JP6695682B2 - Method for producing purified water-soluble seed-based polysaccharide - Google Patents
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- 150000004676 glycans Chemical class 0.000 title claims description 79
- 229920001282 polysaccharide Polymers 0.000 title claims description 77
- 239000005017 polysaccharide Substances 0.000 title claims description 77
- 238000004519 manufacturing process Methods 0.000 title claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 171
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 94
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 235000004298 Tamarindus indica Nutrition 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000002994 raw material Substances 0.000 claims description 33
- 239000012046 mixed solvent Substances 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 23
- 229920002907 Guar gum Polymers 0.000 claims description 22
- 239000000665 guar gum Substances 0.000 claims description 22
- 235000010417 guar gum Nutrition 0.000 claims description 22
- 229960002154 guar gum Drugs 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 229920000926 Galactomannan Polymers 0.000 claims description 11
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 claims description 10
- 229920000161 Locust bean gum Polymers 0.000 claims description 10
- 239000000711 locust bean gum Substances 0.000 claims description 10
- 235000010420 locust bean gum Nutrition 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- 229930182830 galactose Natural products 0.000 claims description 6
- 239000001884 Cassia gum Substances 0.000 claims description 4
- 244000275012 Sesbania cannabina Species 0.000 claims description 4
- 244000250129 Trigonella foenum graecum Species 0.000 claims description 4
- 235000001484 Trigonella foenum graecum Nutrition 0.000 claims description 4
- 235000019318 cassia gum Nutrition 0.000 claims description 4
- 235000010491 tara gum Nutrition 0.000 claims description 4
- 239000000213 tara gum Substances 0.000 claims description 4
- 235000001019 trigonella foenum-graecum Nutrition 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 229920001503 Glucan Polymers 0.000 claims 1
- 240000004584 Tamarindus indica Species 0.000 claims 1
- 125000002519 galactosyl group Chemical group C1([C@H](O)[C@@H](O)[C@@H](O)[C@H](O1)CO)* 0.000 claims 1
- 239000000243 solution Substances 0.000 description 135
- 238000003756 stirring Methods 0.000 description 78
- 239000007864 aqueous solution Substances 0.000 description 67
- 238000001914 filtration Methods 0.000 description 52
- 241000596504 Tamarindus Species 0.000 description 43
- 239000002244 precipitate Substances 0.000 description 37
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 36
- 239000006185 dispersion Substances 0.000 description 29
- 239000000203 mixture Substances 0.000 description 29
- 239000000843 powder Substances 0.000 description 27
- 238000005406 washing Methods 0.000 description 25
- 238000002834 transmittance Methods 0.000 description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 15
- 239000007788 liquid Substances 0.000 description 15
- 230000003287 optical effect Effects 0.000 description 15
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- 238000005259 measurement Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- 230000000704 physical effect Effects 0.000 description 13
- 230000009965 odorless effect Effects 0.000 description 10
- 238000006386 neutralization reaction Methods 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- 239000006228 supernatant Substances 0.000 description 8
- 235000013305 food Nutrition 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 229920002472 Starch Polymers 0.000 description 5
- 235000013373 food additive Nutrition 0.000 description 5
- 239000002778 food additive Substances 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002537 cosmetic Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- -1 tamarind seed gum Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Description
本発明は、精製水溶性種子系多糖類の製造方法に関する。 The present invention relates to a method for producing a purified water-soluble seed-based polysaccharide.
従来、タマリンド種子ガム、フェヌグリークガム、グアーガム、セスバニアガム、タラガム、ローカストビーンガム、カシアガム等の水溶性種子系多糖類は、各種子の粉砕物を温水、熱水等で抽出して製造され、食品、化粧品又は捺染等の糊料等として広く用いられている。 Conventionally, water-soluble seed-based polysaccharides such as tamarind seed gum, fenugreek gum, guar gum, sesbania gum, tara gum, locust bean gum, and cassia gum are produced by extracting a pulverized product of various offspring with hot water, hot water, etc. It is widely used as a sizing agent for cosmetics or printing.
これらの水溶性種子系多糖類は、原料中にタンパク質、脂肪、灰分、繊維質等不純物が混入しているので、当該多糖類の水溶液は透明性に劣るという問題がある。そのため、製品化の際に、不純物を除去して上記水溶液の透明性の向上が図られている。 These water-soluble seed-based polysaccharides contain impurities such as proteins, fats, ash, and fibrous substances in the raw materials, and thus there is a problem that the aqueous solution of the polysaccharide is inferior in transparency. Therefore, in commercialization, impurities are removed to improve the transparency of the aqueous solution.
透明性の良好な精製水溶性多糖類の製造方法として、例えば、アルコール沈澱法による製造方法が知られている。この方法は、水溶性多糖類を含む原料を分散あるいは溶解させた後に、加熱糊化し、不純物を除去するために濾過助剤を加えてから除去し、ろ液にアルコールを加えて多糖類を沈殿させ、この沈殿物を乾燥、粉砕して製造する方法である。 As a method for producing a purified water-soluble polysaccharide having good transparency, for example, an alcohol precipitation method is known. This method involves dispersing or dissolving a raw material containing a water-soluble polysaccharide, heating it to gelatinize it, adding a filter aid to remove impurities, and then removing it, and adding alcohol to the filtrate to precipitate the polysaccharide. And the precipitate is dried and pulverized to produce.
しかしながら、この方法では、濾過助剤を加えて糊液を濾過するために糊液の粘度を低くする必要があるので、０．５〜２％という低濃度の糊液しか用いることができない。したがって、精製水溶性多糖類を得るためには、大量の水を除去する必要があり、そのため、安価に精製水溶性多糖類を製造できないという問題がある。また、濾過助剤を含んだ濾過残渣も生成するので、濾過残渣分を産業廃棄物として処理しなければならないという問題がある。 However, in this method, since it is necessary to reduce the viscosity of the paste solution by adding the filter aid to filter the paste solution, only a paste solution having a low concentration of 0.5 to 2% can be used. Therefore, in order to obtain the purified water-soluble polysaccharide, it is necessary to remove a large amount of water, which causes a problem that the purified water-soluble polysaccharide cannot be manufactured at low cost. Further, since a filter residue containing a filter aid is also produced, there is a problem that the filter residue component must be treated as industrial waste.
グアーガムの精製方法として、グアーガムスプリットを酸で処理した後にアルカリで中和し、アルコール水溶液で脱水する精製方法が開示されている（特許文献１参照）。 As a method for purifying guar gum, a method for treating guar gum splits with an acid, neutralizing with an alkali, and dehydrating with an aqueous alcohol solution is disclosed (see Patent Document 1).
しかしながら、特許文献１に記載の精製方法は、大量の水を使用するので、生じた排水を処理するために大きな処理設備を必要とするという問題がある。 However, since the purification method described in Patent Document 1 uses a large amount of water, there is a problem that a large treatment facility is required to treat the generated wastewater.
従って、透明性に優れた精製水溶性多糖類を効率よく、且つ容易に製造できる製造方法の開発が望まれている。 Therefore, it is desired to develop a production method capable of efficiently and easily producing a purified water-soluble polysaccharide having excellent transparency.
本発明は、透明性に優れた精製水溶性種子系多糖類を効率よく、且つ容易に製造できる製造方法を提供することを目的とする。 An object of the present invention is to provide a method for producing a purified water-soluble seed-based polysaccharide having excellent transparency efficiently and easily.
本発明者は上記目的を達成すべく鋭意研究を重ねた結果、（１）水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する混合溶液を調製する工程１、（２）上記混合溶液を加熱糊化して糊液を調製する工程２、並びに（３）上記糊液にアルコール添加及び／又は冷却を行う工程３を有する精製水溶性種子系多糖類の製造方法によれば、不純分の少ない精製水溶性種子系多糖類を得ることができ、当該精製水溶性種子系多糖類は、透明性が高いことを見出し、本発明を完成するに至った。 As a result of intensive studies to achieve the above object, the present inventor has (1) a step of preparing a mixed solution containing a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound. 1. Production of a purified water-soluble seed-based polysaccharide having 1, (2) step 2 of preparing a paste solution by heating and gelatinizing the mixed solution, and (3) step 3 of adding alcohol and / or cooling the paste solution According to the method, it was possible to obtain a purified water-soluble seed-based polysaccharide having a low impurity content, and it was found that the purified water-soluble seed-based polysaccharide has high transparency, and has completed the present invention.
