JP2005073695A - Highly dispersible whey calcium composition and method for producing the same - Google Patents
Highly dispersible whey calcium composition and method for producing the same Download PDFInfo
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- JP2005073695A JP2005073695A JP2004055659A JP2004055659A JP2005073695A JP 2005073695 A JP2005073695 A JP 2005073695A JP 2004055659 A JP2004055659 A JP 2004055659A JP 2004055659 A JP2004055659 A JP 2004055659A JP 2005073695 A JP2005073695 A JP 2005073695A
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- Prior art keywords
- calcium
- whey
- gum
- whey calcium
- milk
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Images
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/10—Drying, dehydrating
Abstract
Description
本発明は、冷水可溶性で沈澱が起こらない高分散性天然乳清カルシウム組成物及びその製造方法に関し、さらに詳しくは、天然乳清カルシウムを粉砕機で超微粒子に粉砕した後、表面コーティングによって、加温しなくても冷水に直ちに溶け且つ沈澱が起こらない高分散性の天然乳清カルシウム製剤とその組成物を製造することにより、牛乳類や発酵乳類、乳クリーム類、バター類、チーズ類、粉乳類などの乳加工品、パン類や乾果類、キャンディ類、チョコレット類、ガム類、ジャム類などのお菓子類、アイスクリーム製品類、食肉・魚肉製品類、豆腐（蒟蒻）類、麺類、豆乳類などの飲料類、特殊栄養食品類、健康補助食品類、調味食品及びその他の食品類の全般にわたってカルシウム補充用として使用でき、歯磨きなどの生活用品、化粧品及び医薬品の原料としても使用できる、高分散性であって、添加量を高めて長期間放置しても分散安定性が高い高分散性乳清カルシウム組成物及びその製造方法に関する。 The present invention relates to a highly dispersible natural whey calcium composition that is soluble in cold water and does not cause precipitation, and more particularly to a method for producing the same. More specifically, natural whey calcium is pulverized into ultrafine particles by a pulverizer and then applied by surface coating. By producing a highly dispersible natural whey calcium preparation and its composition that dissolves immediately in cold water without precipitation and does not cause precipitation, milk, fermented milk, milk cream, butters, cheeses, Milk products such as powdered milk, breads and dried fruits, candy, chocolatelets, gums, jams and other sweets, ice cream products, meat and fish products, tofu (boiled rice), noodles Can be used as a calcium supplement throughout beverages such as soy milk, special nutrition foods, health supplements, seasoning foods and other foods. Can also be used as a raw material for goods and medicines, a highly dispersible, the addition amount for a long time even when left high dispersion stability highly dispersible whey calcium composition enhances and a manufacturing method thereof.
最近、医学の発達に伴って高齢化社会が到来することにより、人間の平均寿命が延長されたが、骨多孔性、リューマチ、関節炎などの退行性疾患に苦しまれる患者が急増している実情である。このため、高齢化による退行性疾患などの予防、緩和及び治療に効果のある製剤の開発が要求されている。また、カルシウム摂取量の不足が成長期の子供と老人などで著しいと指摘されている。かかる問題点を解決するために、カルシウム強化食品等が開発・販売されている。カルシウムを強化する目的で乳酸カルシウムや塩化カルシウムなどの水溶性の無機又は有機酸カルシウムと、炭酸カルシウムや燐酸カルシウム、卵殻カルシウム、牛骨カルシウム、乳清カルシウム、珊瑚カルシウム、海藻カルシウムなどの水不溶性の無機カルシウムが添加されている。 Recently, with the advent of an aging society with the development of medicine, the average life span of human beings has been extended, but the number of patients suffering from degenerative diseases such as bone porosity, rheumatism, and arthritis is rapidly increasing. is there. For this reason, there is a demand for the development of a preparation effective for prevention, alleviation and treatment of degenerative diseases due to aging. In addition, it has been pointed out that lack of calcium intake is remarkable in growing children and the elderly. In order to solve this problem, calcium-enriched foods and the like have been developed and sold. Water-insoluble inorganic or organic acid calcium such as calcium lactate or calcium chloride and water insoluble such as calcium carbonate, calcium phosphate, eggshell calcium, cow bone calcium, whey calcium, salmon calcium, seaweed calcium for the purpose of strengthening calcium Inorganic calcium is added.
ところが、水溶性の有機酸カルシウムは、遊離されたカルシウムイオンが食品、特に乳製品中の蛋白質と結合して網状構造の蛋白質の巨大分子を形成して沈澱することにより、蛋白質の安定性を阻害し且つ苦味などの異味が発生するため、一定量以上の添加が不可能であって多量の使用ができなくなる。 However, water-soluble organic acid calcium inhibits protein stability by releasing calcium ions that bind to proteins in food, especially dairy products, to form and precipitate macromolecular macromolecular proteins. In addition, since an unpleasant taste such as a bitter taste is generated, addition of a certain amount or more is impossible, and a large amount cannot be used.
一方、水に溶けない炭酸カルシウム、燐酸カルシウム、卵殻カルシウム、牛骨カルシウム、乳清カルシウム、珊瑚カルシウム及び海藻カルシウムなどは、カルシウムイオンが遊離されないので蛋白質との結合が起こらないため、蛋白質の安定性に問題が生ずることなく多量の添加が可能である。しかし、このような無機カルシウムは全般的に比重が高くて乳製品中に分散させる場合、短時間内に沈澱するため、この沈澱などが食品の美観と製品の特性に悪影響を与えることにより、添加量が制限されて多量に使用できないという欠点がある。 On the other hand, calcium carbonate, calcium phosphate, eggshell calcium, bovine bone calcium, whey calcium, salmon calcium, and seaweed calcium, which are not soluble in water, are not released from calcium ions and thus do not bind to protein, so that protein stability A large amount can be added without causing any problems. However, such inorganic calcium generally has a high specific gravity, and when it is dispersed in dairy products, it precipitates within a short period of time, so this precipitation can affect the aesthetics of the food and the properties of the product. There is a disadvantage that the amount is limited and cannot be used in large quantities.
水不溶性のカルシウムを安全に懸濁させる試みが行われてきたが、その例としては、炭酸カルシウムを親水性のエマルジョン化剤で処理することを含む方法（特許文献１参照）、酸素酸と共にやや水溶性のカルシウム塩を撹拌して平均粒径１μｍのカルシウム塩を製造し、次に生成された化合物に親水性エマルジョン化剤を加えることを含む方法（特許文献２参照）、及び高圧均質機で炭酸カルシウム及びエマルジョン化剤の混合物を処理し、混合物を微分散させることを含む方法（特許文献３参照）がある。水不溶性のカルシウム塩が前記例示方法中の一つによって微分散されるとき、沈降速度は遅いが、一定の時間放置後に沈降が起こって硬質のケーキを形成するので、懸濁状態を再び得ることは難しくなる。 Attempts have been made to safely suspend water-insoluble calcium. Examples thereof include a method comprising treating calcium carbonate with a hydrophilic emulsifying agent (see Patent Document 1), and somewhat with oxygen acid. In a method comprising stirring a water-soluble calcium salt to produce a calcium salt having an average particle size of 1 μm, and then adding a hydrophilic emulsifying agent to the resulting compound (see Patent Document 2), and a high-pressure homogenizer There is a method (see Patent Document 3) including treating a mixture of calcium carbonate and an emulsifying agent and finely dispersing the mixture. When a water-insoluble calcium salt is finely dispersed by one of the above exemplary methods, the sedimentation rate is slow, but sedimentation occurs after standing for a certain time to form a hard cake, so that a suspended state is obtained again. Becomes difficult.
ヨーグルト、チーズ、牛乳などといった乳製品の食品添加用としての無機カルシウム剤スラリーの製造方法としては、結晶セルロースを同時に添加してその網状構造によって炭酸カルシウムの粒子を支持させる方法（特許文献４参照）、及びスラリー状の炭酸カルシウム又はスラリー状の炭酸カルシウムにＨＬＢ１０以上の親水性乳化剤を添加したものに超音波を照射して炭酸カルシウムの分散性を改良する方法（特許文献５参照）などが提案されている。ところが、特許文献４のように結晶セルロースを添加する方法は、製品の粘度が非常に高くなるため、食感と製品特性の変化などで好ましくなく、超音波を照射する方法は、熱が発生するため、温度制御を行わなければならず、人為的な分散に多大な時間と費用を必要とするので、好ましい方法とは言えない。 As a method for producing an inorganic calcium preparation slurry for food addition of dairy products such as yogurt, cheese, milk, etc., a method in which crystalline cellulose is added simultaneously and calcium carbonate particles are supported by the network structure (see Patent Document 4). And a method of improving the dispersibility of calcium carbonate by irradiating ultrasonic waves to slurry-like calcium carbonate or slurry-like calcium carbonate to which a hydrophilic emulsifier of HLB 10 or more is added (see Patent Document 5), etc. ing. However, the method of adding crystalline cellulose as in Patent Document 4 is not preferable due to changes in texture and product characteristics because the viscosity of the product is very high, and the method of irradiating ultrasonic waves generates heat. Therefore, temperature control must be performed, and a great deal of time and expense is required for artificial dispersion, which is not a preferable method.
