を５５℃まで急冷して澱粉枝切り酵素（シュードモナス菌を培養して調製したイソアミラーゼ）を澱粉１ｇ当たり５０単位、大豆由来のβアミラーゼ（商品名＃１５００ 長瀬産業（株）製）を同じく２０単位を加えｐＨ５．０に保って４０時間糖化し、マルトース含量が固形物当たり８４．６％の糖化液を得た。これを、常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行って精製し、減圧濃縮して糖濃度４５％のマルトース含有溶液を得て、分画原料とした。 <Preparation of maltose-containing solution>
Commercially available bacterial liquefied α-amylase (Spytase HS manufactured by Nagase Sangyo Co., Ltd.) was added to a suspension of 3 parts by mass of corn starch and 7 parts by mass of water, the temperature was raised to 90 ° C., and gelatinized by heating to 130 ° C. immediately. To stop the enzyme reaction to obtain a liquefied liquid of DE4.3. This starch liquefied solution is rapidly cooled to 55 ° C. and starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacteria) is 50 units per 1 g of starch, soybean-derived β-amylase (trade name # 1500, manufactured by Nagase Sangyo Co., Ltd.) ) Was added in the same manner to 20 units, and saccharified for 40 hours while maintaining the pH at 5.0 to obtain a saccharified solution having a maltose content of 84.6% per solid. This was purified by decolorization by activated carbon treatment and desalting by ion exchange resin treatment according to conventional methods, and concentrated under reduced pressure to obtain a maltose-containing solution having a sugar concentration of 45%, which was used as a fraction raw material.

分画に用いた分画用樹脂は、アルカリ金属型強酸性カチオン交換樹脂（東京有機化学工業（株）製 商品名アンバーライトＸＴ−１００７Ｎａ＋型、架橋度６％）を使用し、内径５．４ｃｍのジャケット付ステンレス製カラムに水懸濁液で充填し、糖質溶液が直列に流れるようにカラム２本を連結して樹脂層全長を１０ｍとした。 As the fractionation resin used for fractionation, an alkali metal type strongly acidic cation exchange resin (trade name Amberlite XT-1007Na + type, manufactured by Tokyo Organic Chemical Industry Co., Ltd., having a crosslinking degree of 6%) was used. A stainless steel column with a 4 cm jacket was filled with a water suspension, and two columns were connected so that the saccharide solution flowed in series, so that the total length of the resin layer was 10 m.

カラム内温度を５５℃に維持しつつ、原料の糖質溶液を樹脂に対して５ｖ／ｖ％加え、これに５５℃の温水をＳＶ０．３で流して分画し、マルトトリオース高含有画分を分離、除去して、マルトースを高含有しているとともに他にオリゴ用などを含有しているマルトース高含有画分を採取した。次いで、常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行って精製し、減圧濃縮してマルトース含有溶液を得た。このマルトース含有溶液の糖組成は、グルコース６．０％、マルトース９０．１％、マルトトリオース０．８％、マルトテトラオース以上３．１％であった。   While maintaining the temperature in the column at 55 ° C., the raw material sugar solution was added to the resin at 5 v / v%, and 55 ° C. warm water was fed at SV 0.3 to perform fractionation. The fraction was separated and removed, and a fraction containing a high content of maltose containing a high content of maltose and other oligos was collected. Subsequently, purifying by decolorization by activated carbon treatment and desalting by ion exchange resin treatment in accordance with a conventional method, the solution was concentrated under reduced pressure to obtain a maltose-containing solution. The sugar composition of this maltose-containing solution was 6.0% glucose, 90.1% maltose, 0.8% maltotriose, and 3.1% maltotetraose or higher.

＜β−マルトース含水結晶含有粉末の調製＞
実施例５で得られたマルトース含有溶液を水分２４％に濃縮したのち助晶機に移し、種晶としてβ−マルトース含水結晶を１％加え、ゆっくり攪拌しながら、マスキットの温度を徐々に２９℃まで低下させ、１５時間かけてβ−マルトース含水結晶を部分的に晶出させた。晶出率は４０％であった。助晶終了後のマスキットは粘度が高いため、高圧ポンプで送液時に加温し、晶出率を低減させることなく、約４０，０００ｃｐに粘度を下げるとともに、加圧ノズルを用いて噴霧乾燥機内に噴霧した。このときの乾燥用熱風の温度は７５℃とし、熱風の送風は噴霧乾燥機内で垂直下降並流とし、送風空気量は噴霧乾燥機内から取出し時の乾燥粉末の水分が９．０％となるように調節した。 <Preparation of β-maltose hydrous crystal-containing powder>
The maltose-containing solution obtained in Example 5 was concentrated to a moisture content of 24% and then transferred to an auxiliary crystal machine. 1% of β-maltose hydrous crystals were added as seed crystals, and the temperature of the mass kit was gradually increased to 29 ° C. while stirring slowly. And the β-maltose hydrous crystals were partially crystallized over 15 hours. The crystallization rate was 40%. Since the mass kit after completion of the auxiliary crystallization has a high viscosity, it is heated at the time of feeding with a high-pressure pump, and the viscosity is reduced to about 40,000 cp without reducing the crystallization rate. Sprayed on. At this time, the temperature of the drying hot air is 75 ° C., the hot air is blown vertically downward in the spray dryer, and the amount of air blown is such that the moisture of the dry powder taken out from the spray dryer is 9.0%. Adjusted.

この粉末を直ちにα−マルトース無水結晶０．２％と混合接触させ、温度８５℃、相対湿度（ＲＨ）２０％で２時間保持し、次いで、３５℃、相対湿度（ＲＨ）７５％で５時間保持し熟成を行って、結晶化度が６９．０％、水分６．４％のβ−マルトース含水結晶含有粉末を、原料コーンスターチに対して、無水物換算で、収率８９％で得た。本粉末は、無水物換算で、マルトース９０．１％とともに、グルコース６．０％、マルトトリオース０．８％及びグルコース重合度４以上のオリゴ糖３．１％を含有し、しかも、マルトース異性体としてマルトース中のα−アノマーを９．９％含有しているもので、水系媒体への溶解性に優れていた。しかも、２５℃、相対湿度（ＲＨ）７５．２％の条件下で保存してもほとんど吸湿性を示さず、保存安定性にも優れ、流動性良好で、取扱い容易な粉末である。また、本粉末の粒度分布を測定した結果、粒子中に微粒子が凝集した粉末を含み、１５０μｍ以上３００μｍ以下の粒子が５１％含まれていた。   This powder was immediately mixed and contacted with 0.2% anhydrous α-maltose crystals, held at a temperature of 85 ° C. and a relative humidity (RH) of 20% for 2 hours, and then at 35 ° C. and a relative humidity (RH) of 75% for 5 hours. Holding and aging, a β-maltose hydrous crystal-containing powder having a crystallinity of 69.0% and a water content of 6.4% was obtained with a yield of 89% in terms of anhydride relative to the raw material corn starch. This powder contains, in terms of anhydride, 90.1% maltose, 6.0% glucose, 0.8% maltotriose, and 3.1% oligosaccharide having a glucose polymerization degree of 4 or more, and maltose isomerism. It contained 9.9% α-anomer in maltose as a body and was excellent in solubility in an aqueous medium. Moreover, even when stored under conditions of 25 ° C. and relative humidity (RH) 75.2%, it exhibits almost no hygroscopicity, excellent storage stability, good flowability, and easy handling. Further, as a result of measuring the particle size distribution of the present powder, 51% of particles having a particle size of 150 μm or more and 300 μm or less were included, including a powder in which fine particles aggregated.