即ち、本発明は、下記の精製水溶性種子系多糖類の製造方法に関する。
１．精製水溶性種子系多糖類の製造方法であって、
（１）水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する溶液を調製する工程１、
（２）前記溶液を加熱糊化して糊液を調製する工程２、並びに
（３）前記糊液にアルコール添加及び／又は糊液の冷却を行う工程３
を有する、ことを特徴とする製造方法。
２．前記水溶性種子系多糖類原料が、ガラクトース含有多糖類である、項１に記載の製造方法。
３．前記水溶性種子系多糖類原料が、ガラクトキシログルカン及びガラクトマンナンから選択される少なくとも１種の粉砕物である、項１又は２に記載の製造方法。
４．前記ガラクトキシログルカンがタマリンド種子ガムであり、前記ガラクトマンナンがフェヌグリークガム、グアーガム、セスバニアガム、タラガム、ローカストビーンガム及びカシアガムからなる群より選択される少なくとも１種である、項３に記載の製造方法
５．前記アルコールが、メタノール、エタノール及びイソプロパノールから選択される少なくとも１種である、項１〜４のいずれかに記載の製造方法。
６．前記アルカリ性化合物が、水酸化リチウム、水酸化ナトリウム、水酸化カリウム、水酸化マグネシウム及び水酸化カルシウムから選択される少なくとも１種である、項１〜５のいずれかに記載の製造方法。
７．前記糊液中の前記アルカリ性化合物の濃度は、前記糊液を１００質量％として１〜２０質量％である、項１〜６のいずれかに記載の製造方法。
８．前記糊液のＰＨは１０以上である、項１〜７のいずれかに記載の製造方法。
That is, the present invention relates to the following method for producing a purified water-soluble seed-based polysaccharide.
1. A method for producing a purified water-soluble seed-based polysaccharide,
(1) Step 1 of preparing a solution containing a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound,
(2) Step 2 of preparing the paste solution by heating and gelatinizing the solution, and (3) Step 3 of adding alcohol to the paste solution and / or cooling the paste solution.
A manufacturing method comprising:
2. Item 2. The method according to Item 1, wherein the water-soluble seed-based polysaccharide raw material is a galactose-containing polysaccharide.
3. Item 3. The production method according to Item 1 or 2, wherein the water-soluble seed-based polysaccharide raw material is at least one pulverized product selected from galactoxyloglucan and galactomannan.
4. The method according to Item 3, wherein the galactoxyloglucan is tamarind seed gum, and the galactomannan is at least one selected from the group consisting of fenugreek gum, guar gum, sesbania gum, tara gum, locust bean gum and cassia gum. 5. Item 5. The method according to any one of Items 1 to 4, wherein the alcohol is at least one selected from methanol, ethanol, and isopropanol.
6. Item 6. The method according to any one of Items 1 to 5, wherein the alkaline compound is at least one selected from lithium hydroxide, sodium hydroxide, potassium hydroxide, magnesium hydroxide and calcium hydroxide.
7. Item 7. The production method according to any one of Items 1 to 6, wherein the concentration of the alkaline compound in the paste solution is 1 to 20 mass% based on 100 mass% of the paste solution.
8. Item 8. The method according to any one of Items 1 to 7, wherein the paste has a pH of 10 or more.
本発明の精製水溶性種子系多糖類の製造方法は、アルカリ性化合物により、水溶性種子系多糖類原料の水溶性成分と不溶性成分とが分離し易くなっており、アルコールの添加や冷却等の簡易な方法により、容易に不溶性成分を除去することができる。このため、不溶成分を除去する目的で、水溶性種子系多糖類原料の溶液又は分散液の粘度を低く保つために、水溶性種子系多糖類原料の溶液または分散液の濃度を低くしたり、濾過助剤を用いて濾過する必要がなく、水溶性種子系多糖類原料の高濃度の混合溶液から不溶性成分を除去することができるので、透明性に優れた精製水溶性種子系多糖類を効率よく、且つ容易に製造することができる。 The method for producing a purified water-soluble seed-based polysaccharide of the present invention, the alkaline compound makes it easy to separate the water-soluble component and the insoluble component of the water-soluble seed-based polysaccharide raw material, and simple addition of alcohol or cooling Insoluble components can be easily removed by various methods. Therefore, for the purpose of removing the insoluble components, in order to keep the viscosity of the solution or dispersion of the water-soluble seed-based polysaccharide raw material low, lower the concentration of the solution or dispersion of the water-soluble seed-based polysaccharide raw material, Since it is not necessary to filter using a filter aid and insoluble components can be removed from a high-concentration mixed solution of a water-soluble seed-based polysaccharide raw material, a highly purified purified water-soluble seed-based polysaccharide can be efficiently used. Good and easy to manufacture.
以下、本発明について詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明の精製水溶性種子系多糖類の製造方法は、
（１）水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する溶液を調製する工程１、
（２）前記溶液を加熱糊化して糊液を調製する工程２、並びに
（３）前記糊液にアルコール添加及び／又は冷却を行う工程３
を有する製造方法である。
The method for producing a purified water-soluble seed-based polysaccharide of the present invention,
(1) Step 1 of preparing a solution containing a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound,
(2) Step 2 of preparing the paste solution by heating and gelatinizing the solution, and (3) Step 3 of adding alcohol and / or cooling the paste solution.
It is a manufacturing method having.
１．工程１
工程１は、（１）水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する溶液を調製する工程である。
1. Process 1
Step 1 is (1) a step of preparing a solution containing a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound.
（水溶性種子系多糖類原料）
本発明に用いられる水溶性種子系多糖類原料は、種子から得られる水溶性多糖類であれば特に限定されず、例えば、ガラクトース含有多糖類が挙げられる。ガラクトース含有多糖類としては、後述する水または水とアルコールとの混合溶媒に溶解し易い点で粉砕物を用いることが好ましい。
(Water soluble seed-based polysaccharide raw material)
The water-soluble seed-based polysaccharide raw material used in the present invention is not particularly limited as long as it is a water-soluble polysaccharide obtained from seeds, and examples thereof include galactose-containing polysaccharides. As the galactose-containing polysaccharide, it is preferable to use a pulverized product because it is easily dissolved in water or a mixed solvent of water and alcohol described later.
上記ガラクトース含有多糖類としては、ガラクトキシログルカン、ガラクトマンナンが挙げられる。 Examples of the galactose-containing polysaccharides include galactoxyloglucan and galactomannan.
上記ガラクトキシログルカンとしては、タマリンド種子ガムを用いることが好ましい。 As the galactoxyloglucan, tamarind seed gum is preferably used.
上記ガラクトマンナンとしては、フェヌグリークガム、グアーガム、セスバニアガム、タラガム、ローカストビーンガム、カシアガムを用いることができる。これらのガラクトマンナンは、１種又は複数種を混合して用いてもよい。 As the galactomannan, fenugreek gum, guar gum, sesbania gum, tara gum, locust bean gum, cassia gum can be used. These galactomannans may be used alone or in combination of two or more.
上記ガラクトマンナンのガラクトースとマンノースとの比率（質量比）は１：１〜１：５程度が好ましい。 The ratio (mass ratio) of galactose and mannose of the galactomannan is preferably about 1: 1 to 1: 5.
水溶性種子系多糖類原料の市販品のグレードは特に限定されないが、異物の混入が少ないものが好ましく、ＪＩＳ標準フルイ３５０μｍ（目開き３５０μｍ）を９９％以上篩過するグレードが好ましい。水溶性種子系多糖類原料の粒子径を上記範囲とすることで、後述する水または水とアルコールとの混合溶媒に溶解し易くなり、より効率よく精製水溶性種子系多糖類を製造することができる。 The grade of a commercially available water-soluble seed-based polysaccharide raw material is not particularly limited, but is preferably a grade with less contamination of foreign substances, and a grade capable of sieving 99% or more of JIS standard sieve 350 μm (opening 350 μm). By setting the particle diameter of the water-soluble seed-based polysaccharide raw material in the above range, it becomes easy to dissolve in water or a mixed solvent of water and alcohol described later, and it is possible to produce a purified water-soluble seed-based polysaccharide more efficiently. it can.