また、特許文献５のように、炭酸カルシウムスラリーにショ糖脂肪酸エステルを添加剤として用いて分散させる方法は、牛乳のような中性又は弱酸性製品に対して僅かなある程度有効な効果を示すのに過ぎず、ロングライフ牛乳などの長期間保存可能食品への添加が可能な平均粒径０．３μｍ未満の極めて分散性の良いカルシウム剤スラリーの製造が困難で、ヨーグルトのような酸性製品ではショ糖脂肪酸エステルが酸に対して不安定な状態になるので、分散性が低下するという欠点のため、好ましくない。 Further, as disclosed in Patent Document 5, the method of dispersing sucrose fatty acid ester as an additive in a calcium carbonate slurry exhibits a slightly effective effect to neutral or weakly acidic products such as milk. However, it is difficult to produce an extremely dispersible calcium agent slurry having an average particle size of less than 0.3 μm that can be added to foods that can be stored for a long period of time such as long-life milk. Since the sugar fatty acid ester becomes unstable with respect to the acid, it is not preferable due to the disadvantage that the dispersibility is lowered.
また、これらの方法は、水分散液中の炭酸カルシウム固形粉の濃度が１０重量％前後と非常に低いため、包装時の輸送容器費用及び流通費の上昇をもたらし、製品の形態が液状なので腐敗し易いため、流通期限が短縮し、常に冷蔵流通及び冷蔵保管が必要であって経済的損失が増加し、好ましい方法とは言えない。 In addition, these methods have a very low concentration of calcium carbonate solid powder in the aqueous dispersion of about 10% by weight, which leads to an increase in transportation container costs and distribution costs at the time of packaging. Therefore, the circulation deadline is shortened, and refrigerated distribution and refrigerated storage are always required, resulting in an increase in economic loss, which is not a preferable method.
また、特許文献６には、ＨＬＢ１６のショ糖ステアリン酸エステルおよび燐酸カルシウムの混合物を特定の条件の下で湿式粉砕して燐酸カルシウム分散体を調製する製造方法が開示されており、特許文献７には、ＨＬＢ１６のショ糖ステアリン酸エステル又は炭酸カルシウムの混合物を同一の方法で湿式粉砕して炭酸カルシウム分散体を調製する製造方法が開示されている。 Patent Document 6 discloses a production method for preparing a calcium phosphate dispersion by wet-grinding a mixture of HLB16 sucrose stearate and calcium phosphate under specific conditions. Discloses a production method of preparing a calcium carbonate dispersion by wet-grinding a mixture of HLB16 sucrose stearate or calcium carbonate by the same method.
前記湿式粉砕機を用いて製造された乳液は、保存中に炭酸カルシウムが分解されるか、液性がアルカリ性である場合、エステルの加水分解が起こって時間が経過するほど粘度が上昇するため、分散液製造後から２日以内に牛乳などの飲料に添加しなければならず、長期保存が困難であった。また、これらの方法は、平均粒径０．３μｍ未満の極めて分散性の良いカルシウム剤スリラーの製造は可能であるが、提案されているカルシウム剤スラリーのカルシウム剤固形分の濃度は約１０重量％に過ぎず、特許文献５の提案の如く設備費、流通経費などの面からみて満足すべき方法とは言えない。 When the emulsion produced using the wet pulverizer is decomposed during storage or the liquidity is alkaline, the viscosity increases as time passes by hydrolysis of the ester, It had to be added to beverages such as milk within 2 days after the dispersion was produced, and long-term storage was difficult. In addition, these methods can produce a calcium agent chiller having an average particle size of less than 0.3 μm and a very good dispersibility, but the concentration of the calcium agent solid content in the proposed calcium agent slurry is about 10% by weight. However, it is not a satisfactory method in terms of equipment costs and distribution costs as proposed in Patent Document 5.
そして、特許文献８には、燐脂質及び蛋白分解物からなる群から選ばれる少なくとも１種を炭酸カルシウムに添加して湿式粉砕を行い、分散性を改良する方法が提案されている。ところが、燐脂質又は蛋白分解物を添加する方法では、燐脂質に特有の異臭と苦味があるため、風味に悪影響を与えるだけでなく、平均粒径１〜３μｍのカルシウム分散液が得られる。この方法で得られた炭酸カルシウムを添加した牛乳は、その製造工程中に遠心分離機における炭酸カルシウムの収率が悪く、食品中に沈澱し易いうえ、ロングライフ牛乳などの長期保存可能食品への添加が不可能である。 Patent Document 8 proposes a method of improving dispersibility by adding at least one selected from the group consisting of phospholipids and protein degradation products to calcium carbonate and performing wet grinding. However, in the method of adding phospholipids or proteolysates, there is a bad smell and bitterness peculiar to phospholipids, so that not only the flavor is adversely affected, but also a calcium dispersion having an average particle size of 1 to 3 μm is obtained. Milk obtained by adding calcium carbonate obtained by this method has a poor yield of calcium carbonate in the centrifuge during the production process, and is easily precipitated in food, and can be used for long-term storable foods such as long-life milk. Addition is impossible.
また、特許文献９には、ＨＬＢ１６のショ糖ステアリン酸エステルおよび燐酸カルシウム又は炭酸カルシウムの混合物からなるカルシウム剤スラリーをスプレードライヤなどの乾燥機を用いて乾燥粉末を製造する方法が提案されているが、乾燥原料としてのカルシウム剤スラリーのカルシウム剤固形分の濃度は１０重量％程度の低濃度であり、乾燥エネルギーだけでなく、乾燥機設備の投資の面においても改善されるべき問題点を有している。 Patent Document 9 proposes a method for producing a dry powder from a calcium agent slurry comprising a mixture of sucrose stearate ester of HLB16 and calcium phosphate or calcium carbonate using a dryer such as a spray dryer. In addition, the concentration of calcium agent solids in the calcium agent slurry as a dry raw material is a low concentration of about 10% by weight, which has problems to be improved not only in drying energy but also in the investment of dryer equipment. ing.
また、特許文献１０には、ＨＬＢ１０のショ糖脂肪酸エステル又は炭酸カルシウム混合物を、特許文献１１には、炭酸カルシウム、燐酸カルシウム及びピロ燐酸第２鉄からなる群より少なくとも１種にアルギン酸プロピレングリコールエステル（ＰＧＡ）を加えた混合物を、特許文献１２には、炭酸カルシウム、燐酸カルシウム及びピロ燐酸第２鉄からなる群より少なくとも１種にアラビアガムと親油性乳化剤を加えた混合物を、それぞれ湿式粉砕機で湿式粉砕して炭酸カルシウム分散体を調製する方法が提案されているが、これらの方法は、平均粒径０．３μｍ未満の極めて分散性の良いカルシウム剤スラリーの製造は可能であるが、カルシウム剤スラリーのカルシウム剤固形分の濃度は約１０重量％に過ぎず、設備費、流通経費などの面において満足すべきではなく、スプレードライヤなどの乾燥機を用いて乾燥粉末を製造する方法が提案されている。 Patent Document 10 discloses sucrose fatty acid ester or calcium carbonate mixture of HLB10, and Patent Document 11 discloses propylene glycol alginate (at least one selected from the group consisting of calcium carbonate, calcium phosphate and ferric pyrophosphate ( PGA) is a mixture of at least one selected from the group consisting of calcium carbonate, calcium phosphate and ferric pyrophosphate with a mixture of gum arabic and lipophilic emulsifier in a wet pulverizer. Methods for preparing a calcium carbonate dispersion by wet pulverization have been proposed. These methods can produce a calcium agent slurry having an average particle size of less than 0.3 μm and extremely good dispersibility. The concentration of solids of calcium agent in the slurry is only about 10% by weight. Not satisfactory Oite, a method of producing a dry powder using a dryer such as a spray dryer has been proposed.
最近、牛乳やヨーグルト、チーズなどの乳製品及び豆乳やジュースなどの液体食品を長期間保存することが可能な容器および保存方法などの開発及び発展に伴い、その食品を販売店、自動販売機、家庭用冷蔵庫等で長期間保存するケースが増加している。これらの食品にカルシウム強化の目的で添加される炭酸カルシウムの粒子は、その食品中における分散状態が極めて良好でない場合、長期間の液体食品の保存期間内に食品容器の底部に沈澱する。このため、食品類を飲用したとき、その沈澱物が飲用者に不快感及び不清潔感を与えることが多くなっている。 Recently, with the development and development of containers and storage methods that can store dairy products such as milk, yogurt and cheese and liquid foods such as soy milk and juice for a long period of time, Cases of long-term storage in home refrigerators and the like are increasing. When the dispersion state in the food is not very good, the calcium carbonate particles added to these foods for the purpose of strengthening calcium precipitate at the bottom of the food container within the storage period of the long-term liquid food. For this reason, when foods are drunk, the precipitates often give the drinker an uncomfortable feeling and an unclean feeling.