また、本粉末は、甘味料、呈味改良剤、品質改良剤、安定剤、変色防止剤、増量剤、賦形剤、結合剤などとして、とりわけ、水系媒体への溶解性に優れているので、例えば、水のみならず、ペースト状、半固状物などに溶解、含有せしめて、飲食物、嗜好物、飼料、餌料、化粧品、医薬品などの各種組成物に有利に利用できる。更に、そのままで、または必要に応じて、増量剤、賦形剤、結合剤などと混合して、顆粒、球状、短棒状、板状、立方体、錠剤など各種形状に成形して使用することも随意である。   In addition, the powder is excellent in solubility in an aqueous medium, especially as a sweetener, taste improver, quality improver, stabilizer, anti-discoloring agent, extender, excipient, binder, etc. For example, it can be dissolved and contained not only in water but also in a paste or semi-solid material, and can be advantageously used in various compositions such as foods and drinks, foods, feeds, foods, cosmetics, and pharmaceuticals. Further, it can be used as it is or mixed with a bulking agent, excipient, binder, etc., and shaped into various shapes such as granules, spheres, short bars, plates, cubes, tablets, etc. Is voluntary.

＜マルトース含有溶液の調製＞
コーンスターチ１質量部と水２質量部との懸濁液に市販の細菌液化型α−アミラーゼ（スピターゼＨＳ 長瀬産業（株）製）を加え９０℃に昇温し、加熱糊化したのち直ちに１３０℃に加熱して酵素反応を止め、ＤＥ４．３の液化液を得た。この澱粉液化液を５５℃まで急冷して澱粉枝切り酵素（シュードモナス菌を培養して調製したイソアミラーゼ）を澱粉１ｇ当たり５０単位、大豆由来のβアミラーゼ（商品名＃１５００ 長瀬産業（株）製）を同じく１０単位加え、ｐＨ５．０に保って４０時間糖化し、マルトース含量が固形物当たり７４．１％の糖化液を得た。これを、常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行って精製し、減圧濃縮して糖濃度４５％のマルトース含有溶液を得て、分画原料とした。 <Preparation of maltose-containing solution>
A commercially available bacterial liquefied α-amylase (Spytase HS manufactured by Nagase Sangyo Co., Ltd.) is added to a suspension of 1 part by weight of corn starch and 2 parts by weight of water, the temperature is raised to 90 ° C., and gelatinized by heating to 130 ° C. immediately. To stop the enzyme reaction, and a liquefied liquid of DE 4.3 was obtained. This starch liquefied solution is rapidly cooled to 55 ° C., and starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacteria) is 50 units per 1 g of starch, soybean-derived β-amylase (trade name # 1500, manufactured by Nagase Sangyo Co., Ltd.) 10 units) and saccharified for 40 hours while maintaining the pH at 5.0 to obtain a saccharified solution having a maltose content of 74.1% per solid. This was purified by decolorization by activated carbon treatment and desalting by ion exchange resin treatment according to conventional methods, and concentrated under reduced pressure to obtain a maltose-containing solution having a sugar concentration of 45%, which was used as a fraction raw material.

分画に用いた分画用樹脂は、アルカリ金属型強酸性カチオン交換樹脂（東京有機化学工業（株）製 商品名アンバーライトＸＴ−１００７Ｎａ＋型、架橋度６％）を使用し、内径５．４ｃｍのジャケット付ステンレス製カラムに水懸濁液で充填し、糖質溶液が直列に流れるようにカラム２本を連結して樹脂層全長を１０ｍとした。 As the fractionation resin used for fractionation, an alkali metal type strongly acidic cation exchange resin (trade name Amberlite XT-1007Na + type, manufactured by Tokyo Organic Chemical Industry Co., Ltd., having a crosslinking degree of 6%) was used. A stainless steel column with a 4 cm jacket was filled with a water suspension, and two columns were connected so that the saccharide solution flowed in series, so that the total length of the resin layer was 10 m.

カラム内温度を５５℃に維持しつつ、原料の糖質溶液を樹脂に対して５ｖ／ｖ％加え、これに５５℃の温水をＳＶ０．３で流して分画し、マルトトリオース高含有画分を分離、除去して、マルトースを高含有しているとともに他にオリゴ用などを含有しているマルトース高含有画分を採取した。次いで、常法に従って、活性炭処理による脱色、イオン交換樹脂処理による脱塩を行って精製し、減圧濃縮してマルトース含有溶液を得た。マルトース含有溶液の糖組成は、グルコース９．８％、マルトース８７．４％、マルトトリオース１．０％、マルトテトラオース以上１．８％であった。   While maintaining the temperature in the column at 55 ° C., the raw material sugar solution was added to the resin at 5 v / v%, and 55 ° C. warm water was fed at SV 0.3 to perform fractionation. The fraction was separated and removed, and a fraction containing a high content of maltose containing a high content of maltose and other oligos was collected. Subsequently, purifying by decolorization by activated carbon treatment and desalting by ion exchange resin treatment in accordance with a conventional method, the solution was concentrated under reduced pressure to obtain a maltose-containing solution. The sugar composition of the maltose-containing solution was 9.8% glucose, 87.4% maltose, 1.0% maltotriose, and 1.8% maltotetraose or higher.