水溶性種子系多糖類原料の含有量は、溶液を１００質量％として、２〜２０質量％が好ましく、３〜１５質量％がより好ましく、４〜１２質量％がさらに好ましい。水溶性種子系多糖類原料の含有量を上述の範囲とすることより、加熱、冷却等の操作を容易に行うことができ、かつ、溶液の量が多くなり過ぎず、より生産性が向上する。 The content of the water-soluble seed-based polysaccharide raw material is preferably 2 to 20% by mass, more preferably 3 to 15% by mass, and further preferably 4 to 12% by mass, with the solution as 100% by mass. By setting the content of the water-soluble seed-based polysaccharide raw material in the above range, operations such as heating and cooling can be easily performed, and the amount of the solution does not become too large, and the productivity is further improved. ..
(水または水とアルコールとの混合溶媒)
本発明の製造方法では、水又は水とアルコールとの混合溶媒(以下「水又は混合溶媒」ともいう)が用いられる。混合溶媒に用いられるアルコールとしては特に限定されず、例えば、メタノール、エタノール、イソプロパノール等が挙げられる。これらの中でも、メタノール及びエタノールが好ましい。また、上記アルコールは、単独で用いてもよいし、２種以上を混合して用いてもよい。
(Water or mixed solvent of water and alcohol)
In the production method of the present invention, water or a mixed solvent of water and alcohol (hereinafter also referred to as “water or mixed solvent”) is used. The alcohol used in the mixed solvent is not particularly limited, and examples thereof include methanol, ethanol and isopropanol. Among these, methanol and ethanol are preferable. The above alcohols may be used alone or in combination of two or more.
混合溶媒中の水とアルコールとの質量比は、９９：１〜５０：５０が好ましい。混合溶媒中の水とアルコールとの質量比を上述の範囲とすることにより、水溶性種子系多糖類原料中の水溶性成分と不溶性成分とを、より容易に分離することができる。 The mass ratio of water and alcohol in the mixed solvent is preferably 99: 1 to 50:50. By setting the mass ratio of water and alcohol in the mixed solvent within the above range, the water-soluble component and the insoluble component in the water-soluble seed-based polysaccharide raw material can be more easily separated.
本発明の製造方法において、溶液中の水又は混合溶媒の濃度は、溶液を１００質量％として、７０〜９７質量％が好ましく、７５〜９２質量％がより好ましく、８０〜８８質量％が更に好ましい。溶液中の水又は混合溶媒の濃度を上述の範囲とすることにより、加熱、冷却等の操作を容易に行うことができ、かつ、溶液等の量が多くなり過ぎず、より生産性に優れるとの利点を有する。 In the production method of the present invention, the concentration of water or a mixed solvent in the solution is preferably 70 to 97% by mass, more preferably 75 to 92% by mass, still more preferably 80 to 88% by mass, with the solution as 100% by mass. .. By setting the concentration of water or a mixed solvent in the solution within the above range, operations such as heating and cooling can be easily performed, and the amount of the solution or the like does not become too large, and is more excellent in productivity. Have the advantage of.
（アルカリ性化合物）
アルカリ性化合物としては特に限定されず、水溶性種子系多糖類原料の不溶性成分と水溶性成分とを容易に分離できるものであればよい。上記アルカリ性化合物としては、例えば、水酸化リチウム、水酸化ナトリウム、水酸化カリウム、水酸化マグネシウム、水酸化カルシウム等が挙げられる。アルカリ性化合物は、製造される精製水溶性種子系多糖類の使用目的に応じたものを用いることが好ましい。例えば、食品用途に使用するのであれば水酸化ナトリウム、水酸化カリウム等を用いることが好ましい。上記アルカリ性化合物は単独で用いてもよいし、２種以上を組み合わせてもよい。
(Alkaline compound)
The alkaline compound is not particularly limited as long as it can easily separate the insoluble component and the water-soluble component of the water-soluble seed-based polysaccharide raw material. Examples of the alkaline compound include lithium hydroxide, sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide and the like. As the alkaline compound, it is preferable to use an alkaline compound according to the purpose of use of the purified water-soluble seed-based polysaccharide produced. For example, if it is used for food use, it is preferable to use sodium hydroxide, potassium hydroxide or the like. The alkaline compounds may be used alone or in combination of two or more.
溶液中のアルカリ性化合物の含有量は、溶液を１００質量％として、１〜２０質量％が好ましく、３〜１５質量％がより好ましく、更に好ましくは４〜１２質量％である。アルカリ性化合物の含有量を上記範囲とすることにより、加熱、冷却等の操作を容易に行うことができ、且つ、水溶性種子系多糖類原料の水溶性成分と不溶性成分との分離をより容易に行うことができる。 The content of the alkaline compound in the solution is preferably 1 to 20% by mass, more preferably 3 to 15% by mass, and further preferably 4 to 12% by mass, based on 100% by mass of the solution. By setting the content of the alkaline compound in the above range, operations such as heating and cooling can be easily performed, and separation of the water-soluble component and the insoluble component of the water-soluble seed-based polysaccharide raw material can be performed more easily. It can be carried out.
(溶液の調製)
溶液の調製方法としては特に限定されず、例えば、水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を、従来より広く知られた方法により混合撹拌する方法等が挙げられる。
(Preparation of solution)
The method for preparing the solution is not particularly limited, for example, a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound, a method of mixing and stirring by a method widely known from the past, and the like. Can be mentioned.
以上説明した工程１により、水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する溶液が調製される。 By the step 1 described above, a solution containing the water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound is prepared.
２．工程２
工程２は、工程１で調製された溶液を加熱糊化して糊液を調製する工程である。加熱糊化の際の加熱温度は、水溶性種子系多糖類原料の品質、溶液または分散液中の水溶性種子系多糖類原料の濃度を考慮して適宜設定することができる。具体的には、上記加熱温度は、好ましくは５０℃以上、より好ましくは６０℃以上、更に好ましくは７０℃以上である。また、上記加熱温度の上限は、高圧反応機を用いて製造することができるので特に限定されない。加熱温度の上限は、１２０℃であることが好ましい。加熱温度を上記範囲とすることで、水溶性種子系多糖類原料の水溶性成分と不溶性成分とを分離しやすくなり、加熱糊化の際の攪拌や、冷却の際の撹拌等の操作を容易に行うことができる。
2. Process 2
Step 2 is a step of preparing a paste solution by heating and gelatinizing the solution prepared in Step 1. The heating temperature at the time of heat gelatinization can be appropriately set in consideration of the quality of the water-soluble seed-based polysaccharide raw material and the concentration of the water-soluble seed-based polysaccharide raw material in the solution or dispersion. Specifically, the heating temperature is preferably 50 ° C. or higher, more preferably 60 ° C. or higher, even more preferably 70 ° C. or higher. The upper limit of the heating temperature is not particularly limited because it can be produced using a high pressure reactor. The upper limit of the heating temperature is preferably 120 ° C. By setting the heating temperature in the above range, it becomes easy to separate the water-soluble component and the insoluble component of the water-soluble seed-based polysaccharide raw material, and the operations such as stirring during heating gelatinization and stirring during cooling are easy. Can be done.
加熱糊化の際の加熱時間は特に限定されず、３０分〜５時間が好ましく、１時間〜４時間がより好ましい。加熱時間を上記範囲とすることにより、糊液を十分に調製することができる。 The heating time in the heating gelatinization is not particularly limited, and is preferably 30 minutes to 5 hours, more preferably 1 hour to 4 hours. By setting the heating time within the above range, the paste solution can be sufficiently prepared.
上記加熱糊化は、溶液を攪拌しながら行うことが好ましい。溶液を攪拌しながら加熱糊化を行うことにより、均一な糊液を調製することができる。 The heating gelatinization is preferably performed while stirring the solution. By heating and gelatinizing the solution while stirring, a uniform paste solution can be prepared.