したがって、従来の技術により調製された炭酸カルシウムと燐酸カルシウムなどの無機粒子をカルシウム強化の目的で添加した市販の液体食品類は、その無機粒子が食品中において短い分散安定期間をもつため、その無機粒子の添加量が極少量に制限されるべきであり、また一般消費者の購入後から１〜２日以内に消費されるようにしなければならないという欠点がある。 Therefore, commercially available liquid foods to which inorganic particles such as calcium carbonate and calcium phosphate prepared by conventional techniques are added for the purpose of strengthening calcium have a short dispersion stability period in the food. The added amount of the particles should be limited to a very small amount, and there is a disadvantage that it should be consumed within 1 to 2 days after purchase by a general consumer.
また、現在カルシウム強化の目的で使用されている高分散性のカルシウム製剤の中でも、炭酸カルシウムと燐酸カルシウムなどは、その起源が化学的合成によって生成されたカルシウムなので消費者の認知度が低く、食品添加物中の化学的合成品なのでその使用の限界範囲があるうえ、体内吸収率（一般に１４％以下）も非常に低い。 Also, among the highly dispersible calcium preparations currently used for the purpose of calcium fortification, calcium carbonate and calcium phosphate, etc. are low in consumer awareness because their origins are chemically synthesized calcium. Since it is a chemically synthesized product in an additive, its use is limited, and the absorption rate in the body (generally 14% or less) is very low.
したがって、天然乳清カルシウムがカルシウム強化の目的で使用されるところ、天然乳清カルシウムは、牛乳中に存在する無機質を非焼成方法で製造する良質のカルシウム源であり、他のカルシウム源より体内吸収率が非常に高く、カルシウムと燐の割合が適当であって体内吸収を促進させ、何よりも牛乳由来の天然カルシウム源なので消費者の認知度が高くて、健康補助食品及び栄養補充用食品のカルシウム補充用として広く用いられている。ところが、天然乳清カルシウムは、良質のカルシウム源であるが、食品類に使用するとき、分散性が極めて不安定であって沈澱を形成することにより、その食品類の品質低下及び製品の特性変化をもたらし、その沈澱物が飲用者に不快感を与えることが多いという欠点を抱えている。
したがって、本発明の目的は、かかる従来の技術の問題点、諸般事項及び実情を鑑みて創案されたもので、天然乳清カルシウムを粉砕機で超微粒子に粉砕した後、表面のコーティングによって、加温しなくても冷水に直ちに溶け且つ沈澱が起こらない高分散性の天然乳清カルシウム組成物およびその製造方法を提供することにある。 Accordingly, the object of the present invention was devised in view of the problems, general matters and actual situations of the conventional technology. After natural whey calcium is pulverized into ultrafine particles by a pulverizer, it is added by surface coating. An object of the present invention is to provide a highly dispersible natural whey calcium composition that dissolves immediately in cold water and does not cause precipitation even if it is not warm, and a method for producing the same.
本発明の他の目的は、牛乳類や発酵乳類、乳クリーム類、バター類、チーズ類、粉乳類などの乳加工品、パン類や乾果類、キャンディ類、チョコレット類、ガム類、ジャム類などのお菓子類、アイスクリーム製品類、食肉・魚肉製品類、豆腐（蒟蒻）類、麺類、豆乳類などの飲料類、特殊栄養食品類、健康補助食品類、調味食品及びその他の食品類の全般にわたってカルシウム補充用として使用でき、歯磨きなどの生活用品、化粧品及び医薬品の原料としても使用できる、高分酸性であって、添加量を高めて長期間放置しても分散安定性が高い高分散性乳清カルシウム組成物及びその製造方法を提供する。 Other objects of the present invention are milk products, fermented milks, milk creams, butters, cheeses, milk products such as milk powder, breads and dried fruits, candy, chocolates, gums, jams. And other sweets, ice cream products, meat and fish products, tofu (boiled) products, beverages such as noodles, soy milk, special nutrition foods, health supplements, seasoning foods and other foods It can be used as a calcium supplement throughout, and can be used as a raw material for daily items such as toothpaste, cosmetics and pharmaceuticals. Dispersible whey calcium composition and method for producing the same are provided.
上記目的を達成するための本発明は、天然の乳清カルシウム粉末に水を加えた後、撹拌混合して水和物を形成させる水和過程と、前記水和過程で形成された水和物に含まれた乳清カルシウム粒子を粉砕機で粉砕させる粉砕過程と、乳清カルシウムが粒径０．０００１〜５．０μｍの超微粒子となるように粒度を調節するスラリー製造過程と、スラリー中の超微粒子の乳清カルシウム粒子が互いに縮合しないように、超微粒子の表面に分散及びコーティング剤でコーティングさせるコーティング過程と、スラリー中に含まれている異物を除去する異物除去過程と、濃縮して液状の含有物を製造する濃縮過程と、濃縮過程を経た液状の含有物を乾燥させて粉末化する粉末化過程とを含んでなる高分散性乳清カルシウム組成物の製造方法を提供する。 In order to achieve the above object, the present invention provides a hydration process in which water is added to natural whey calcium powder and then mixed by stirring to form a hydrate, and the hydrate formed in the hydration process. A pulverization process in which the whey calcium particles contained in the powder are pulverized by a pulverizer, a slurry production process in which the particle size is adjusted so that the whey calcium becomes ultrafine particles having a particle diameter of 0.0001 to 5.0 μm, In order to prevent the ultra-fine whey calcium particles from condensing with each other, a coating process in which the surface of the ultra-fine particles is dispersed and coated with a coating agent, a foreign substance removing process for removing foreign substances contained in the slurry, and a concentrated liquid A method for producing a highly dispersible whey calcium composition comprising: a concentration process for producing a content of sucrose; and a powdering process for drying and pulverizing the liquid content after the concentration process
ここで、前記水和過程は、乳清カルシウム粒子：水の混合比を重量比で１：１〜５として行われ、前記コーティング過程は、超微粒子乳清カルシウム固形分１００重量％にカルボキシメチルセルロースやグァーガム、ガティガム、トラガントガム、キサンタンガム、プルラン、カシアガム、アラビノガラクタン、スクレロガム、カラギーナン、寒天、ローカストビーンガム、タラガム、アラビアガム、アルギン酸、アルギン酸ソーダ、タマリンドガムなどの増粘多糖類、デキストリンやシクロデキストリンなどの澱粉加水分解物類、カゼインやカゼインソーダなどの蛋白質類、グリセリン脂肪酸エステル類やポリグリセリン脂肪酸エステル類、ショ糖脂肪酸エステル類、ショ糖ステアリン酸エステル類、レシチン、プロピレングリコールアルギン酸エステル類などの親水（油）性乳化剤からなる群より選ばれた少なくとも１種以上を１〜４００重量部含有させることからなることが好ましい。 Here, the hydration process is performed by setting the mixing ratio of whey calcium particles: water as 1: 1 to 5 by weight, and the coating process is performed by adding carboxymethylcellulose and 100% by weight of ultrafine whey calcium solids. Guar gum, gati gum, tragacanth gum, xanthan gum, pullulan, cassia gum, arabinogalactan, sclerogum, carrageenan, agar, locust bean gum, tara gum, gum arabic, alginic acid, sodium alginate, tamarind gum, etc., dextrin, cyclodextrin, etc. Starch hydrolysates, proteins such as casein and casein soda, glycerin fatty acid esters, polyglycerin fatty acid esters, sucrose fatty acid esters, sucrose stearate esters, lecithin, propylene glycol alcohol It is preferable that the at least one kind selected from the group consisting of hydrophilic (oil) emulsifiers, such as phosphate esters since is contained 1-400 parts by weight.
また、前記粉末化過程は、熱風乾燥、真空乾燥、噴霧乾燥、ドラム乾燥及び凍結乾燥からなる群より選ばれた１種以上の方法で行われる。前記粉末化過程を経た乳清カルシウム組成物は、牛乳類や発酵乳類、乳クリーム類、バター類、チーズ類、粉乳類などの乳加工品、パン類や乾果類、キャンディ類、チョコレット類、ガム類、ジャム類などのお菓子類、アイスクリーム製品類、食肉・魚肉製品類、豆腐（蒟蒻）類、麺類、豆乳類などの飲料類、特殊栄養食品類、健康補助食品類、調味食品及びその他の食品類の全般にわたってカルシウム補充用として用いられ、歯磨き、化粧品及び医薬品からなる群より選ばれる少なくとも一つに添加剤として用いられることが好ましい。 The powdering process is performed by one or more methods selected from the group consisting of hot air drying, vacuum drying, spray drying, drum drying, and freeze drying. The whey calcium composition that has undergone the powdering process includes milk products, fermented milk, milk creams, butters, cheeses, milk products such as powdered milk, breads, dried fruits, candy, and chocolates. , Sweets such as gums and jams, ice cream products, meat and fish products, beverages such as tofu (noodles), noodles, soy milk, special nutrition foods, health supplements, seasoning foods In addition, it is used as a supplement for calcium throughout the food and other foods, and is preferably used as an additive in at least one selected from the group consisting of toothpaste, cosmetics and pharmaceuticals.