＜β−マルトース含水結晶含有粉末の調製＞
実施例７で得られたマルトース含有溶液を水分２０％に濃縮したのち助晶機に移し、種晶としてβ−マルトース含水結晶を１％加え、ゆっくり攪拌しながら、マスキットの温度を徐々に３２℃まで低下させ、１６時間かけてβ−マルトース含水結晶を部分的に晶出させた。晶出率は３９％となった。助晶終了後のマスキットは粘度が高いために、高圧ポンプで送液時に加温し、晶出率を低減させることなく、約４５，０００ｃｐ以下に粘度を下げるとともに、回転円盤を用いて噴霧乾燥機内に噴霧した。このときの乾燥用熱風の温度は９０℃とし、熱風の送風は噴霧乾燥機内で垂直下降並流とし、送風空気量は噴霧乾燥機内から取出し時の乾燥粉末の水分が９．５％となるように調節した。 <Preparation of β-maltose hydrous crystal-containing powder>
The maltose-containing solution obtained in Example 7 was concentrated to 20% moisture and transferred to an auxiliary crystal machine. 1% of β-maltose hydrous crystals were added as seed crystals, and the temperature of the mass kit was gradually increased to 32 ° C. while stirring slowly. The β-maltose hydrous crystals were partially crystallized over a period of 16 hours. The crystallization rate was 39%. Since the mass kit after completion of the auxiliary crystal has high viscosity, it is heated at the time of feeding with a high-pressure pump, the viscosity is reduced to about 45,000 cp or less without reducing the crystallization rate, and spray drying using a rotating disk. Sprayed into the machine. At this time, the temperature of the hot air for drying is 90 ° C., the blowing of the hot air is a vertical downward co-current flow in the spray dryer, and the amount of blown air is such that the moisture of the dry powder when taken out from the spray dryer is 9.5%. Adjusted.

この粉末を直ちにα−マルトース無水結晶０．２％と混合接触させ、温度９０℃、相対湿度（ＲＨ）２０％で３時間保持し、次いで、３０℃、相対湿度（ＲＨ）８０％で５時間保持し熟成を行って、結晶化度が６４．６％、水分６．８％のβ−マルトース含水結晶含有粉末を、原料のコーンスターチに対し、無水物換算で、収率８０％で得た。本粉末は、無水物換算で、マルトース８７．４％とともに、グルコース９．８％、マルトトリオース１．０％及びグルコース重合度４以上のオリゴ糖１．８％を含有し、しかも、マルトース異性体としてマルトース中のα−アノマーを１２．７％含有しているもので、水系媒体への溶解性に優れていた。しかも、２５℃、相対湿度（ＲＨ）７５．２％の条件下で保存してもほとんど吸湿性を示さず、保温安定性に優れ、流動性良好で、取扱い容易な粉末であった。また、本粉末の粒度分布を測定した結果、粒子中に微粒子が凝集した粉末を含み、１５０μｍ以上３００μｍ以下の粒子が５３％含まれていた。   This powder was immediately mixed and contacted with 0.2% α-maltose anhydrous crystals, held at a temperature of 90 ° C. and a relative humidity (RH) of 20% for 3 hours, and then at 30 ° C. and a relative humidity (RH) of 80% for 5 hours. This was retained and aged to obtain a β-maltose hydrous crystal-containing powder having a crystallinity of 64.6% and a water content of 6.8%, based on the raw material corn starch, in an yield of 80% in terms of anhydride. This powder contains, in terms of anhydride, 87.4% maltose, 9.8% glucose, 1.0% maltotriose, and 1.8% oligosaccharides having a glucose polymerization degree of 4 or more, and maltose isomerism. It contained 12.7% α-anomer in maltose as a body and was excellent in solubility in an aqueous medium. Moreover, even when stored under the conditions of 25 ° C. and relative humidity (RH) 75.2%, it hardly showed hygroscopicity, had excellent heat retention stability, good fluidity, and was easy to handle. Further, as a result of measuring the particle size distribution of the present powder, 53% of particles having a particle size of 150 μm or more and 300 μm or less were included, including a powder in which fine particles aggregated.

また、本粉末は、甘味料、呈味改良剤、品質改良剤、安定剤、変色防止剤、増量剤、賦形剤、結合剤などとして、とりわけ、水系媒体への溶解性に優れているので、例えば、水のみならず、ペースト状、半固状物などに溶解、含有せしめて、飲食物、嗜好物、飼料、餌料、化粧品、医薬品などの各種組成物に有利に利用できる。更に、そのままで、または必要に応じて、増量剤、賦形剤、結合剤などと混合して、顆粒、球状、短棒状、板状、立方体、錠剤など各種形状に成形して使用することも随意である。   In addition, the powder is excellent in solubility in an aqueous medium, especially as a sweetener, taste improver, quality improver, stabilizer, anti-discoloring agent, extender, excipient, binder, etc. For example, it can be dissolved and contained not only in water but also in a paste or semi-solid material, and can be advantageously used in various compositions such as foods and drinks, foods, feeds, foods, cosmetics, and pharmaceuticals. Further, it can be used as it is or mixed with a bulking agent, excipient, binder, etc., and shaped into various shapes such as granules, spheres, short bars, plates, cubes, tablets, etc. Is voluntary.

＜甘味料＞
実施例２の方法で得たβ−マルトース含水結晶含有粉末０．５質量部、ソルビトール無水結晶０．５質量部、α−グリコシルステビオシド（東洋精糖（株）販売登録商標「αＧスイート」）０．０１質量部及びＬ−アスパルチル−Ｌ−フェニルアラニンメチルエステル（味の素（株）社販売 登録商標「アスパルテーム」）０．０１質量部を均一に混合し、顆粒成型機にかけて、顆粒状甘味料を得た。本品は、甘味の質が優れ、蔗糖の約２倍の甘味度を有し、実質的に低カロリーである。本甘味料は、それに配合した高甘味度甘味物の分解もなく、安定性に優れており、低カロリー甘味料として、カロリー摂取を制限している肥満者、糖尿病者などのための低カロリー飲食物などに対する甘味付けに好適である。また、本甘味料は、虫歯誘発菌による酸の生成が少なく、不溶性グルカンの生成も少ないことより、虫歯を抑制する飲食物などに対する甘味付けにも好適である。 <Sweetener>
0.5 parts by weight of β-maltose hydrous crystal-containing powder obtained by the method of Example 2, 0.5 part by weight of anhydrous sorbitol crystals, α-glycosyl stevioside (Toyo Seika Co., Ltd., registered trademark “αG Sweet”) 01 parts by mass and 0.01 parts by mass of L-aspartyl-L-phenylalanine methyl ester (Ajinomoto Co., Ltd., registered trademark “Aspartame”) were mixed uniformly and applied to a granule molding machine to obtain a granular sweetener. This product has excellent sweetness quality, has about twice the sweetness of sucrose, and is substantially low in calories. This sweetener has no degradation of the high-sweetness sweetener blended in it, has excellent stability, and as a low-calorie sweetener, it is a low-calorie food and drink for obese and diabetics who restrict caloric intake. Suitable for sweetening products. In addition, the present sweetener is suitable for sweetening foods and the like that suppress dental caries because it produces less acid by caries-inducing bacteria and produces less insoluble glucan.