工程２により調製される糊液のＰＨは、１０以上が好ましく、１１以上がより好ましい。糊液のＰＨを上記範囲とすることにより、精製水溶性種子系多糖類の低分子化を行わずに、精製水溶性種子系多糖類の水溶性成分と不溶性成分とを容易に分離することができる。なお、上記糊液のＰＨは、ＰＨ試験紙により測定することができる。 The pH of the paste solution prepared in step 2 is preferably 10 or more, more preferably 11 or more. By adjusting the pH of the paste solution to the above range, it is possible to easily separate the water-soluble component and the insoluble component of the purified water-soluble seed-based polysaccharide without lowering the molecular weight of the purified water-soluble seed-based polysaccharide. it can. The pH of the glue solution can be measured with a PH test paper.
以上説明した工程２により、糊液が調製される。 The paste solution is prepared by the step 2 described above.
３．工程３
工程３は、工程２で調製された糊液にアルコールを添加する工程、及び／又は、糊液を冷却する工程である。工程３により、糊液中に精製水溶性種子系多糖類が析出し、上記糊液が、析出した精製水溶性種子系多糖類及び不溶性成分を含む分散液（スラリー）となる。
3. Process 3
Step 3 is a step of adding alcohol to the paste solution prepared in step 2 and / or a step of cooling the paste solution. In step 3, the purified water-soluble seed-based polysaccharide is precipitated in the paste solution, and the paste solution becomes a dispersion (slurry) containing the precipitated purified water-soluble seed-based polysaccharide and the insoluble component.
(アルコール添加)
上記工程２により調製された糊液に、アルコールを添加することにより、糊液中に精製水溶性種子系多糖類が析出する。アルコール添加は、工程２において、溶媒として水、又は、アルコール濃度が低濃度である水とアルコールとの混合溶媒を用いる場合に有効である。すなわち、アルコール添加は、工程２において溶媒として、水、又は、水とアルコールとの混合溶媒を用い、上記混合溶媒中のアルコールの含有量は、混合溶媒を１００質量％として１５質量％未満である場合に有効である。
(Alcohol addition)
By adding alcohol to the paste solution prepared in the above step 2, the purified water-soluble seed-based polysaccharide is precipitated in the paste solution. Addition of alcohol is effective when water or a mixed solvent of water and alcohol having a low alcohol concentration is used as the solvent in step 2. That is, the alcohol addition uses water or a mixed solvent of water and alcohol as a solvent in step 2, and the content of the alcohol in the mixed solvent is less than 15% by mass with the mixed solvent as 100% by mass. It is effective in some cases.
アルコール添加に用いられるアルコールとしては、水と相溶性のあるアルコールであれば特に限定されず、例えば、メタノール、エタノール、イソプロパノール等が挙げられる。アルコール添加に用いられるアルコールとしては、本発明の製造方法によって製造される精製水溶性種子系多糖類の用途に応じたものを適宜選択することができる。例えば、食品、食品添加物、化粧品、医薬部外品等の用途に使用する場合には、エタノールを用いる等、その用途に適したアルコールを用いることが好ましい。 The alcohol used for adding alcohol is not particularly limited as long as it is compatible with water, and examples thereof include methanol, ethanol and isopropanol. As the alcohol used for alcohol addition, one suitable for the use of the purified water-soluble seed-based polysaccharide produced by the production method of the present invention can be appropriately selected. For example, when used for foods, food additives, cosmetics, quasi-drugs, etc., it is preferable to use alcohol suitable for the application such as ethanol.
アルコール添加後の糊液中のアルコールの含有量は、アルコール添加後の糊液を１００質量％として、３０〜７０質量％が好ましく、４０〜６０質量％がより好ましく、５０〜６０質量％が更に好ましい。アルコール添加後の糊液の含有量を上述の範囲とすることにより、糊液中に精製水溶性種子系多糖類をより効率よく析出させることができる。 The content of alcohol in the paste solution after addition of alcohol is preferably 30 to 70% by mass, more preferably 40 to 60% by mass, and further preferably 50 to 60% by mass based on 100% by mass of the paste solution after addition of alcohol. preferable. By setting the content of the paste solution after adding alcohol to the above range, the purified water-soluble seed-based polysaccharide can be more efficiently precipitated in the paste solution.
(冷却)
上記工程２により調製された糊液を冷却することにより、糊液中に精製水溶性種子系多糖類が析出する。冷却は、工程２において、溶媒としてアルコール濃度が高濃度である水とアルコールとの混合溶媒を用いる場合に有効である。即ち、冷却は、工程２において溶媒として水とアルコールとの混合溶媒を用い、上記混合溶媒中のアルコール含有量は、混合溶媒を１００質量％として１５〜６０質量％である場合、好ましくは、１８〜４０質量％である場合に有効である。
(cooling)
By cooling the paste solution prepared in the above step 2, the purified water-soluble seed-based polysaccharide is precipitated in the paste solution. Cooling is effective when a mixed solvent of water and alcohol having a high alcohol concentration is used as the solvent in step 2. That is, the cooling uses a mixed solvent of water and alcohol as a solvent in Step 2, and the alcohol content in the mixed solvent is preferably 15 to 60 mass% when the mixed solvent is 100 mass%, and preferably 18 It is effective when the content is up to 40% by mass.
糊液の冷却温度は、−５〜４０℃が好ましく、１０〜３０℃がより好ましい。糊液の温度を上記範囲とすることにより、糊液中に精製水溶性種子系多糖類をより効率よく析出させることができる。 -5-40 degreeC is preferable and, as for the cooling temperature of a paste solution, 10-30 degreeC is more preferable. By setting the temperature of the paste solution within the above range, the purified water-soluble seed-based polysaccharide can be more efficiently precipitated in the paste solution.
上記冷却により生じる上澄み液は、工程１における溶液の調製時に再利用できる。すなわち、本発明の製造方法において、工程３として冷却のみを行う場合、工程３により生成する分散液（スラリー）の上澄み液と、工程１により調製される溶液との間で、アルコールとアルカリ性化合物との質量比が同一であるので、次回の製造時の工程１において、当該回収した上澄み液を用いて溶液を調製することができる。上記上澄み液を再利用することにより、製造に使用するアルコール及びアルカリ性化合物の量を低減できるので、安価に精製水溶性種子系多糖類を製造することができる。 The supernatant liquid generated by the above cooling can be reused when preparing the solution in step 1. That is, in the production method of the present invention, when only cooling is performed as Step 3, an alcohol and an alkaline compound are added between the supernatant liquid of the dispersion liquid (slurry) produced in Step 3 and the solution prepared in Step 1. Since the mass ratio is the same, it is possible to prepare a solution using the recovered supernatant in step 1 of the next production. By reusing the supernatant, the amounts of alcohol and alkaline compound used in the production can be reduced, so that the purified water-soluble seed-based polysaccharide can be produced at low cost.
本発明の製造方法では、工程３において、上記アルコール添加及び冷却は、どちらか一方を行ってもよいし、両方行ってもよい。特に、上記工程２において、溶媒として水、又は、アルコール濃度が低濃度である水とアルコールとの混合溶媒を用いる場合には、アルコール添加を行った上で冷却を行うことにより、より効率良く精製水溶性種子系多糖類を製造することができる。 In the production method of the present invention, in step 3, the addition of alcohol and the cooling may be performed either one or both. In particular, in the above step 2, when water or a mixed solvent of water and alcohol having a low alcohol concentration is used as the solvent, purification is performed more efficiently by adding alcohol and then cooling. Water-soluble seed-based polysaccharides can be produced.
以上説明した工程３により、精製水溶性種子系多糖類を製造することができる。 The purified water-soluble seed-based polysaccharide can be produced by the step 3 described above.
（中和工程）
本発明の製造方法では、上記工程３の後に、中和工程を有していてもよい。工程３の後に中和工程を行うことにより、析出した精製水溶性種子系多糖類に付着したアルカリ性化合物を中和することができ、より純度の高い精製水溶性種子系多糖類を調製することができる。
(Neutralization process)
The production method of the present invention may have a neutralization step after the above step 3. By performing the neutralization step after step 3, the alkaline compound attached to the precipitated purified water-soluble seed-based polysaccharide can be neutralized, and a purified water-soluble seed-based polysaccharide having a higher purity can be prepared. it can.