また、本願発明は、超微粒子乳清カルシウム（Ａ）固形分１００重量部に対してカルボキシメチルセルロースやグァーガム、ガティガム、トラガントガム、キサンタンガム、プルラン、カシアガム、アラビノガラクタン、スクレロガム、カラギーナン、寒天、ローカストビーンガム、タラガム、アラビアガム、アルギン酸、アルギン酸ソーダ、タマリンドガムなどの増粘多糖類、デキストリンやシクロデキストリンなどの澱粉加水分解物類全般、カゼインやカゼインソーダなどの蛋白質類、グリセリン脂肪酸エステル類、ポリグリセリン脂肪酸エステル類、ショ糖脂肪酸エステル類、ショ糖ステアリン酸エステル類、レシチン及びプロピレングリコールアルギン酸エステル類のような親水（油）性乳化剤（Ｂ）からなる群より選ばれた少なくとも１種以上を１〜４００重量部含有させてなる高分散性乳清カルシウム組成物を提供する。 Further, the present invention relates to carboxymethylcellulose, guar gum, gati gum, tragacanth gum, xanthan gum, pullulan, cassia gum, arabinogalactan, sclerogum, carrageenan, agar, locust bean gum with respect to 100 parts by weight of ultrafine whey calcium (A) solid content , Tara gum, gum arabic, alginic acid, sodium alginate, tamarind gum and other thickening polysaccharides, starch hydrolysates such as dextrin and cyclodextrin, proteins such as casein and casein soda, glycerin fatty acid esters, polyglycerin fatty acid Less selected from the group consisting of hydrophilic (oil) emulsifiers (B) such as esters, sucrose fatty acid esters, sucrose stearates, lecithin and propylene glycol alginates Also it provides one or more of 1 to 400 formed by incorporating parts highly disperse whey calcium composition.
これにより、加温しなくても冷水に直ちに溶け且つ沈澱が起こらず、製造された組成物を牛乳類や発酵乳類、乳クリーム類、バター類、チーズ類、粉乳類などの乳加工品、パン類や乾果類、キャンディ類、チョコレット類、ガム類、ジャム類などのお菓子類、アイスクリーム製品類、食肉・魚肉製品類、豆腐（蒟蒻）類、麺類、豆乳類などの飲料類、特殊栄養食品類、健康補助食品類、調味食品及びその他の食品類の全般にわたってカルシウム補充用として使用でき、歯磨きなどのような生活用品、化粧品及び医薬品の原料として使用できる、高分散性であって、添加量を高めて長期間放置しても分散安定性が高いという利点がある。 Thereby, even if it does not heat, it dissolves immediately in cold water and precipitation does not occur, and the manufactured composition is processed into milk products such as milks, fermented milks, milk creams, butters, cheeses, powdered milks, Breads and dried fruits, candy, chocolatelets, gums, jams and other sweets, ice cream products, meat and fish products, tofu (boiled), noodles, soy milk and other beverages, It can be used as a calcium supplement throughout all of special nutritional foods, health supplements, seasoning foods and other foods, and can be used as a raw material for daily necessities such as toothpaste, cosmetics and pharmaceuticals. There is an advantage that the dispersion stability is high even if the additive amount is increased and left for a long period of time.
本発明は、乳清カルシウムを超微粒子に粉砕した後、表面のコーティングを行うことにより、分酸性に優れるという効果がある。 The present invention has an effect of excellent acid separation by pulverizing whey calcium into ultrafine particles and then coating the surface.
また、冷水における再分散性と長期間の分散安定性を保つだけでなく、官能評価によって風味に極めて優れて、高濃度で添加することができるという効果もある。 In addition to maintaining redispersibility in cold water and long-term dispersion stability, there is also an effect that it can be added at a high concentration with an extremely excellent flavor by sensory evaluation.
また、ｐＨを問わず、中性及び酸性領域においても長期間の保存安定性が相当良好であり、一般食品用、健康補助食品、特殊栄養食品、医薬品、化粧品及び生活用品などの原料として使用可能であるという効果がある。 In addition, the long-term storage stability is considerably good in neutral and acidic regions regardless of pH, and it can be used as a raw material for general foods, health supplements, special nutrition foods, pharmaceuticals, cosmetics, and daily necessities. There is an effect that.
以下、添付図面に基づいて本発明の好適な実施例を詳細に説明する。 Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
図１は本発明に係る高分散性乳清カルシウム組成物の製造方法を示す図、図２は本発明に係る乳清カルシウムスラリーの電子顕微鏡（ＴＥＭ）写真を示す図、図３は従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の分散安定性の変化を示す図、図４は従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の貯蔵期間による分散安定性の変化を示す図、図５は従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の平均粒径及び分布を示す図、図６は従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の電子顕微鏡（ＴＥＭ）写真を示す図である。 FIG. 1 is a view showing a method for producing a highly dispersible whey calcium composition according to the present invention, FIG. 2 is an electron microscope (TEM) photograph of whey calcium slurry according to the present invention, and FIG. 3 is a conventional milk. FIG. 4 is a graph showing changes in dispersion stability of whey calcium and the whey calcium composition according to the present invention. FIG. 4 shows changes in dispersion stability depending on the storage period of conventional whey calcium and the whey calcium composition according to the present invention. FIG. 5 shows the average particle size and distribution of the conventional whey calcium and the whey calcium composition according to the present invention. FIG. 6 shows the conventional whey calcium and the whey calcium composition according to the present invention. It is a figure which shows an electron microscope (TEM) photograph.
図示したように、本発明に係る高分散性乳清カルシウム組成物の製造方法は、水和過程、粉砕過程、スラリー製造過程、コーティング過程、異物除去過程、濃縮過程及び粉末化過程からなる。 As shown, the method for producing a highly dispersible whey calcium composition according to the present invention comprises a hydration process, a pulverization process, a slurry production process, a coating process, a foreign substance removal process, a concentration process, and a powdering process.
まず、水和過程について説明する。 First, the hydration process will be described.
前記水和過程は、乳清カルシウムと水を混ぜて撹拌する過程であって、粒子サイズの分布１〜１００μｍであり且つ約２０μｍの平均粒径を有する乳清カルシウム粉末１．０ｋｇに、水又は精製水を１．０ｋｇ（固形分の濃度約５０．０％）〜５．０ｋｇ（固形分の濃度約１６．７％）程度加えて１０〜３，０００ｒｐｍで撹拌して乳清カルシウムを水和させる。 The hydration process is a process in which whey calcium and water are mixed and stirred, and 1.0 kg of whey calcium powder having a particle size distribution of 1 to 100 μm and an average particle diameter of about 20 μm is added to water or Add about 1.0kg of purified water (concentration of solid content about 50.0%) to 5.0kg (concentration of solid content of about 16.7%) and stir at 10-3,000rpm to hydrate whey calcium. Let
ここで、本発明に使用されるカルシウム剤としての乳清カルシウムは、カルシウム質が約２８％程度であり、カルシウムと燐が２：１の割合で含有されている市販の牛乳由来の一般的な乳清カルシウムを用いた。 Here, whey calcium as a calcium preparation used in the present invention is about 28% of calcium, and is generally derived from commercially available milk containing calcium and phosphorus in a ratio of 2: 1. Whey calcium was used.
次に、分散過程が行われる。前記で製造された乳清カルシウム水和液を物理的な方法による粉砕又は分散方法によってダイノーミル、ボールミル、サンドミル、コボルミル、ビードミルなどの湿式粉砕機、ナノマイザ、ホモゲナイザ、マイクロフリューダイザなどの乳化／分散装置、超音波分散機及びロールミルを用いて粉砕させる。 Next, a dispersion process is performed. Emulsification / dispersion of the whey calcium hydrate prepared above by a pulverization or dispersion method using a physical method, such as a wet pulverizer such as a dyno mill, ball mill, sand mill, cobol mill, or bead mill, nanomizer, homogenizer, or microfluidizer. It grind | pulverizes using an apparatus, an ultrasonic disperser, and a roll mill.