＜ハードキャンディー＞
蔗糖５０質量部と実施例４の方法で得たβ−マルトース含水結晶含有粉末５０質量部を水１００質量部に溶解、加熱混合し、次いで減圧下で水分２％未満になるまで加熱濃縮し、これにクエン酸０．６質量部及び適量のレモン香料と着色料とを混和し、常法に従って成形し、製品を得た。本品は歯切れ、色調、呈味、風味とも良好で、蔗糖の晶出も起こさず、吸湿性少なく、ダレも起こさない安定で高品質のハードキャンディーである。 <Hard candy>
50 parts by mass of sucrose and 50 parts by mass of the β-maltose hydrous crystal-containing powder obtained by the method of Example 4 were dissolved in 100 parts by mass of water, heated and mixed, and then heated and concentrated under reduced pressure until the water content was less than 2%. This was mixed with 0.6 parts by mass of citric acid and an appropriate amount of lemon flavor and coloring agent, and molded according to a conventional method to obtain a product. This product is a stable, high-quality hard candy that has good crispness, color, taste, and flavor, does not cause sucrose crystallization, has low hygroscopicity, and does not cause dripping.

＜チューインガム＞
ガムベース３質量部を柔らかくなる程度に加熱溶融し、これに無水結晶マルチトール（（株）林原商事販売 登録商標「マビット」）２質量部、キシリトール２質量部、実施例６の方法で得たβ−マルトース含水結晶含有粉末２質量部、及び含水結晶トレハロース（（株）林原商事販売 登録商標「トレハ」）１質量部を加え、更に適量の香料と着色料とを混合し、常法に従って、ロールにより練り合わせ、成形、包装して製品を得た。本品は、テクスチャー、呈味、風味良好で、低う蝕性、低カロリーのチューインガムとして好適である。 <Chewing gum>
3 parts by weight of a gum base was heated and melted to a degree of softening, and then 2 parts by weight of anhydrous crystalline maltitol (trademark “Mabit” sold by Hayashibara Corporation), 2 parts by weight of xylitol, β obtained by the method of Example 6 -Add 2 parts by weight of maltose water-containing crystal-containing powder and 1 part by weight of water-containing crystal trehalose (trademark “Trehha”, Hayashibara Shoji Co., Ltd.), mix an appropriate amount of perfume and coloring, and roll according to conventional methods. Kneaded, molded and packaged to obtain a product. This product is suitable as a chewing gum having a good texture, taste and flavor, low caries and low calories.

＜加糖練乳＞
原乳１００質量部に実施例８の方法で得たβ−マルトース含水結晶含有粉末２質量部及び蔗糖２質量部を溶解し、プレートヒーターで加熱殺菌し、次いで濃度７０％に濃縮し、無菌状態で缶詰して製品を得た。本品は、温和な甘味で風味も良く、フルーツ、コーヒー、ココア、紅茶などの調味用に有利に利用できる。 <Sweetened condensed milk>
2 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 8 and 2 parts by mass of sucrose obtained by the method of Example 8 are dissolved in 100 parts by mass of raw milk, sterilized by heating with a plate heater, and then concentrated to a concentration of 70% and aseptic. And canned product. This product has mild sweetness and good flavor, and can be advantageously used for seasoning fruits, coffee, cocoa, tea, and the like.

＜乳酸菌飲料＞
脱脂粉乳１７５質量部、実施例４の方法で得たβ−マルトース含水結晶含有粉末６０質量部及びラクトスクロース高含有粉末（株式会社林原商事販売、登録商標『乳果オリゴ』）５０質量部を水１，１５０質量部に溶解し、６５℃で３０分間殺菌し、４０℃に冷却後、これに、常法に従って、乳酸菌のスターターを３０質量部植菌し、３７℃で８時間培養して乳酸菌飲料を得た。本品は、風味良好で、オリゴ糖を含有し、乳酸菌を安定に保つだけでなく、ビフィズス菌増殖促進作用、整腸作用を有する乳酸菌飲料として好適である。 <Lactic acid bacteria beverage>
175 parts by weight of skim milk powder, 60 parts by weight of β-maltose hydrous crystal-containing powder obtained by the method of Example 4 and 50 parts by weight of lactosucrose high-containing powder (sales by Hayashibara Shoji Co., Ltd., registered trademark “milk fruit oligo”) Dissolve in 1,150 parts by mass, sterilize at 65 ° C. for 30 minutes, cool to 40 ° C., inoculate 30 parts by mass of a lactic acid bacteria starter according to a conventional method, and incubate at 37 ° C. for 8 hours. I got a drink. This product has a good flavor, contains oligosaccharides, and not only keeps lactic acid bacteria stable, but is also suitable as a lactic acid bacteria drink having bifidobacteria growth promoting action and intestinal regulating action.

＜粉末ジュース＞
噴霧乾燥により製造したオレンジ果汁粉末３３質量部に対して、実施例８の方法で得たβ−マルトース含水結晶含有粉末５０質量部、無水結晶マルチトール（（株）林原商事販売 登録商標「マビット」）１０質量部、無水クエン酸０．６５質量部、リンゴ酸０．１質量部、アスコルビン酸２−グルコシド結晶粉末（（株）林原商事販売）０．２質量部、クエン酸ソーダ０．１質量部、プルラン（（株）林原商事販売 ＰＦ−２０）０．５質量部及び粉末香料の適量をよく混合攪拌し、粉砕し微粉末にして、これを流動層造粒機に仕込み、排風温度４０℃とし、これに実施例−４−ｂの方法で得たβ−マルトース含水結晶含有粉末を水に溶解した７０％溶液をバインダーとして適量スプレーし、３０分間造粒し、計量、包装して製品を得た。本品は、果汁含有率約３０％の粉末ジュースである。又、本品は、異味、異臭がなく、高品質のジュースとして商品価値の高いものである。 <Powder juice>
With respect to 33 parts by mass of orange juice powder produced by spray drying, 50 parts by mass of the β-maltose hydrous crystal-containing powder obtained by the method of Example 8, anhydrous crystal maltitol (registered trademark “Mabit” sold by Hayashibara Corporation) ) 10 parts by weight, anhydrous citric acid 0.65 parts by weight, malic acid 0.1 parts by weight, ascorbic acid 2-glucoside crystal powder (sales by Hayashibara Corporation), sodium citrate 0.1 parts by weight Part, pullulan (Hayashibara Shoji Co., Ltd. PF-20) 0.5 parts by mass and appropriate amount of powdered fragrance are mixed and stirred well, pulverized into a fine powder, charged into a fluidized bed granulator, exhaust air temperature 40 ° C., sprayed with an appropriate amount of a 70% solution obtained by dissolving the β-maltose hydrous crystal-containing powder obtained in the method of Example-4-b in water as a binder, granulated for 30 minutes, weighed and packaged. Got the product. This product is a powdered juice with a fruit juice content of about 30%. Moreover, this product has no off-flavor and off-flavor, and has a high commercial value as a high-quality juice.