上記中和工程で用いられる酸としては、特に限定されず、無機酸、有機酸等を用いることができる。食品等の用途に使用する場合には、クエン酸等、その用途に適した酸を用いるのが好ましい。 The acid used in the neutralization step is not particularly limited, and inorganic acids, organic acids and the like can be used. When used for food applications, it is preferable to use an acid suitable for the application such as citric acid.
中和工程は、工程３の後に行われることが好ましい。中和工程を工程３の後に行うことにより、中和後の糊液の粘度の上昇を抑制できるので撹拌がより容易となる。また、中和工程を工程３の後に行うことにより、工程３により生ずる上澄み液を除去すれば中和によって生成する塩の量が少なくなり、洗浄工程も簡単な洗浄で十分となる点で好ましい。 The neutralization step is preferably performed after step 3. By performing the neutralization step after step 3, it is possible to suppress an increase in the viscosity of the paste solution after the neutralization, and thus the stirring becomes easier. Further, by performing the neutralization step after the step 3, the amount of salt produced by the neutralization is reduced by removing the supernatant liquid generated in the step 3, and the washing step is preferable because simple washing is sufficient.
（洗浄工程）
本発明の製造方法は、上記工程３の後に、洗浄工程を有していてもよい。工程３の後に洗浄工程を行うことにより、精製水溶性種子系多糖類に付着した不溶性成分等を除去することができ、より純度の高い精製水溶性種子系多糖類を調製することができる。洗浄工程は、上記工程３により析出した精製水溶性種子系多糖類を、例えば、濾紙を用いた吸引濾過等の従来より広く知られた方法により濾別して濾過残渣として得た後、当該濾過残渣をアルコール等の揮発性を有する溶剤を添加して洗浄し、再度濾紙により濾別して、濾過残渣を得ることにより行うことができる。
(Washing process)
The production method of the present invention may have a cleaning step after the above step 3. By performing the washing step after the step 3, insoluble components and the like attached to the purified water-soluble seed-based polysaccharide can be removed, and a purified water-soluble seed-based polysaccharide having a higher purity can be prepared. In the washing step, the purified water-soluble seed-based polysaccharide precipitated in the above step 3 is filtered as a filtration residue by a widely known method such as suction filtration using filter paper to obtain a filtration residue. It can be carried out by adding a volatile solvent such as alcohol and washing, and again filtering with a filter paper to obtain a filtration residue.
上記洗浄工程で用いられる溶剤としては、揮発性を有していれば特に限定されず、例えば、メタノール、エタノール、イソプロピルアルコール等のアルコールが挙げられる。揮発性に優れる点で、メタノール及びエタノールを用いることが好ましい。これらの溶剤は、単独で用いてもよいし、２種以上を混合して用いてもよい。 The solvent used in the washing step is not particularly limited as long as it has volatility, and examples thereof include alcohols such as methanol, ethanol and isopropyl alcohol. It is preferable to use methanol and ethanol because of their excellent volatility. These solvents may be used alone or in combination of two or more.
（精製水溶性種子系多糖類）
以上説明した本発明の製造方法により、精製水溶性種子系多糖類を製造することができる。このような精製水溶性種子系多糖類としては、例えば、精製タマリンド種子ガム、精製ガラクトマンナン（精製グアーガム）が挙げられる。
(Purified water-soluble seed-based polysaccharide)
The purified water-soluble seed-based polysaccharide can be produced by the production method of the present invention described above. Examples of such purified water-soluble seed-based polysaccharides include purified tamarind seed gum and purified galactomannan (purified guar gum).
（精製タマリンド種子ガム）
本発明の製造方法により製造された精製タマリンド種子ガムは、様々な用途に用いることができる。上記精製タマリンド種子ガムは、Ｂ型粘度計を用いて２５℃の条件で測定される１．５％水溶液の粘度が１００〜８００ｍＰａ・sであることが好ましく、３００〜８００ｍＰａ・sであることがより好ましい。
(Purified tamarind seed gum)
The purified tamarind seed gum produced by the production method of the present invention can be used for various purposes. In the purified tamarind seed gum, the viscosity of a 1.5% aqueous solution measured with a B-type viscometer at 25 ° C. is preferably 100 to 800 mPa · s, and 300 to 800 mPa · s. More preferable.
上記精製タマリンド種子ガムの１．５％水溶液の、測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃の条件で測定した透過率は、４０％以上が好ましく、５０％以上がより好ましい。上記水溶液の透過率が上述の範囲であることにより、透明性に優れた精製タマリンド種子ガムとなる。 The transmittance of the 1.5% aqueous solution of the purified tamarind seed gum measured at a measurement wavelength of 440 nm, an optical path length of 10 mm, and 25 ° C. is preferably 40% or more, more preferably 50% or more. When the transmittance of the aqueous solution is within the above range, the purified tamarind seed gum has excellent transparency.
上記精製タマリンド種子ガムの用途としては特に限定されないが、上記の特徴を有することから、食品、食品添加物、化粧品、医薬部外品、工業用糊剤等の様々な分野に用いることができる。 The use of the above-mentioned purified tamarind seed gum is not particularly limited, but it can be used in various fields such as foods, food additives, cosmetics, quasi-drugs, and industrial sizing agents because it has the above characteristics.
本発明の製造方法により製造された上記精製タマリンド種子ガムは、従来の精製タマリンド種子ガムが有する特有の植物臭が抑制されている。上記精製タマリンド種子ガムの粉末及び１．５％水溶液は、臭気がほとんど認められないほど低減されているので、食品添加物等の分野に好適に用いることができる。 The above-mentioned purified tamarind seed gum produced by the production method of the present invention suppresses the peculiar vegetable odor of conventional purified tamarind seed gum. Since the powder of the purified tamarind seed gum and the 1.5% aqueous solution have the odor reduced so that almost no odor is observed, they can be suitably used in the field of food additives and the like.
（精製ガラクトマンナン（精製グアーガム））
本発明の製造方法により製造された精製ガラクトマンナン（精製グアーガム）は、様々な用途に用いることができる。上記精製グアーガムは、Ｂ型粘度計を用いて２５℃の条件で測定される１％水溶液の粘度が１００〜５０００ｍＰａ・ｓであることが好ましく、１０００〜５０００ｍＰａ・sであることがより好ましい。
(Purified galactomannan (purified guar gum))
The purified galactomannan (purified guar gum) produced by the production method of the present invention can be used for various purposes. The purified guar gum preferably has a 1% aqueous solution having a viscosity of 100 to 5000 mPa · s, and more preferably 1000 to 5000 mPa · s, measured with a B-type viscometer at 25 ° C.
上記精製グアーガムの１％水溶液の、波長４４０ｎｍ、光路長１０ｍｍ、２５℃の条件で測定した透過率は、４０％以上が好ましく、５０％以上がより好ましい。上記水溶液の透過率が上述の範囲であることにより、透明性に優れた精製グアーガムとなる。 The transmittance of the 1% aqueous solution of the purified guar gum measured under the conditions of a wavelength of 440 nm, an optical path length of 10 mm and 25 ° C is preferably 40% or more, more preferably 50% or more. When the transmittance of the aqueous solution is within the above range, the purified guar gum has excellent transparency.
上記精製グアーガムの用途としては特に限定されない。精製グアーガムは、上記の特徴を有することから、食品、食品添加物、化粧品、医薬部外品、工業用糊剤等の様々な分野に用いることができる。 The use of the purified guar gum is not particularly limited. Since the purified guar gum has the above-mentioned characteristics, it can be used in various fields such as foods, food additives, cosmetics, quasi drugs, and industrial sizing agents.
本発明の製造方法により製造された上記精製グアーガムは、従来の精製グアーガムが有する特有の植物臭が抑制されている。上記精製タマリンド種子ガムの粉末及び１％水溶液は、臭気がほとんど認められないほど低減されているので、食品添加物等の分野に好適に用いることができる。 The above-mentioned purified guar gum produced by the production method of the present invention suppresses the peculiar vegetable odor of conventional purified guar gum. Since the powder of the purified tamarind seed gum and the 1% aqueous solution have the odor reduced so that almost no odor is observed, they can be suitably used in the field of food additives and the like.