前記粉砕過程後には、乳清カルシウム粒子の粒度を調節するスラリー製造過程が行われるところ、前記の粉砕過程を澄ませた乳清カルシウム粒子の粒度分布及び平均粒径などは下記の方法で測定した。
１．粒度分析機による方法
測定機種：Ｍａｓｔｅｒｓｉｚｅｒ ２０００（Ｍａｌｖｅｒｎ，ＵＫ）
試料調製：粉砕された乳清カルシウムスラリー組成物を下記２０℃の溶媒中に滴下し、粒度分布測定試料として使用する。
溶媒：イオン交換水
予備分散：Ｈｙｄｒｏ ２０００ＭＵ（Ｍａｌｖｅｒｎ，ＵＫ）を用いて超音波分散１２０秒
測定温度：２０℃±１℃
２．透過電子顕微鏡（ＴＥＭ）による方法
測定機種：ＪＥＭ−１２３０（Ｊｅｏｌ，Ｊａｐｎａ）
加速電圧：８０ｋＶ
倍率：×５０，０００
After the pulverization process, a slurry manufacturing process for adjusting the particle size of the whey calcium particles is performed. The particle size distribution and average particle size of the whey calcium particles clarified by the pulverization process were measured by the following methods.
1. Method measurement model by particle size analyzer: Mastersizer 2000 (Malvern, UK)
Sample preparation: The pulverized whey calcium slurry composition is dropped into the following solvent at 20 ° C. and used as a particle size distribution measurement sample.
Solvent: Ion-exchange water Predispersion: Ultrasonic dispersion for 120 seconds using Hydro 2000MU (Malvern, UK) Measurement temperature: 20 ° C. ± 1 ° C.
2. Method measurement model by transmission electron microscope (TEM): JEM-1230 (Jeol, Japan)
Acceleration voltage: 80 kV
Magnification: x50,000
すなわち、前記において物理的な方法によって乳清カルシウムを超微粒子に粉砕して適正の粒子に到達したときに粉砕を終了する方式でスラリー製造過程を経て、粒径０．０００１〜５．０μｍの乳清カルシウムスラリーを製造する。 That is, in the above, whey calcium is pulverized into ultrafine particles by a physical method and the pulverization is completed when the appropriate particles are reached. A fresh calcium slurry is produced.
次にコーティング過程が行われる。前記で製造されたスラリー中の乳清カルシウムの固形分濃度が１５重量％程度の乳清カルシウム（Ａ）固形分１００重量部に対してカルボキシメチルセルロースやグァーガム、ガティガム、トラガントガム、キサンタンガム、プルラン、カシアガム、アラビノガラクタン、スクレロガム、カラギーナン、寒天、ローカストビーンガム、タラガム、アラビアガム、アルギン酸、アルギン酸ソーダ、タマリンドガムなどの増粘多糖類、デキストリンやシクロデキストリンなどの澱粉加水分解物類全般、カゼインやカゼインソーダなどの蛋白質類、グリセリン脂肪酸エステル類、ポリグリセリン脂肪酸エステル類、ショ糖脂肪酸エステル類、ショ糖ステアリン酸エステル類、レシチン及びプロピレングリコールアルギン酸エステル類などの親水（油）性乳化剤（Ｂ）を１〜４００重量部含有させ、乳清カルシウムが互いに縮合しないように超微粒子乳清カルシウムの表面にコーティング剤でコーティングさせる。 Next, a coating process is performed. Carboxymethylcellulose, guar gum, gati gum, tragacanth gum, xanthan gum, pullulan, cassia gum, whey calcium (A) solid content concentration of about 15% by weight in the slurry produced above with respect to 100 parts by weight of whey calcium (A) solid content Thickening polysaccharides such as arabinogalactan, sclerogum, carrageenan, agar, locust bean gum, tara gum, gum arabic, alginic acid, sodium alginate, tamarind gum, starch hydrolysates such as dextrin and cyclodextrin, casein and casein soda Proteins such as glycerin fatty acid esters, polyglycerin fatty acid esters, sucrose fatty acid esters, sucrose stearate esters, lecithin and propylene glycol alginate esters (oil) Sex emulsifier (B) to be contained 1 to 400 parts by weight, is coated with a coating agent to the surface of the ultrafine whey calcium as whey calcium are not fused to each other.
前記コーティング過程は、乳清カルシウムの粒子が粒子相互間の静電気的力などによって縮合又は結合して粒度が大きくなることを防止し、沈澱せずに、高分散性の分散安定性を保つためである。 The coating process is to prevent whey calcium particles from condensing or binding due to electrostatic force between the particles and increasing the particle size, and to maintain high dispersion stability without precipitation. is there.
前記乳清カルシウムスラリーにアラビアガムのような増粘安定剤、澱粉加水分解物類と親水（油）性乳化剤を投入して乳清カルシウムの超微粒子の表面にコーティングする方法では、撹拌、溶解、加熱、ホモミックス、高圧均質などの方法を１種以上並行して完全に溶解し、粒子を分離してコーティングすることが好ましい。 In the method of coating the surface of ultrafine particles of whey calcium by adding a thickening stabilizer such as gum arabic, starch hydrolyzate and hydrophilic (oil) emulsifier to the whey calcium slurry, stirring, dissolving, Preferably, one or more methods such as heating, homomixing, and high-pressure homogenization are completely dissolved in parallel, and the particles are separated and coated.
前記の撹拌はコーティング剤が完全に溶解して表面のコーティングが完了するまで長時間行われる。ホモミキサは３，０００ｒｐｍで１０分以上循環しながら物理的な衝撃を強く与えてコーティングし、高圧均質は一般に２００ｂａｒ程度の圧力で１回以上通過させて行い、これを１種以上並行することが一層効率的である。撹拌、溶解、加熱、ホモミキサ及び高圧均質化過程中の全ての過程を経ず、１つ又は２つの過程を経てもコーディングされる。 The stirring is performed for a long time until the coating agent is completely dissolved and the surface coating is completed. The homomixer is coated with a strong physical impact while circulating at 3,000 rpm for 10 minutes or more, and high-pressure homogenization is generally performed at least once at a pressure of about 200 bar. Efficient. It is coded through one or two steps without going through all the steps of stirring, dissolving, heating, homomixer and high pressure homogenization.
コーティングが完了すると、コーティングされた乳清カルシウム水懸濁液のｐＨを調節するが、クエン酸、リンゴ酸、乳酸、燐酸及び塩酸などの苛性ソーダ、水酸化カルシウム及び水酸化カリウムなどのｐＨ調節剤を用いて、コーティングされた乳清カルシウム水懸濁液のｐＨを１０．０以下に調節する。 When coating is complete, the pH of the coated whey calcium water suspension is adjusted, but pH adjusting agents such as caustic soda such as citric acid, malic acid, lactic acid, phosphoric acid and hydrochloric acid, calcium hydroxide and potassium hydroxide are added. Use to adjust the pH of the coated whey calcium water suspension to 10.0 or lower.
次に、異物除去過程が行われる。前記でコーティングされた乳清カルシウム水懸濁液の中に含まれている異物と、コーティングされないか乳清カルシウムの平均粒径が大きいものを除去するために、３４０メッシュの篩を通過させ、１〜２０μｍの空隙を有する濾過フィルタで濾過し、或いは５，０００ｒｐｍで６，０００Ｌ／時間の流速で連続式及びバッチ式遠心分離機で遠心分離して異物を完全に除去し、これを１種以上並行することが好ましい。 Next, a foreign matter removal process is performed. In order to remove the foreign substances contained in the aqueous whey calcium suspension coated as described above and those that are not coated or have a large average particle size of whey calcium, the mixture is passed through a 340 mesh sieve, Filter through a filter with a gap of ~ 20 μm, or centrifuge in a continuous and batch centrifuge at a flow rate of 6,000 L / hour at 5,000 rpm to completely remove foreign matters, one or more of these It is preferable to run in parallel.
前記異物の除去された乳清カルシウム水懸濁液に対して濃縮過程が行われるところ、乳清カルシウム水懸濁液を真空濃縮機で乳清カルシウム固形分が１〜６０重量％となるように濃縮し、連続式瞬間殺菌機（ＵＨＴ）で殺菌して液状の製品に包装し、或いは乾燥粉末化過程の原料として用いる。 When the concentration process is performed on the whey calcium water suspension from which the foreign matter has been removed, the whey calcium water suspension is adjusted to 1 to 60% by weight with a vacuum concentrator. It is concentrated, sterilized by a continuous instantaneous sterilizer (UHT), packaged in a liquid product, or used as a raw material for the dry powdering process.
前記濃縮過程が完了すると、粉末化過程が行われる。粉末化過程は熱風乾燥、真空乾燥、噴霧乾燥、ドラム乾燥及び凍結乾燥などの１種以上の方法で濃縮された乳清カルシウム水懸濁液を乾燥させた後粉末化するか、或いは濃縮過程が不要な場合には直ちに乾燥粉末化過程に進むことが好ましい。 When the concentration process is completed, a powdering process is performed. The pulverization process may be performed by drying the whey calcium water suspension concentrated by one or more methods such as hot air drying, vacuum drying, spray drying, drum drying and freeze-drying and then pulverizing, or the concentration process may be If unnecessary, it is preferable to immediately proceed to a dry powdering process.