＜コーヒー飲料＞
焙煎したコーヒー豆１００質量部を粉砕し、これに熱水１，０００質量部を用いて抽出し、抽出液８６０質量部を得た。本液４５０質量部に実施例２の方法で得たβ−マルトース含水結晶含有粉末９０質量部及び適量の重曹を含む水４００質量部を加え、均一に混合して中性ｐＨのコーヒー飲料を調製し、次いで、これを常法に従って、缶に充填し、１２０℃、３０分間加熱殺菌して缶入りコーヒー飲料を製造した。本品は、香り、味ともに良好な高品質のコーヒー飲料である。また、本品を自動販売機に入れ、６０℃で１ヶ月間保持した後も、その良好な風味をよく維持していた。また、本品は、夏場向けに冷却して保存しても、香り、味ともに良好な高品質のコーヒー飲料である。 <Coffee drink>
100 parts by mass of roasted coffee beans were pulverized and extracted with 1,000 parts by mass of hot water to obtain 860 parts by mass of an extract. A neutral pH coffee drink is prepared by adding 90 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 2 and 400 parts by mass of water containing an appropriate amount of baking soda to 450 parts by mass of this liquid and mixing them uniformly. Then, according to a conventional method, this was filled in a can, and heat sterilized at 120 ° C. for 30 minutes to produce a canned coffee drink. This product is a high quality coffee drink with good aroma and taste. Further, even after the product was put in a vending machine and held at 60 ° C. for 1 month, the good flavor was well maintained. In addition, this product is a high-quality coffee drink with good fragrance and taste even after being cooled and stored for summer.

＜カスタードクリーム＞
コーンスターチ１００質量部、実施例４の方法で得たβ−マルトース含水結晶含有粉末５０質量部、含水結晶トレハロース（（株）林原商事販売 登録商標「トレハ」）６０質量部、砂糖４０質量部、及び食塩１質量部を充分に混合し、鶏卵２８０質量部を加えて攪拌し、これに沸騰した牛乳１，０００質量部を徐々に加え、更に火にかけて攪拌を続け、コーンスターチが完全に糊化して全体が半透明になった時に火を止め、これを冷却して適量のバニラ香料を加え、計量、充填、包装して製品を得た。本品は、なめらかな光沢を有し、風味良好で、澱粉の老化も抑制され、高品質のカスタードクリームである。 <Custard cream>
100 parts by mass of corn starch, 50 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 4, 60 parts by mass of hydrous crystal trehalose (registered trademark “Trehha”, Hayashibara Shoji Co., Ltd.), 40 parts by mass of sugar, and Thoroughly mix 1 part by weight of salt, add 280 parts by weight of chicken egg, stir in it, gradually add 1,000 parts by weight of boiled milk, and continue to stir on fire until the corn starch is completely gelatinized. When it became translucent, the fire was turned off, cooled, added with an appropriate amount of vanilla flavor, weighed, filled and packaged to obtain a product. This product is a high-quality custard cream with a smooth luster, good flavor, and reduced starch aging.

＜ういろうの素＞
米粉９０質量部に、コーンスターチ２０質量部、無水結晶マルチトール（（株）林原商事販売 登録商標「マビット」）７０質量部、実施例２の方法で得たβ−マルトース含水結晶含有粉末５０質量部、及びプルラン（（株）林原商事販売 ＰＦ−２０）４質量部を均一に混合してういろうの素を製造した。ういろうの素と適量の抹茶と水とを混練し、これを容器に入れて６０分間蒸し上げて抹茶ういろうを製造した。本品は、照り、口当たりも良好で、風味も良い。又、澱粉の老化も抑制され、日持ちも良く、低カロリーのういろうとしても好適である。 <Uiro no Moto>
90 parts by mass of rice flour, 20 parts by mass of corn starch, 70 parts by mass of anhydrous crystal maltitol (registered trademark “Mabit” sold by Hayashibara Corporation), and 50 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 2 , And 4 parts by weight of pullulan (Hayashibara Shoji Sales PF-20) were mixed uniformly to produce a waxy raw material. Uiro-no-Momo, an appropriate amount of Matcha and water were kneaded, and this was placed in a container and steamed for 60 minutes to produce Matcha Uiro. This product has good shine, mouthfeel, and good flavor. In addition, aging of starch is suppressed, the shelf life is good, and it is also suitable as a low calorie umbilicus.

＜求肥＞
餅粉４質量部を水６質量部で溶いて、木枠に濡れ布巾を敷いたものに流し込み、これを１００℃で２０分間蒸した後、これに実施例２の方法で得たβ−マルトース含水結晶含有粉末２質量部及び砂糖２質量部を加えて十分にこねた後に成形し、求肥を得た。本品は、風味良好であり、しかも糊化した餅米澱粉の老化が抑制され、その賞味期間を大幅に延長することができる。 <Fertilization>
4 parts by weight of starch is dissolved in 6 parts by weight of water, poured into a wooden frame covered with a wet cloth, steamed at 100 ° C. for 20 minutes, and then β-maltose obtained by the method of Example 2 After adding 2 parts by mass of water-containing crystal-containing powder and 2 parts by mass of sugar and kneading sufficiently, it was molded to obtain a fertilizer. This product has a good flavor, and the aging of the gelatinized brown rice starch is suppressed, and the shelf life can be extended significantly.

＜あん＞
原料あずき１０質量部に、常法に従って、水を加えて煮沸し、渋切り、あく抜きし、水溶性夾雑物を除去して、あずきつぶあん約２１質量部を得た。この生あんに砂糖１４質量部、実施例６の方法で得たβ−マルトース含水結晶含有粉末３質量部及び水７質量部を加えて煮沸し、これに少量のサラダオイルを加えてつぶあんを壊さないように練り上げ、製品のあんを約３５質量部得た。本品は、色焼け、離水もなく安定で、舌触り、風味良好で、あんパン、まんじゅう、団子、最中、氷菓などの製菓材料として好適である。 <An>
In accordance with a conventional method, water was added to 10 parts by mass of raw material azuki and boiled, astringent and extracted, and water-soluble impurities were removed to obtain about 21 parts by mass of azuki bean paste. 14 parts by weight of sugar, 3 parts by weight of β-maltose hydrous crystal-containing powder obtained by the method of Example 6 and 7 parts by weight of water are boiled, and a small amount of salad oil is added thereto to break up the mash. The product was kneaded so that about 35 parts by mass of the product was obtained. This product is stable without color burns and water separation, has a good touch and good taste, and is suitable as a confectionery material such as anpan, manju, dumplings, and ice confectionery.

＜パン＞
小麦粉１００質量部、イースト２質量部、砂糖５質量部、実施例２の方法で得たβ−マルトース含水結晶含有粉末５質量部および無機フード０．１質量部を、常法に従って、水でこね、中種を２６℃で２時間発酵させ、その後３０分間熟成、焼き上げた。本品は、色相、すだちとも良好で、適度な弾力、温和な甘味を有する高品質のパンである。 <Bread>
Knead 100 parts by weight of flour, 2 parts by weight of yeast, 5 parts by weight of sugar, 5 parts by weight of β-maltose hydrous crystal-containing powder obtained by the method of Example 2 and 0.1 part by weight of an inorganic hood according to a conventional method. The middle seed was fermented at 26 ° C. for 2 hours, and then aged and baked for 30 minutes. This product is a high-quality bread with good hue and quality, moderate elasticity and mild sweetness.