なお、本発明の製造方法は、原料として澱粉を用いた場合にも応用できる。澱粉種子又は根塊の粉砕物を原料として本発明の製造方法と同様に処理することにより、部分α化澱粉又は水溶性澱粉を得ることができる。この澱粉の製造方法は、一般に水系で澱粉を処理する方法に比べて、水の使用量を低減できるので、排水処理設備を小さくすることができる。 The production method of the present invention can also be applied when starch is used as a raw material. A partially pregelatinized starch or a water-soluble starch can be obtained by treating a crushed product of starch seeds or root nodules as a raw material in the same manner as in the production method of the present invention. In this starch production method, the amount of water used can be reduced as compared with the method of treating starch generally with an aqueous system, so that the waste water treatment facility can be downsized.
以下に、実施例および比較例を示して本発明を具体的に説明する。但し、本発明は実施例に限定されない。なお、以下の実施例および比較例において、遠心分離は日立製作所製ｈａｉｍａｃ ＳＣＲ２０Ｂを用いて行った。また、粘度は東京計器製ＤＶＬ−Ｂ粘度計を用いて測定を行った。更に、透過率は日立製作所製Ｕ−２０００ダブルビーム分光光度計を用いて測定を行った。 The present invention will be specifically described below with reference to Examples and Comparative Examples. However, the present invention is not limited to the examples. In the following examples and comparative examples, centrifugation was carried out using a haimac SCR20B manufactured by Hitachi Ltd. The viscosity was measured using a DVL-B viscometer manufactured by Tokyo Keiki. Further, the transmittance was measured using a U-2000 double beam spectrophotometer manufactured by Hitachi Ltd.
（実施例１）
３１％メタノール水溶液４６０ｇにカセイソーダ４０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））４０ｇを加え、浴温６０℃で３時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で遠心分離を行った。上澄み液を２５０ｇ取り分けておき、沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ.２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再び、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．２とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して３３ｇの精製タマリンド種子ガムを得た。
(Example 1)
40 g of caustic soda was added to 460 g of 31% methanol aqueous solution, 40 g of tamarind seed gum (Food Made TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and the mixture was stirred at a bath temperature of 60 ° C. for 3 hours to obtain a paste solution. Was prepared. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. The dispersion liquid containing the precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. 250 g of the supernatant was set aside, 200 g of 50% methanol aqueous solution was added to the precipitate, and the mixture was washed with stirring. Then, it was filtered by suction using No. 2 filter paper. After adding 200 g of a 50% aqueous methanol solution to the filtration residue and stirring and washing, No. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.2. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 33 g of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．０％、蛋白分は０．０７％であった。また、１．５％水溶液の粘度は７２８ｍＰａ・s（２５℃、Ｎｏ．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は６７％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１．５％水溶液の臭気は、殆ど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.0% and a protein content of 0.07%. The viscosity of the 1.5% aqueous solution is 728 mPa · s (25 ° C., No. 2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 67% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C.) Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
（実施例２）
実施例１で遠心分離によって得られた上澄み液２５０ｇに３１％メタノール水溶液２３０ｇとカセイソーダ２０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））４０ｇを加え、浴温７０℃で２時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で、遠心分離を行った。沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．０とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して３１ｇの精製タマリンド種子ガムを得た。
(Example 2)
To 250 g of the supernatant obtained by centrifugation in Example 1, 230 g of 31% methanol aqueous solution and 20 g of caustic soda were added, and 40 g of tamarind seed gum (Foodmaid TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was stirred. In addition, a paste solution was prepared by stirring at a bath temperature of 70 ° C. for 2 hours. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. The dispersion liquid containing this precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. After adding 200 g of 50% methanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.0. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 31 g of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．１％、蛋白分は０．０８％であった。また、１．５％水溶液の粘度は６３０ｍＰａ・ｓ（２５℃ 、Ｎｏ．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は５９％（測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.1% and a protein content of 0.08%. The viscosity of the 1.5% aqueous solution is 630 mPa · s (25 ° C, No. 2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 59% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
(実施例３)
３２％エタノール水溶液３７０ｇにカセイソーダ３０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））３０ｇを加え、浴温７０℃で１．５時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で遠心分離を行った。沈澱分に５０％エタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％エタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％エタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．０とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのエタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して２０ｇの精製タマリンド種子ガムの粉末を得た。
(Example 3)
30 g of caustic soda was added to 370 g of 32% ethanol aqueous solution, 30 g of tamarind seed gum (Foodmaid TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and stirred at a bath temperature of 70 ° C. for 1.5 hours. A paste solution was prepared. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. The dispersion liquid containing the precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. After adding 200 g of 50% ethanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. After adding 200 g of 50% aqueous ethanol solution to the filtration residue and washing with stirring, No. 1 was added again. It suction-filtered using the filter paper of 2. 200 g of 50% ethanol aqueous solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.0. This dispersion was It suction-filtered using the filter paper of 2. 200 g of ethanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 20 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．１％、蛋白分は０．０６％であった。また、１．５％水溶液の粘度は６６３ｍＰａ・ｓ（２５℃、Ｎｏ．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は６４％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.1% and a protein content of 0.06%. The viscosity of the 1.5% aqueous solution is 663 mPa · s (25 ° C, No. 2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 64% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
(実施例４)
３２％メタノール水溶液４６０ｇにカセイソーダ４０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））６０ｇを加え、浴温７０℃で１時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を１晩放置した後に、上澄み部分を除去した。残りの沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．１とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて６０℃で乾燥させ、万能粉砕機で粉砕して３５ｇの精製タマリンド種子ガムの粉末を得た。
(Example 4)
40 g of caustic soda was added to 460 g of 32% methanol aqueous solution, and 60 g of tamarind seed gum (Foodmaid TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and the mixture was stirred at a bath temperature of 70 ° C. for 1 hour to obtain a paste solution. Was prepared. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. After leaving the dispersion liquid containing this precipitate overnight, the supernatant portion was removed. After adding 200 g of 50% aqueous methanol solution to the remaining precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.1. This dispersion was It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 60 ° C., and pulverized with a universal pulverizer to obtain 35 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．３％、蛋白分は０．０８％であった。また、１．５％水溶液の粘度は６３３ｍＰａ・ｓ（２５℃、Ｎ０．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は５８％（測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.3% and a protein content of 0.08%. The viscosity of the 1.5% aqueous solution is 633 mPa · s (25 ° C., N0.2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 58% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C.). Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
(実施例５)
３０％メタノール水溶液４５０ｇにカセイソーダ５０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））５０ｇを加え、浴温７０℃で２時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で遠心分離を行った。沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．１とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して３５ｇの精製タマリンド種子ガムの粉末を得た。
(Example 5)
50 g of caustic soda was added to 450 g of a 30% aqueous methanol solution, 50 g of tamarind seed gum (Foodmaid TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and the mixture was stirred for 2 hours at a bath temperature of 70 ° C. Was prepared. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. The dispersion liquid containing the precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. After adding 200 g of 50% methanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.1. This dispersion was It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of methanol was added and stirred, and No. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 35 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．０％、蛋白分は０．０５％であった。また、１．５％水溶液の粘度は７８６ｍＰａ・ｓ（２５℃、Ｎ０．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は６７％（測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.0% and a protein content of 0.05%. The viscosity of the 1.5% aqueous solution is 786 mPa · s (25 ° C, N0.2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 67% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
(実施例６)
３１％メタノール水溶液４５０ｇにカセイソーダ５０ｇを加えて、撹拌しながらタマリンド種子ガム（タマリンドカーネルパウダー）５０ｇを加え、浴温８０℃で２時間撹拌して糊液を調製した。この糊液を撹拌しながら、糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で遠心分離を行った。沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．２とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して３５ｇの精製タマリンド種子ガムの粉末を得た。
(Example 6)
50 g of caustic soda was added to 450 g of 31% aqueous methanol solution, 50 g of tamarind seed gum (tamarind kernel powder) was added with stirring, and the mixture was stirred at a bath temperature of 80 ° C. for 2 hours to prepare a paste solution. While stirring the paste solution, the paste solution was cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower, to obtain a precipitate. The dispersion liquid containing the precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. After adding 200 g of 50% methanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.2. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 35 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１．０％、蛋白分は０．１１％であった。また、１．５％水溶液の粘度は５６６ｍＰａ・ｓ（２５℃、Ｎ０．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は５４％（測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 1.0% and a protein content of 0.11%. The viscosity of the 1.5% aqueous solution is 566 mPa · s (25 ° C, N0.2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 54% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. The odor of the powder and the 1.5% aqueous solution was almost odorless.