前記の過程が完了すると、高分散性乳清カルシウム組成物の製造が完了する。 When the above process is completed, the production of the highly dispersible whey calcium composition is completed.
以下、前記の製造過程を具体的な実施例で例示して本発明をより詳細に説明する。本発明はこれらの実施例に限定されない。 Hereinafter, the present invention will be described in more detail by exemplifying the above manufacturing process with specific examples. The present invention is not limited to these examples.
まず、２つの方法を用いてそれぞれの実施例に使用される乳清カルシウムスラリー（Ａ）の製造方法を下記に例示する。
乳清カルシウムスラリー（１）：
粒子サイズの分布が１〜１００μｍであり且つ約２０μｍ程度の平均粒径を有する乳清カルシウム粉末１．０ｋｇに、水又は精製水を５．０ｋｇ（固形分の濃度約１６．７％）程度添加し、３，０００ｒｐｍで３０分間撹拌して乳清カルシウムを水和する。乳清カルシウム水和液を湿式粉砕機（Ａｇｉｔａｔｏｒ Ｂｅａｄ Ｍｉｌｌ ＬＭＫ ２０）パイロット型（Ｎｅｔｚｓｃｈ社製）で湿式粉砕し、乳清カルシウムスラリー５．９５ｋｇを得た。そのスラリー中の乳清カルシウムの平均粒径は０．１３μｍであった。
乳清カルシウムスラリー（２）：
粒子サイズの分布が１〜１００μｍであり且つ約２０μｍ程度の平均粒径を有する乳清カルシウム粉末１．０ｋｇに、水又は精製水を４．０ｋｇ（固形分の濃度約２０．０％）程度添加し、１，０００ｒｐｍで３０分間撹拌して乳清カルシウムを水和する。乳清カルシウム水和液を湿式粉砕機（Ａｇｉｔａｔｏｒ Ｂｅａｄ Ｍｉｌｌ ＬＭＫ ２０）パイロット型（Ｎｅｔｚｓｃｈ社製）で湿式粉砕し、乳清カルシウムスラリー４．９７ｋｇを得た。そのスラリー中の乳清カルシウムの平均粒径は０．１５μｍであった。
First, the manufacturing method of the whey calcium slurry (A) used for each Example using two methods is illustrated below.
Whey calcium slurry (1):
About 1.0 kg of water or purified water (solids concentration of about 16.7%) is added to 1.0 kg of whey calcium powder having a particle size distribution of 1 to 100 μm and an average particle size of about 20 μm. Then, whey calcium is hydrated by stirring at 3,000 rpm for 30 minutes. The whey calcium hydrate was wet pulverized with a wet pulverizer (Agitator Bead Mill LMK 20) pilot type (manufactured by Netzsch) to obtain 5.95 kg of whey calcium slurry. The average particle size of whey calcium in the slurry was 0.13 μm.
Whey calcium slurry (2):
About 4.0 kg of water or purified water (solid content concentration of about 20.0%) is added to 1.0 kg of whey calcium powder having a particle size distribution of 1 to 100 μm and an average particle size of about 20 μm. Then, whey calcium is hydrated by stirring at 1,000 rpm for 30 minutes. The whey calcium hydrate was wet pulverized with a wet pulverizer (Agitator Bead Mill LMK 20) pilot type (manufactured by Netzsch) to obtain 4.97 kg of whey calcium slurry. The average particle diameter of whey calcium in the slurry was 0.15 μm.
前記で製造された乳清カルシウムスラリー（１）及び乳清カルシウムスラリー（２）に含まれた超微粒子乳清カルシウムの粒子形態を電子顕微鏡で観察した結果を図２に示した。 The result of having observed the particle | grain form of the ultrafine whey calcium contained in the whey calcium slurry (1) manufactured above by the whey calcium slurry (2) with the electron microscope was shown in FIG.
次に、前記乳清カルシウムスラリー（１）又は（２）を用いた高分散性乳清カルシウム組成物の具体的な製造方法を詳細に説明する。 Next, the specific manufacturing method of the highly dispersible whey calcium composition using the said whey calcium slurry (1) or (2) is demonstrated in detail.
前記で製造された乳清カルシウムスラリー（１）１．０Ｌにアラビアガム１６７ｇを徐々に投入し、３，０００ｒｐｍで約３０分間ホモミックスして完全に分散させた後、３４０メッシュの篩に透過させ、２０μｍと１μｍの空隙を有する濾過フィルタで順次濾過して異物を除去する。液のｐＨを８．５に調節し、１５０〜２００ｂａｒ程度の圧力で１回高圧均質した後、５，０００ｒｐｍで１０分間遠心分離して異物を完全に除去し、必要に応じて真空濃縮機で乳清カルシウム固形分が１〜６０重量％となるように濃縮し、連続式瞬間殺菌機（ＵＨＴ）で殺菌した後、液状の乳清カルシウム製剤６３０ｇとこれを噴霧乾燥機で噴霧乾燥させて粉末状の高分散性天然乳清カルシウム製剤とその組成物３００ｇを得た。 167 g of gum arabic is gradually added to 1.0 L of the whey calcium slurry (1) produced above, and after thorough mixing at 3,000 rpm for about 30 minutes, the mixture is completely dispersed and allowed to pass through a 340 mesh sieve. The foreign matter is removed by sequentially filtering through a filter having a gap of 20 μm and 1 μm. The pH of the solution is adjusted to 8.5 and homogenized once at a pressure of about 150 to 200 bar, and then centrifuged at 5,000 rpm for 10 minutes to completely remove foreign matter. If necessary, use a vacuum concentrator. After concentrating to 1-60 wt% whey calcium solids and sterilizing with a continuous instantaneous sterilizer (UHT), 630 g of liquid whey calcium preparation and spray-dried with a spray dryer to obtain powder 300 g of a highly dispersible natural whey calcium preparation and its composition were obtained.
前記で製造された乳清カルシウムスラリー（２）１．０Ｌにアラビアガム２００ｇを徐々に投入したことを除いては、実施例１と同様の方法で製造して液状のカルシウム製剤７００ｇと粉末状の高分散性天然乳清カルシウム製剤とその組成物３７５ｇを得た。 Except that 200 g of gum arabic was gradually added to 1.0 L of the whey calcium slurry (2) produced above, 700 g of a liquid calcium preparation and a powdery powder were produced in the same manner as in Example 1. A highly dispersible natural whey calcium preparation and its composition 375 g were obtained.
前記で製造された乳清カルシウムスラリー（１）１．０Ｌにアラビアガム１００ｇ及びシクロデキストリン６７ｇを徐々に投入したことを除いては、実施例１と同様の方法で製造して液状のカルシウム製剤６３５ｇと粉末状の高分散性天然乳清カルシウム製剤とその組成物３０２ｇを得た。 Except that 100 g of gum arabic and 67 g of cyclodextrin were gradually added to 1.0 L of the whey calcium slurry (1) produced above, 635 g of a liquid calcium preparation produced in the same manner as in Example 1. And 302 g of a powdery highly dispersible natural whey calcium preparation and its composition were obtained.
前記で製造された乳清カルシウムスラリー（２）１．０Ｌにアラビアガム１４５ｇ及びシクロデキストリン５５ｇを徐々に投入したことを除いては、実施例１と同様の方法で製造して液状のカルシウム製剤６４０ｇと粉末状の高分散性天然乳清カルシウム製剤とその組成物３０３ｇを得た。 640 g of a liquid calcium preparation manufactured in the same manner as in Example 1 except that 145 g of gum arabic and 55 g of cyclodextrin were gradually added to 1.0 L of the whey calcium slurry (2) prepared above. And a powdery highly dispersible natural whey calcium preparation and its composition 303 g were obtained.
前記で製造された乳清カルシウムスラリー（１）１．０Ｌにアラビアガム１００ｇ及びポリグリセリン脂肪酸エステル６７ｇを徐々に投入したことを除いては、実施例１と同様の方法で製造して液状のカルシウム製剤６２０ｇと粉末状の高分散性天然乳清カルシウム製剤とその組成物２８９ｇを得た。 Liquid calcium produced in the same manner as in Example 1 except that 100 g of gum arabic and 67 g of polyglycerol fatty acid ester were gradually added to 1.0 L of the whey calcium slurry (1) produced above. 620 g of the preparation, 289 g of a powdery highly dispersible natural whey calcium preparation and its composition were obtained.
前記で製造された乳清カルシウムスラリー（２）１．０Ｌにアラビアガム１４５ｇ及びポリグリセリン脂肪酸エステル５５ｇを徐々に投入したことを除いては、実施例１と同様の方法で製造して液状のカルシウム製剤６３５ｇと粉末状の高分散性天然乳清カルシウム製剤とその組成物２９２ｇを得た。 Liquid calcium produced in the same manner as in Example 1 except that 145 g of gum arabic and 55 g of polyglycerol fatty acid ester were gradually added to 1.0 L of the whey calcium slurry (2) produced above. 635 g of the preparation, 292 g of a powdery highly dispersible natural whey calcium preparation and its composition were obtained.