＜アイシング＞
実施例４の方法で得たβ−マルトース含水結晶含有粉末１０質量部に乳化剤（シュガーエステル）１．２質量部を加熱混合し、次いで、含水結晶トレハロース（（株）林原商事販売 登録商標「トレハ」）１０７質量部を混合し、更に４５℃に保ちながら、油脂７．５質量部を混合してアイシングを製造した。本品は、トレハロース微結晶を含有し、成形性良好でべたつきもなく、経日変化の少ないアイシングである。 <Icing>
1.2 parts by mass of an emulsifier (sugar ester) was heated and mixed with 10 parts by mass of the β-maltose hydrous crystal-containing powder obtained by the method of Example 4, and then hydrous crystal trehalose (trade name “Treha” sold by Hayashibara Corporation). ”) 107 parts by mass were mixed, and while maintaining the temperature at 45 ° C., 7.5 parts by mass of fats and oils were mixed to produce an icing. This product contains trehalose microcrystals, has good moldability, is not sticky, and has little change over time.

＜ボンボン＞
実施例６の方法で得たβ−マルトース含水結晶含有粉末３質量部、含水結晶トレハロース（（株）林原商事販売 登録商標「トレハ」）３００質量部及び水１１５質量部を混合し、加熱してＢｘ７０まで煮詰め、品温を８０℃まで冷却し、ブランディー４０質量部を混合した後、常法に従って成形してボンボンを得た。本品は、トレハロースの微結晶を含有し、ブランディー風味豊かで、径日変化の少ない高品質のボンボンである。 <Bonbon>
3 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 6, 300 parts by mass of hydrous crystal trehalose (trademark “Trehha”, Hayashibara Shoji Co., Ltd.) and 115 parts by mass of water were mixed and heated. The product was boiled to Bx70, the product temperature was cooled to 80 ° C., 40 parts by mass of brandy were mixed, and then molded according to a conventional method to obtain a bonbon. This product is a high-quality bonbon that contains trehalose microcrystals, is rich in brandy, and has little diurnal variation.

＜ハム＞
豚もも肉１，０００質量部に食塩１５質量部および硝酸カリウム３質量部を均一にすり込んで、冷室に１昼夜堆積する。これを水５００質量部、食塩１００質量部、硝酸カリウム３質量部、実施例８の方法で得たβ−マルトース含水結晶含有粉末４０質量部および香辛料からなる塩漬液に冷室で７日間漬け込み、次いで、常法に従い、冷水で洗浄し、ひもで巻き締め、薫煙し、クッキングし、冷却、包装して製品を得た。本品は、色合いもよく、風味良好な高品質のハムである。 <Ham>
A pork thigh of 1,000 parts by mass is uniformly rubbed with 15 parts by mass of sodium chloride and 3 parts by mass of potassium nitrate, and deposited in a cold room for a whole day and night. This was soaked in a salt solution consisting of 500 parts by weight of water, 100 parts by weight of sodium chloride, 3 parts by weight of potassium nitrate, 40 parts by weight of the β-maltose hydrous crystal-containing powder obtained by the method of Example 8 and spices in a cold room for 7 days, According to a conventional method, the product was washed with cold water, wound with a string, smoked, cooked, cooled and packaged to obtain a product. This product is a high quality ham with good color and good flavor.

＜佃煮＞
砂取り、酸処理して角切りした昆布２５０質量部に醤油２１２質量部、アミノ酸液３１８質量部及び実施例６の方法で得たβ−マルトース含水結晶含有粉末３５質量部及び砂糖２０質量部を加えて煮込みつつ、更にグルタミン酸ソーダ１２質量部、カラメル８質量部を加えて炊きあげ、昆布の佃煮を得た。本品は低う蝕性の佃煮である。また、味、香りだけでなく、色、艶ともに食欲をそそるものである。 <Simmered>
Sanded, acid-treated kelp 250 parts by weight, soy sauce 212 parts by weight, amino acid solution 318 parts by weight and β-maltose hydrous crystal-containing powder 35 parts by weight and sugar 20 parts by weight In addition, while stewed, 12 parts by mass of sodium glutamate and 8 parts by mass of caramel were added and cooked to obtain boiled kelp. This product is a low carious boiled eel. Moreover, not only taste and fragrance, but also appetite both in color and gloss.

＜浴用剤＞
ユズの皮ジュース１質量部に対して、実施例２の方法で得たβ−マルトース含水結晶含有粉末１０質量部の割合で混合し、ユズの皮エキス含有粉末を得た。本粉末５質量部に、焼塩９０質量部、含水結晶トレハロース（（株）林原商事販売 登録商標「トレハ」）２質量部、無水ケイ酸１質量部及びα−グルコシル ヘスペリジン（（株）林原商事販売、商品名αＧヘスペリジン）０．５質量部、アスコルビン酸２−グルコシド結晶粉末（（株）林原商事販売）２質量部を混合して浴用剤を製造した。本品は、ユズの香りも豊かで、入浴用の湯に１００乃至１０，０００倍に希釈して利用すればよく、入浴後は、肌がしっとりしなめらかで、湯冷めしない高品質の浴用剤である。 <Bath agent>
It mixed in the ratio of 10 mass parts of (beta) -maltose hydrous crystal containing powder obtained by the method of Example 2 with respect to 1 mass part of yuzu peel juice, and obtained the yuzu peel extract containing powder. To 5 parts by weight of this powder, 90 parts by weight of baked salt, 2 parts by weight of hydrous crystal trehalose (trademark “Trehha” sold by Hayashibara Corporation), 1 part by weight of silicic anhydride and α-glucosyl hesperidin (sales by Hayashibara Corporation) , Trade name αG hesperidin) 0.5 parts by mass and ascorbic acid 2-glucoside crystal powder (produced by Hayashibara Shoji Co., Ltd.) 2 parts by mass were mixed to produce a bath preparation. This product is rich in scent of yuzu and can be used by diluting it 100-10,000 times in hot water for bathing. After bathing, it is a high quality bathing agent that keeps your skin moist and smooth and does not cool down. is there.