(実施例７)
２０％メタノール水溶液３７６ｇにカセイソーダ２４ｇを加えて、撹拌しながらグアーガム２４ｇを加え、浴温８５℃で４時間撹拌して糊液を調製した。この糊液を撹拌しながら液温が１０℃以下になるまで冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、３０００回転、２分間の条件で遠心分離を行った。沈澱分に３０％メタノール水溶液２００ｇを加えてホモジナイザーを用いて５０００回転で１０分間撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に３０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．１とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して１８ｇの精製グアーガムの粉末を得た。
(Example 7)
24 g of caustic soda was added to 376 g of 20% aqueous methanol solution, 24 g of guar gum was added with stirring, and the mixture was stirred at a bath temperature of 85 ° C. for 4 hours to prepare a paste solution. The paste solution was cooled with stirring until the temperature of the solution became 10 ° C. or lower to obtain a precipitate. The dispersion liquid containing the precipitate was centrifuged by a centrifuge under the conditions of 3000 rpm and 2 minutes. After adding 200 g of a 30% aqueous methanol solution to the precipitate and stirring and washing with a homogenizer at 5,000 rpm for 10 minutes, No. It suction-filtered using the filter paper of 2. After adding 200 g of a 30% aqueous methanol solution to the filtration residue and washing with stirring, No. 1 was added again. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.1. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 18 g of purified guar gum powder.
得られた精製グアーガムの物性を測定したところ、１％水溶液の粘度は２０１５ｍＰａ・ｓ（２５℃、Ｎｏ．３スピンドル、３０ｒｐｍ）であり、１％水溶液の透過率は６４％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified guar gum were measured, the viscosity of the 1% aqueous solution was 2015 mPa · s (25 ° C, No. 3 spindle, 30 rpm), and the transmittance of the 1% aqueous solution was 64% (measurement wavelength 440 nm, optical path The length was 10 mm and 25 ° C). Also, the odor of the powder and the 1% aqueous solution was almost odorless.
(実施例８)
１８％エタノール水溶液５８４ｇにカセイソーダ１８ｇを加えて、撹拌しながらグアーガム１８ｇを加え、高圧反応機で１２０℃で２時間撹拌して糊液を調製した。この糊液を撹拌しながら液温が１０℃以下になるまで冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、３０００回転、２分間の条件で遠心分離を行った。沈澱分に２０％エタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２０％エタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％エタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．０とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのエタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して１３ｇの精製グアーガムの粉末を得た。
(Example 8)
18 g of caustic soda was added to 584 g of 18% aqueous ethanol solution, 18 g of guar gum was added with stirring, and the mixture was stirred at 120 ° C. for 2 hours in a high pressure reactor to prepare a paste solution. The paste solution was cooled with stirring until the temperature of the solution became 10 ° C. or lower to obtain a precipitate. The dispersion liquid containing the precipitate was centrifuged by a centrifuge under the conditions of 3000 rpm and 2 minutes. After adding 200 g of 20% ethanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. After adding 200 g of 20% ethanol aqueous solution to the filtration residue and washing with stirring, No. It suction-filtered using the filter paper of 2. 200 g of 50% ethanol aqueous solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.0. This dispersion was It suction-filtered using the filter paper of 2. 200 g of ethanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 13 g of a powder of purified guar gum.
得られた精製グアーガムの物性を測定したところ、１％水溶液の粘度は２４２３ｍＰａ・ｓ（２５℃、Ｎｏ．３スピンドル、３０ｒｐｍ）であり、１％水溶液の透過率は６２％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified guar gum were measured, the viscosity of the 1% aqueous solution was 2423 mPa · s (25 ° C, No. 3 spindle, 30 rpm), and the transmittance of the 1% aqueous solution was 62% (measurement wavelength 440 nm, optical path The length was 10 mm and 25 ° C). Also, the odor of the powder and the 1% aqueous solution was almost odorless.
(実施例９)
２０％メタノール水溶液３７６ｇにカセイソーダ２４ｇを加えて、撹拌しながらローカストビーンガム２４ｇを加え、浴温８５℃で４時間撹拌して糊液を調製した。この糊液を撹拌しながら液温が１０℃以下になるまで冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、３０００回転、２分間の条件で遠心分離を行った。沈澱分に３０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に３０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．０とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して１６ｇの精製ローカストビーンガムの粉末を得た。
(Example 9)
24 g of caustic soda was added to 376 g of 20% aqueous methanol solution, 24 g of locust bean gum was added with stirring, and the mixture was stirred at a bath temperature of 85 ° C. for 4 hours to prepare a paste solution. The paste solution was cooled with stirring until the temperature of the solution became 10 ° C. or lower to obtain a precipitate. The dispersion liquid containing the precipitate was centrifuged by a centrifuge under the conditions of 3000 rpm and 2 minutes. After adding 200 g of a 30% aqueous methanol solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. After adding 200 g of a 30% aqueous methanol solution to the filtration residue and washing with stirring, No. 1 was added again. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.0. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 16 g of purified locust bean gum powder.
得られた精製ローカストビーンガムの物性を測定したところ、１％水溶液の粘度は２４５７ｍＰａ・ｓ（２５℃、Ｎｏ．３スピンドル、３０ｒｐｍ）であり、１％水溶液の透過率は６１％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１％水溶液の臭気はほとんど無臭であった。 When the physical properties of the obtained purified locust bean gum were measured, the viscosity of the 1% aqueous solution was 2457 mPa · s (25 ° C, No. 3 spindle, 30 rpm), and the transmittance of the 1% aqueous solution was 61% (measurement wavelength 440 nm. , Optical path length 10 mm, 25 ° C.). Also, the odor of the powder and the 1% aqueous solution was almost odorless.
（実施例１０）
２０％メタノール水溶液３７６ｇにカセイソーダ２４ｇを加えて、撹拌しながらローカストビーンガム２４ｇを加え、浴温８５℃で４時間撹拌して糊液を調製した。この糊液を撹拌しながら液温が１０℃以下になるまで冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、３０００回転、２分間の条件で遠心分離を行った。沈澱分に３０％メタノール水溶液２００ｇを加えてホモジナイザーを用いて５０００回転で１０分間撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に３０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌しながらクエン酸を添加して、中和してＰＨを７．２とした。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して１５ｇの精製ローカストビーンガムの粉末を得た。
(Example 10)
24 g of caustic soda was added to 376 g of 20% aqueous methanol solution, 24 g of locust bean gum was added with stirring, and the mixture was stirred at a bath temperature of 85 ° C. for 4 hours to prepare a paste solution. The paste solution was cooled with stirring until the temperature of the solution became 10 ° C. or lower to obtain a precipitate. The dispersion liquid containing the precipitate was centrifuged by a centrifuge under the conditions of 3000 rpm and 2 minutes. After adding 200 g of a 30% aqueous methanol solution to the precipitate and stirring and washing with a homogenizer at 5,000 rpm for 10 minutes, No. It suction-filtered using the filter paper of 2. After adding 200 g of a 30% aqueous methanol solution to the filtration residue and washing with stirring, No. 1 was added again. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and citric acid was added with stirring to neutralize the pH to 7.2. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 15 g of powder of purified locust bean gum.
得られた精製ローカストビーンガムの物性を測定したところ、１％水溶液の粘度は２２６０ｍＰａ・ｓ（２５℃、Ｎｏ．３スピンドル、３０ｒｐｍ）であり、１％水溶液の透過率は６２％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１％水溶液の臭気はほとんど無臭であった When the physical properties of the obtained purified locust bean gum were measured, the viscosity of the 1% aqueous solution was 2260 mPa · s (25 ° C, No. 3 spindle, 30 rpm), and the transmittance of the 1% aqueous solution was 62% (measurement wavelength 440 nm. , Optical path length 10 mm, 25 ° C.). The odor of the powder and the 1% aqueous solution was almost odorless.