前記実施例１〜６で製造された高分散性天然乳清カルシウム組成物の理化学的特性比較結果は表１に示した。 The physicochemical property comparison results of the highly dispersible natural whey calcium compositions prepared in Examples 1 to 6 are shown in Table 1.
表１に示すように、性状は微細な白色粉末であり、平均粒径は約０．１９５μｍである。 As shown in Table 1, the property is a fine white powder, and the average particle size is about 0.195 μm.
図３は、従来の乳清カルシウムと本発明に係る高分散性乳清カルシウム組成物の分散安定性の変化を示す図であって、実施例１で調製した乳清カルシウム粉末組成物を用いて各カルシウム剤の固形分濃度が１．０重量％となるように希釈した後、その希釈液を５℃に２４時間静置したとき、沈澱によって生ずる透明部分と分散部分との界面高さの変化写真である。 FIG. 3 is a diagram showing a change in dispersion stability of conventional whey calcium and the highly dispersible whey calcium composition according to the present invention, using the whey calcium powder composition prepared in Example 1. After diluting each calcium preparation to a solid content concentration of 1.0% by weight, when the diluted solution is allowed to stand at 5 ° C. for 24 hours, the change in the interfacial height between the transparent portion and the dispersed portion caused by precipitation It is a photograph.
図３に示すように、本発明に係る乳清カルシウム組成物は、沈澱が起こらず、分散性に優れることが分る。 As shown in FIG. 3, it can be seen that the whey calcium composition according to the present invention does not cause precipitation and is excellent in dispersibility.
図４は、従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の貯蔵期間による分散安定性の変化を示す図であって、実施例１で調製した乳清カルシウム粉末組成物を用いて各カルシウム剤の固形分濃度が１．０重量％となるように希釈した後、その希釈液を５℃に２１日間静置した後、沈澱によって生じる透明部分と分散部分との界面高さの変化写真である。ここで、表示された数字は貯蔵日数を示す。 FIG. 4 is a diagram showing a change in dispersion stability depending on the storage period of conventional whey calcium and the whey calcium composition according to the present invention, using the whey calcium powder composition prepared in Example 1. After diluting so that the solid content concentration of each calcium preparation is 1.0% by weight, the diluted solution is allowed to stand at 5 ° C. for 21 days, and then the change in the interfacial height between the transparent portion and the dispersed portion caused by precipitation It is a photograph. Here, the displayed number indicates the number of storage days.
図４に示すように、本発明に係る乳清カルシウム組成物は、貯蔵期間が経過しても、沈澱が起こらず、分散性に優れることがわかる。 As shown in FIG. 4, it can be seen that the whey calcium composition according to the present invention is excellent in dispersibility without precipitation even after the storage period has elapsed.
図５は、従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の平均粒径及び分布を示す図であって、実施例１で調製した高分散性天然乳清カルシウム製剤粉末組成物の平均粒径及び分布度をＡｕｔｏ‐ｓａｍｐｌｅ ｕｎｉｔ（Ｈｙｄｒｏ ２０００ＭＵ，Ｍａｌｖｅｒｎ，ＵＫ）付きレーザ粒度分析機（Ｍａｓｔｅｒｓｉｚｅｒ ２０００，Ｍａｌｖｅｒｎ，ＵＫ）で分析した。 FIG. 5 is a diagram showing the average particle size and distribution of conventional whey calcium and the whey calcium composition according to the present invention, and shows the high dispersibility natural whey calcium preparation powder composition prepared in Example 1. The average particle size and distribution were analyzed with a laser particle size analyzer (Mastersizer 2000, Malvern, UK) with an Auto-sample unit (Hydro 2000MU, Malvern, UK).
図５に示した分析結果は次の通りである。
１．従来の乳清カルシウム
ｄ（０．１）：４．３２５μｍ
ｄ（０．５）：１９．２０５μｍ
ｄ（０．９）：４２．２７４μｍ
Ｖｏｌ．Ｗｅｉｇｈｔｅｄ Ｍｅａｎ ｄ［４，３］：２１．６６９μｍ
２．高分散性乳清カルシウム組成物
ｄ（０．１）：０．０６６μｍ
ｄ（０．５）：０．１３０μｍ
ｄ（０．９）：０．２５３μｍ
Ｖｏｌ．Ｗｅｉｇｈｔｅｄ Ｍｅａｎ Ｄ［４，３］：０．１５０μｍ
The analysis results shown in FIG. 5 are as follows.
1. Conventional whey calcium d (0.1): 4.325 μm
d (0.5): 19.205 μm
d (0.9): 42.274 μm
Vol. Weighted Mean d [4,3]: 21.669 μm
2. Highly dispersible whey calcium composition d (0.1): 0.066 μm
d (0.5): 0.130 μm
d (0.9): 0.253 μm
Vol. Weighted Mean D [4,3]: 0.150 μm
図６は従来の乳清カルシウムと本発明に係る乳清カルシウム組成物の電子顕微鏡（ＴＥＭ）写真を示す図であって、本願発明の乳清カルシウム組成物の粒度が従来の乳清カルシウムに比べて小さいことがわかる。 FIG. 6 is a view showing an electron microscope (TEM) photograph of the conventional whey calcium and the whey calcium composition according to the present invention, wherein the particle size of the whey calcium composition of the present invention is larger than that of the conventional whey calcium. It is small.
次に、実施例１〜６で調製した高分散性乳清カルシウム粉末組成物を用いて各カルシウム剤の固形分濃度が１．０重量％となるように希釈した後、その希釈液を１００ｍｌのメスシリンダに取って１０℃に静置し、乳清カルシウムの沈澱によって生じる透明部分とカルシウム剤分散部分の着色部分との界面高さの経時変化、沈澱物量の経時変化を肉眼で観察して判断し、各分散液の長期貯蔵時の分散安定性を調査した。メスシリンダに刻まれたｍｌ単位の表示を読み取ってその結果を下記５段階の表示基準によって表２に示した。
（界面の高さ）
界面が略９８以上１００ｍｌである．．．．．．．．．．．．５
界面が９０以上９８未満．．．．．．．．．．．．．．．．．４
界面が９０以上９５未満．．．．．．．．．．．．．．．．．３
界面が５０以上９０未満．．．．．．．．．．．．．．．．．２
界面が５０未満．．．．．．．．．．．．．．．．．．．．．１
（沈澱物量）
殆ど沈澱が確認されない．．．．．．．．．．．．．．．．．５
やや沈澱が確認される．．．．．．．．．．．．．．．．．．４
０．５ｍｍ未満程度の沈澱がある ．．．．．．．．．．．．．３
０．５ｍｍ以上２．０ｍｍ未満の沈澱がある．．．．．．．．．２
２．０ｍｍ以上の沈澱がある ．．．．．．．．．．．．．．．１
Next, after diluting using the highly dispersible whey calcium powder composition prepared in Examples 1 to 6 so that the solid content concentration of each calcium preparation is 1.0% by weight, Take it in a measuring cylinder and let it stand at 10 ° C. Judgment is made by observing the changes over time in the interfacial height between the transparent part and the colored part of the calcium agent-dispersed part caused by the precipitation of whey calcium and the change in the amount of the precipitate over time The dispersion stability of each dispersion during long-term storage was investigated. Table 2 shows the results of reading the unit of ml inscribed on the graduated cylinder, and the results are shown in Table 2 according to the following five display standards.
(Interface height)
The interface is approximately 98 to 100 ml. . . . . . . . . . . . 5
The interface is 90 or more and less than 98. . . . . . . . . . . . . . . . . 4
The interface is 90 or more and less than 95. . . . . . . . . . . . . . . . . 3
The interface is 50 or more and less than 90. . . . . . . . . . . . . . . . . 2
The interface is less than 50. . . . . . . . . . . . . . . . . . . . . 1
(Precipitate amount)
Almost no precipitation is confirmed. . . . . . . . . . . . . . . . . 5
Slight precipitation is confirmed. . . . . . . . . . . . . . . . . . 4
There is a precipitation of less than 0.5mm. . . . . . . . . . . . . 3
There is precipitation of 0.5 mm or more and less than 2.0 mm. . . . . . . . . 2
There is a precipitation of 2.0 mm or more. . . . . . . . . . . . . . . 1
表２に示すように、本願発明の乳清カルシウム組成物は、時間が経過しても沈殿が起こらないことが分る。 As shown in Table 2, it can be seen that the whey calcium composition of the present invention does not precipitate over time.