＜化粧用クリーム＞
モノステアリン酸ポリオキシエチレングリコール２質量部、自己乳化型モノステアリン酸グリセリン５質量部、実施例２の方法で得たβ−マルトース含水結晶含有粉末５質量部、α−グルコシル ルチン（株式会社林原販売、登録商標「αＧルチン」）１質量部、アスコルビン酸２−グルコシド結晶粉末（（株）林原商事販売）１質量部流動パラフィン１質量部、トリオクタン酸グリセリン１０質量部および防腐剤の適量を常法に従って加熱溶解し、これにＬ−乳酸２質量部、１，３−ブチレングリコール５質量部および精製水６６質量部を加え、ホモゲナイザーにかけ乳化し、更に香料の適量を加えて撹拌混合し、化粧用クリームを製造した。本品は、抗酸化性を有し、安定性が高く、高品質の日焼け止め、美肌剤、色白剤などとして有利に利用できる。 <Cosmetic cream>
2 parts by mass of polyoxyethylene glycol monostearate, 5 parts by mass of glyceryl monostearate monostearate, 5 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 2, α-glucosyl rutin (Hayashibara Sales Co., Ltd.) , Registered trademark “αG rutin”) 1 part by mass, ascorbic acid 2-glucoside crystal powder (sales by Hayashibara Corporation) 1 part by weight liquid paraffin 1 part by weight, trioctanoic acid glycerin 10 parts by weight and an appropriate amount of preservative And then, 2 parts by mass of L-lactic acid, 5 parts by mass of 1,3-butylene glycol and 66 parts by mass of purified water are added thereto, emulsified with a homogenizer, an appropriate amount of fragrance is added, and the mixture is stirred and mixed. A cream was produced. This product has antioxidant properties, high stability, and can be advantageously used as a high-quality sunscreen, skin beautifying agent, whitening agent, and the like.

＜練歯磨＞
第二リン酸カルシウム４５質量部、ラウリル硫酸ナトリウム１．５質量部、グリセリン２５質量部、ポオキシエチレンソルビタンラウレート０．５質量部、実施例４の方法で得たβ−マルトース含水結晶含有粉末１０質量部、サッカリン０．０２質量部および防腐剤０．０５質量部を水１３質量部と混合して練歯磨を得た。本品は、界面活性剤の洗浄力を落とすことなく、嫌味を改良し、使用後感も良好である。 <Toothpaste>
45 parts by mass of dibasic calcium phosphate, 1.5 parts by mass of sodium lauryl sulfate, 25 parts by mass of glycerin, 0.5 parts by mass of poxyethylene sorbitan laurate, 10 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 4 Part, 0.02 part by weight of saccharin and 0.05 part by weight of preservative were mixed with 13 parts by weight of water to obtain a toothpaste. This product improves taste and does not deteriorate the detergency of the surfactant and has a good feeling after use.

＜流動食用固体製剤＞
実施例６の方法で得たβ−マルトース含水結晶含有粉末１００質量部、トレハロース含水結晶２００質量部、マルトテトラオース高含有粉末２００質量部、粉末卵黄２７０質量部、脱脂粉乳２０９質量部、塩化ナトリウム４．４質量部、塩化カリウム１．８質量部、硫酸マグネシウム４質量部、チアミン０．０１質量部、アスコルビン酸ナトリウム０．１質量部、ビタミンＥアセテート０．６質量部及びニコチン酸アミド０．０４質量部からなる配合物を調製し、この配合物２５グラムずつ防湿性ラミネート小袋に充填し、ヒートシールして製品を得た。本品は、β−マルトース含水結晶含有粉末及びトレハロース含水結晶により適度の甘味が付加され、整腸作用に優れた流動食である。１袋分を約１５０乃至３００ｍｌの水に溶解して流動食とし、経口的、又は鼻腔、胃、腸などへ経管的使用方法により利用され、生体へのエネルギー補給用に有利に利用できる。 <Food edible solid formulation>
100 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 6, 200 parts by mass of hydrous crystals of trehalose, 200 parts by mass of high maltotetraose-containing powder, 270 parts by mass of powdered egg yolk, 209 parts by mass of skim milk powder, sodium chloride 4.4 parts by mass, 1.8 parts by mass of potassium chloride, 4 parts by mass of magnesium sulfate, 0.01 parts by mass of thiamine, 0.1 parts by mass of sodium ascorbate, 0.6 parts by mass of vitamin E acetate and 0. A formulation consisting of 04 parts by mass was prepared, and 25 grams of this formulation was filled into moisture-proof laminated sachets and heat sealed to obtain a product. This product is a liquid food that is moderately sweetened with β-maltose hydrated crystal-containing powder and trehalose hydrated crystal, and has excellent intestinal action. One bag is dissolved in about 150 to 300 ml of water to obtain a liquid food, which is used orally or by a tube-use method for the nasal cavity, stomach, intestine, etc., and can be advantageously used for energy supply to a living body.

＜錠剤＞
アスピリン５０質量部に実施例８の方法で得たβ−マルトース含水結晶含有粉末１４質量部、コーンスターチ４質量部を充分に混合した後、常法に従って打錠機により打錠して厚さ５．２５ｍｍ、１錠６８０ｍｇの錠剤を製造した。本品は、β−マルトース含水結晶含有粉末の賦形性を利用したもので、吸湿性がなく、物理的強度も充分にあり、しかも水中での崩壊はきわめて良好である。 <Tablets>
After sufficiently mixing 14 parts by mass of the β-maltose hydrous crystal-containing powder obtained by the method of Example 8 and 4 parts by mass of corn starch with 50 parts by mass of aspirin, the tablet was compressed by a tableting machine according to a conventional method to obtain a thickness of 5. Tablets of 25 mm, 1 tablet 680 mg were produced. This product utilizes the formability of β-maltose hydrous crystal-containing powder, is not hygroscopic, has sufficient physical strength, and is very good in disintegration in water.

＜糖衣錠＞
重量１５０ｍｇの素錠を芯剤とし、これに実施例８の方法で得たβ−マルトース含水結晶含有粉末４０質量部、プルラン（（株）林原商事販売 ＰＦ−２０）２質量部、水３０質量部、タルク２５質量部および酸化チタン３質量部からなる下掛け液を用いて錠剤重量が約２３０ｍｇになるまで糖衣し、次いで、同じβ−マルトース含水結晶含有粉末６５質量部、プルラン（（株）林原商事販売 ＰＦ−２０）１質量部および水３４質量部からなる上掛け液を用いて、糖衣し、更に、ロウ液で艶出しして光沢のある外観の優れた糖衣錠を得た。本品は、耐衝撃性にも優れており、高品質を長期間維持する。 <Sugar-coated tablets>
An uncoated tablet having a weight of 150 mg is used as a core, and 40 parts by mass of β-maltose hydrous crystal-containing powder obtained by the method of Example 8, 2 parts by mass of pullulan (Hayashibara Shoji PF-20), 30 parts by mass of water Part, 25 parts by mass of talc and 3 parts by mass of titanium oxide, and sugar coating until the tablet weight reaches about 230 mg, and then 65 parts by mass of the same β-maltose hydrous crystal-containing powder, Pullulan (Co., Ltd.) Hayashibara Shoji Co., Ltd. PF-20) A sugar-coated tablet having a glossy appearance was obtained by sugar-coating using a top coating solution consisting of 1 part by mass and 34 parts by mass of water, and further glazing with a wax solution. This product has excellent impact resistance and maintains high quality for a long time.