(実施例１１)
３１％メタノール水溶液４６０ｇにカセイソーダ４０ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））４０ｇを加え、浴温６０℃で３時間撹拌して糊液を調製した。この糊液を撹拌しながら、５０％クエン酸７０ｇを加えて、中和してＰＨを７．１とした。この糊液は餅状となり、冷却しても沈澱は析出しなかったので、５０％メタノール水溶液３００ｇを加えてアルコール沈澱させ、ホモジナイザーを用いて８０００回転で、１０分間撹拌して沈澱分を得た。この沈澱分をＮｏ.２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再び、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌洗浄し、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して４３ｇの精製タマリンド種子ガムを得た。
(Example 11)
40 g of caustic soda was added to 460 g of 31% methanol aqueous solution, 40 g of tamarind seed gum (Food Made TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and the mixture was stirred at a bath temperature of 60 ° C. for 3 hours to obtain a paste solution. Was prepared. While stirring this paste solution, 70 g of 50% citric acid was added to neutralize the pH to 7.1. Since this paste solution became dough-like and no precipitate was formed even when cooled, 300 g of a 50% methanol aqueous solution was added to cause alcohol precipitation, and the precipitate was obtained by stirring for 10 minutes at 8000 rpm using a homogenizer. .. The precipitate was filtered off with suction using No. 2 filter paper. After adding 200 g of a 50% aqueous methanol solution to the filtration residue and stirring and washing, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 43 g of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は１４．１％、蛋白分は０．０８％であった。また、１．５％水溶液の粘度は２５４ｍＰａ・s（２５℃、Ｎｏ．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は４９％（測定波長４４０ｎｍ、光路長１０mm、２５℃）であった。また、粉末および１．５％水溶液の臭気はほとんど無臭であったが、灰分が若干多く、粘度の低い製品であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 14.1% and a protein content of 0.08%. The viscosity of the 1.5% aqueous solution is 254 mPa · s (25 ° C, No. 2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 49% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. Further, although the powder and the 1.5% aqueous solution had almost no odor, the product had a small amount of ash and a low viscosity.
（比較例１）
３０％メタノール水溶液５００ｇに、撹拌しながらタマリンド種子ガム（タマリンドカーネルパウダー）５０ｇを加え、浴温８０℃で２時間撹拌して糊液を調製した。この糊液を撹拌しながら、５０％メタノール水溶液２００ｇを加えて糊液の温度が３９℃以下になるまで約３０分間冷却して析出物を得た。この析出物を含んだ分散液を、遠心分離機により、２０００回転、２分間の条件で遠心分離を行った。沈澱分に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて撹拌洗浄した後に、再びＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に５０％メタノール水溶液２００ｇを加えて、撹拌洗浄した。この分散液をＮｏ．２の濾紙を用いて吸引濾別した。濾過残渣に２００ｇのメタノールを加えて撹拌洗浄し、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて５０℃で乾燥させ、万能粉砕機で粉砕して２８ｇの精製タマリンド種子ガムの粉末を得た。
(Comparative Example 1)
To 500 g of a 30% aqueous methanol solution, 50 g of tamarind seed gum (tamarind kernel powder) was added with stirring, and the mixture was stirred at a bath temperature of 80 ° C. for 2 hours to prepare a paste solution. While stirring the paste solution, 200 g of a 50% aqueous methanol solution was added and cooled for about 30 minutes until the temperature of the paste solution became 39 ° C. or lower to obtain a precipitate. The dispersion liquid containing the precipitate was subjected to centrifugal separation under conditions of 2000 rpm and 2 minutes by a centrifuge. After adding 200 g of 50% methanol aqueous solution to the precipitate and washing with stirring, No. It suction-filtered using the filter paper of 2. To the filtration residue, 200 g of 50% aqueous methanol solution was added, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. 200 g of 50% aqueous methanol solution was added to the filtration residue, and the mixture was washed with stirring. This dispersion was It suction-filtered using the filter paper of 2. 200 g of methanol was added to the filtration residue, and the mixture was washed with stirring. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 50 ° C., and ground with a universal grinder to obtain 28 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は０．４％、蛋白分は１．８５％であった。また、１．５％水溶液の粘度は７６０ｍＰａ・ｓ（２５℃、Ｎ０．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は８％（測定波長４４０ｎｍ、光路長１０ｍｍ、２５℃）であった。また、粉末および１．５％水溶液の臭気は、かなり原料由来の臭気が残っていた。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 0.4% and a protein content of 1.85%. The viscosity of the 1.5% aqueous solution is 760 mPa · s (25 ° C., N0.2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 8% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C.). Met. In addition, the odor of the powder and the 1.5% aqueous solution was considerably odor derived from the raw materials.
（比較例２）
５０％イソプロピルアルコール水溶液２００ｇにカセイソーダ２ｇを加えて、撹拌しながらタマリンド種子ガム（シキボウ（株）製 フードメイドＴＡ−１００（商品名））２０ｇを加え、浴温８５℃で３０分撹拌した。３０分後、分散液を塩酸でＰＨ６．５に調製した後に、ＪＩＳ標準フルイ８８μｍ（目開き８８μｍ）の篩を用いて分散液を濾別した。篩残渣分に５０％イソプロピルアルコール水溶液１００ｇを加えて１０分間撹拌洗浄した後に、Ｎｏ．２の濾紙を用いて吸引濾別した。濾過残渣をバットに広げて６０℃で乾燥させ、万能粉砕機で粉砕して１７ｇの精製タマリンド種子ガムの粉末を得た。
(Comparative example 2)
2 g of caustic soda was added to 200 g of a 50% isopropyl alcohol aqueous solution, and 20 g of tamarind seed gum (Foodmaid TA-100 (trade name) manufactured by Shikibo Co., Ltd.) was added with stirring, and the mixture was stirred at a bath temperature of 85 ° C. for 30 minutes. After 30 minutes, the dispersion was adjusted to pH 6.5 with hydrochloric acid, and then the dispersion was filtered using a JIS standard sieve 88 μm (opening 88 μm) sieve. After adding 100 g of 50% isopropyl alcohol aqueous solution to the residue of the sieve and stirring and washing for 10 minutes, No. It suction-filtered using the filter paper of 2. The filtration residue was spread on a vat, dried at 60 ° C., and pulverized with a universal pulverizer to obtain 17 g of powder of purified tamarind seed gum.
得られた精製タマリンド種子ガムの物性を測定したところ、生成物の灰分は２．０％、蛋白分は０．０７％であった。また、１．５％水溶液の粘度は３７５ｍＰａ・ｓ（２５℃、Ｎｏ．２スピンドル、３０ｒｐｍ）であり、１．５％水溶液の透過率は３５％（測定波長４４０ｎｍ，光路長１０mm、２５℃）であった。また、粉末および水溶液の臭気はわずかに認められる程度であった。 When the physical properties of the obtained purified tamarind seed gum were measured, the product had an ash content of 2.0% and a protein content of 0.07%. The viscosity of the 1.5% aqueous solution is 375 mPa · s (25 ° C, No. 2 spindle, 30 rpm), and the transmittance of the 1.5% aqueous solution is 35% (measurement wavelength 440 nm, optical path length 10 mm, 25 ° C). Met. In addition, the odor of the powder and the aqueous solution was slightly recognized.
Claims (8)
（１）水溶性種子系多糖類原料、水又は水とアルコールとの混合溶媒、及びアルカリ性化合物を含有する溶液を調製する工程１、
（２）前記溶液を加熱糊化して糊液を調製する工程２、並びに
（３）前記糊液にアルコール添加及び／又は糊液の冷却を行う工程３
を有する、ことを特徴とする製造方法。 A method for producing a purified water-soluble seed-based polysaccharide,
(1) Step 1 of preparing a solution containing a water-soluble seed-based polysaccharide raw material, water or a mixed solvent of water and alcohol, and an alkaline compound,
(2) Step 2 of preparing the paste solution by heating and gelatinizing the solution, and (3) Step 3 of adding alcohol to the paste solution and / or cooling the paste solution.
A manufacturing method comprising:
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