以上の説明から明らかなように、本発明の噴霧方式で粉末化され、無水物換算で、マルトース８６％以上９３％未満及びグルコース２％以上を含有し、結晶化度が６２％以上７２％未満であるβ−マルトース含水結晶含有粉末は、マルトース異性体としてマルトース中のα−アノマーを７％以上１４％未満含有し、水系媒体への溶解性に優れ、且つ、保存安定性に優れ、流動性良好で、取扱い容易な粉末である。また、これらのβ−マルトース含水結晶含有粉末は、グルコース、マルトトリオース及びグルコース重合度４以上のオリゴ糖などのマルトース以外の糖質を７％以上１４％未満と比較的多量共存含有しているにもかかわらず、噴霧方式での製造が容易であり、連続的で、短時間に製造することもでき、粉末収率も高いことから、コストダウンを計ることも容易である。   As is apparent from the above description, it is pulverized by the spray method of the present invention and contains, in terms of anhydride, maltose of 86% to less than 93% and glucose of 2% or more, and the crystallinity is from 62% to less than 72%. The β-maltose hydrous crystal-containing powder is a maltose isomer containing an α-anomer in maltose of 7% to less than 14%, excellent solubility in aqueous media, excellent storage stability, and fluidity. Good and easy to handle powder. These β-maltose hydrous crystal-containing powders contain a relatively large amount of carbohydrates other than maltose, such as glucose, maltotriose and oligosaccharides having a glucose polymerization degree of 4 or more, such as 7% to less than 14%. Nevertheless, it is easy to manufacture by spraying, it can be manufactured continuously and in a short time, and the powder yield is high, so it is easy to reduce costs.

従って、本発明の確立は、水系媒体への溶解性に優れたβ−マルトース含水結晶含有粉末を容易に、低コストで製造できることから、澱粉糖製造業だけでなく、利用する側の人にとっても作業性の向上などが期待できるために好都合であり、該当する業界を初めとする産業界に与える工業的意義は極めて大きい。   Therefore, the establishment of the present invention allows easy production of β-maltose hydrous crystal-containing powder having excellent solubility in an aqueous medium at low cost, so that not only starch sugar manufacturers but also those who use it. This is advantageous because improvement in workability can be expected, and the industrial significance given to the industry including the corresponding industry is extremely large.

マルトース含量が、無水物換算で８６．２％で結晶化度が６２．１％を示すβ−マルトース含水結晶含有粉末の粉末Ｘ線回折図形。A powder X-ray diffraction pattern of a β-maltose hydrous crystal-containing powder having a maltose content of 86.2% in terms of anhydride and a crystallinity of 62.1%. マルトース含量が、無水物換算で９１．３％で結晶化度が７０．８％を示すβ−マルトース含水結晶含有粉末の粉末Ｘ線回折図形。The powder X-ray-diffraction figure of the beta-maltose hydrous crystal containing powder whose maltose content is 91.3% in conversion of an anhydride and a crystallinity degree is 70.8%. マルトース含量が、無水物換算で９５．０％で結晶化度が７４．５％を示す精製マルトース 登録商標「サンマルトＳ」の粉末Ｘ線回折図形。A powder X-ray diffraction pattern of a purified maltose registered trademark “Sanmalt S” having a maltose content of 95.0% in terms of anhydride and a crystallinity of 74.5%. マルトース含量が、無水物換算で９９．６％で結晶化度が８２．６％を示す試薬β−マルトース含水結晶 商品名「マルトースＨＨＨ」の粉末Ｘ線回折図形。Reagent β-maltose hydrous crystal having a maltose content of 99.6% in terms of anhydride and a crystallinity of 82.6%. Powder X-ray diffraction pattern of trade name “Maltose HHH”. マルトース含量が、無水物換算で９８．５％で結晶化度が７６．３％を示すα−マルトース無水結晶 登録商標「ファイントース」の粉末Ｘ線回折図形。An α-maltose anhydrous crystal showing a maltose content of 98.5% in terms of anhydride and a crystallinity of 76.3%.

Claims (3)

液化澱粉に、α−アミラーゼ、β−アミラーゼおよび澱粉枝切り酵素を作用させて糖化し、適宜精製することによって、無水物換算で、マルトース８６質量％以上９３質量％未満およびグルコース２質量％以上を含有するマルトース含有溶液とする工程と、そのマルトース含有溶液を適宜濃縮、助晶した後、噴霧方式で粉末化して、無水物換算で、マルトース８６質量％以上９３質量％未満およびグルコース２質量％以上を含有し、マルトース異性体としてマルトース中のα−アノマー含量が７質量％以上１４質量％未満で、結晶化度６２％以上７２％未満のβ−マルトース含水結晶含有粉末とする工程とを含んでなることを特徴とするβ−マルトース含水結晶含有粉末の製造方法。 By saccharification by allowing α-amylase, β-amylase and starch debranching enzyme to act on liquefied starch and purifying it appropriately , maltose is 86% by mass to less than 93% by mass and glucose is 2% by mass or more in terms of anhydride. The step of preparing a maltose-containing solution to be contained, and the maltose-containing solution are appropriately concentrated and crystallized, and then pulverized by a spray method, in terms of anhydride, not less than 86% by mass and less than 93% by mass and 2% by mass or more of glucose A β-maltose hydrous crystal-containing powder having an α-anomer content in the maltose of 7% to less than 14% by mass and a crystallinity of 62% to less than 72% as a maltose isomer. A process for producing a β-maltose water-containing crystal-containing powder. マルトース含有溶液を、マスキットの形態で、噴霧方式で粉末化することを特徴とする請求項１記載のβ−マルトース含水結晶含有粉末の製造方法。   2. The method for producing a β-maltose hydrous crystal-containing powder according to claim 1, wherein the maltose-containing solution is pulverized by a spray method in the form of a mass kit. スルホン化スチレンジビニルベンゼン共重合体（ナトリウム型）カラムを用いた液体クロマトグラフィーによる糖組成分析において、β−マルトース含水結晶含有粉末が、マルトトリオースと見なされるものを、無水物換算で、０．６質量％以上１．９質量％以下含有することを特徴とする請求項１又は２記載のβ−マルトース含水結晶含有粉末の製造方法。 Sulfonated styrene-divinylbenzene copolymer in (sodium form) Liquid chromatography with sugar composition analysis using a column, beta-maltose hydrated crystal-containing powder, what is considered as maltotriose, on a dry solid basis, 0. The method for producing a β-maltose hydrous crystal-containing powder according to claim 1 or 2, wherein the content is 6% by mass or more and 1.9% by mass or less .
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