次に、実施例１〜６で調製した高分散性乳清カルシウム粉末組成物１０．０ｇを牛乳１，０００ｍｌに添加して溶解した後、殺菌してカルシウム強化牛乳を得た。そのカルシウム強化牛乳を１００ｍｌの数個のマスシリンダに取って５℃に保存しながら、定期的にマスシリンダ中の牛乳を静かに廃棄し、マスシリンダの底部に残存している沈澱物量の経時変化を肉眼で観察した。その結果を下記４段階表示基準で表３に示した。また、そのカルシウム強化牛乳に対して男女各１０名に官能試験を施した後、その食感に関してそれぞれ５段階判定を行い、その平均値を表３に示した。
（沈澱物量）
略沈澱が確認されない．．．．．．．．．．．．．．．．．４
やや沈澱が観察される．．．．．．．．．．．．．．．．．３
多少沈澱が観察される．．．．．．．．．．．．．．．．．２
相当な沈澱が観察される．．．．．．．．．．．．．．．．１
（風味）
風味が良好である．．．．．．．．．．．．．．．．．．．５
風味がやや異常である．．．．．．．．．．．．．．．．．４
風味が多少悪い（若干の不快さ）．．．．．．．．．．．．３
風味が相当悪い（相当な不快さ）．．．．．．．．．．．．．２
風味が非常に悪い．．．．．．．．．．．．．．．．．．．１
Next, 10.0 g of the highly dispersible whey calcium powder composition prepared in Examples 1 to 6 was added and dissolved in 1,000 ml of milk, and then sterilized to obtain calcium-enriched milk. While taking the calcium-enriched milk in several 100 ml mass cylinders and storing them at 5 ° C, periodically discarding the milk in the mass cylinders periodically and changing the amount of precipitate remaining at the bottom of the mass cylinder Was observed with the naked eye. The results are shown in Table 3 on the basis of the following four-step display standard. In addition, after subjecting the calcium-enriched milk to 10 men and women, a sensory test was performed, and the texture was evaluated in 5 stages, and the average values are shown in Table 3.
(Precipitate amount)
Almost no precipitation is confirmed. . . . . . . . . . . . . . . . . 4
Slight precipitation is observed. . . . . . . . . . . . . . . . . 3
Some precipitation is observed. . . . . . . . . . . . . . . . . 2
Considerable precipitation is observed. . . . . . . . . . . . . . . . 1
(Flavor)
The flavor is good. . . . . . . . . . . . . . . . . . . 5
The flavor is slightly abnormal. . . . . . . . . . . . . . . . . 4
Flavor is slightly bad (slight discomfort). . . . . . . . . . . . 3
Flavor is quite bad (substantial discomfort). . . . . . . . . . . . . 2
The flavor is very bad. . . . . . . . . . . . . . . . . . . 1
表３に示すように、カルシウム強化牛乳に添加される場合にも、時間が経っても略沈澱が起こらず、風味も時間が経っても良好であった。 As shown in Table 3, even when added to calcium-enriched milk, almost no precipitation occurred over time, and the flavor and time were good.
次に、実施例１〜６で調製した高分散性乳清カルシウム粉末組成物１０．０ｇを牛乳１，０００ｍｌに添加して溶解した後、超高温瞬間殺菌（ＵＨＴ）を行ってカルシウム強化用牛乳を得た。その牛乳を１００ｍｌの数個のメスシリンダに取って５℃に保存しながら定期的にメスシリンダ中の牛乳を静かに廃棄し、メスシリンダの底部に残存している沈澱物量の経時変化を肉眼で観察した。その結果を下記４段階の表示基準で表４に示した。また、そのカルシウム強化牛乳に対して男女各１０名に官能試験を施した後、食感に関してそれぞれ４段階の判定を行い、その平均値を表４に示した。
（沈澱物量）
略沈澱が確認されない．．．．．．．．．．．．．．．．．４
やや沈澱が観察される．．．．．．．．．．．．．．．．．３
多少沈澱が観察される．．．．．．．．．．．．．．．．．２
相当な沈澱が観察される．．．．．．．．．．．．．．．．１
（食感）
食感が非常に良好である．．．．．．．．．．．．．．．．４
粘度が多少高く、少しちくちくする．．．．．．．．．．．３
粘度が相当高く、非常にちくちくする．．．．．．．．．．２
食感が相当悪い（非常にちくちくする）．．．．．．．．．１
Next, 10.0 g of the highly dispersible whey calcium powder composition prepared in Examples 1 to 6 was added and dissolved in 1,000 ml of milk, and then ultrahigh temperature instant sterilization (UHT) was performed to milk for calcium enrichment. Got. While taking the milk into several 100 ml measuring cylinders and storing them at 5 ° C, periodically discard the milk in the measuring cylinders periodically, and visually observe the amount of sediment remaining on the bottom of the measuring cylinder. Observed. The results are shown in Table 4 with the following four display criteria. In addition, after a sensory test was performed on the calcium-enriched milk for 10 men and women, a four-stage determination was made on the texture, and the average values are shown in Table 4.
(Precipitate amount)
Almost no precipitation is confirmed. . . . . . . . . . . . . . . . . 4
Slight precipitation is observed. . . . . . . . . . . . . . . . . 3
Some precipitation is observed. . . . . . . . . . . . . . . . . 2
Considerable precipitation is observed. . . . . . . . . . . . . . . . 1
(Texture)
The texture is very good. . . . . . . . . . . . . . . . 4
Viscosity is slightly high and a little tingled. . . . . . . . . . . 3
Viscosity is quite high and very tingling. . . . . . . . . . 2
The texture is quite bad (very tingling). . . . . . . . . 1
表４に示すように、乳清カルシウム粉末組成物を超高温瞬間殺菌してカルシウム強化牛乳として使用する場合、相当な時間が経過しても沈澱が殆どなく、また相当な時間が経過しても食感の優秀性が保たれる。 As shown in Table 4, when the whey calcium powder composition is instantly sterilized by ultra-high temperature and used as calcium-enriched milk, there is almost no precipitation even after a considerable time has passed, and even if a considerable time has passed. Excellent texture is maintained.
Claims (6)
前記水和過程で形成された水和物に含まれた乳清カルシウム粒子を粉砕機で粉砕させる粉砕過程と、
乳清カルシウムが粒径０．０００１〜５．０μｍの超微粒子となるように粒度を調節するスラリー製造過程と、
スラリー中の超微粒子乳清カルシウム粒子が互いに縮合しないように超微粒子の表面に分散及びコーティング剤でコーティングさせるコーティング過程と、
スラリー中に含有されている異物を除去する異物除去過程と、
濃縮して液状の含有物を製造する濃縮過程と、
濃縮過程を経た液状の含有物を乾燥させて粉末化する粉末化過程とを含んでなることを特徴とする高分散性乳清カルシウム組成物の製造方法。 A hydration process in which water is added to natural whey calcium powder and then mixed with stirring to form a hydrate;
A pulverization process in which whey calcium particles contained in the hydrate formed in the hydration process are pulverized by a pulverizer;
A slurry production process for adjusting the particle size so that whey calcium becomes ultrafine particles having a particle size of 0.0001 to 5.0 μm;
A coating process in which the surface of the ultrafine particles is dispersed and coated with a coating agent so that the ultrafine whey calcium particles in the slurry do not condense with each other,
Foreign matter removal process for removing foreign matter contained in the slurry,
A concentration process for producing liquid contents by concentration;
A method for producing a highly dispersible whey calcium composition, comprising: a pulverization step of drying and pulverizing a liquid content after the concentration step.
超微粒子乳清カルシウム固形分１００重量％にカルボキシメチルセルロースやグァーガム、ガティガム、トラガントガム、キサンタンガム、プルラン、カシアガム、アラビノガラクタン、スクレロガム、カラギーナン、寒天、ローカストビーンガム、タラガム、アラビアガム、アルギン酸、アルギン酸ソーダ、タマリンドガムなどの増粘多糖類、デキストリンやシクロデキストリンなどの澱粉加水分解物類、カゼインやカゼインソーダなどの蛋白質類、グリセリン脂肪酸エステル類、ポリグリセリン脂肪酸エステル類、ショ糖脂肪酸エステル類、ショ糖ステアリン酸エステル類、レシチン及びプロピレングリコールアルギン酸エステル類のような親水（油）性乳化剤からなる群より選ばれた少なくとも１種以上を１〜４００重量部含有させることからなることを特徴とする請求項１又は２記載の高分散性乳清カルシウム組成物の製造方法。 The coating process includes
Carboxymethylcellulose, guar gum, gati gum, tragacanth gum, xanthan gum, pullulan, cassia gum, arabinogalactan, sclerogum, carrageenan, agar, locust bean gum, tara gum, gum arabic, alginic acid, sodium alginate, Thickening polysaccharides such as tamarind gum, starch hydrolysates such as dextrin and cyclodextrin, proteins such as casein and casein soda, glycerin fatty acid esters, polyglycerin fatty acid esters, sucrose fatty acid esters, sucrose stearin 1 to 400 parts by weight of at least one selected from the group consisting of hydrophilic (oil) emulsifiers such as acid esters, lecithin and propylene glycol alginates The method according to claim 1 or 2 highly dispersible whey calcium composition, wherein the comprising a.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009526748A (en) * | 2006-02-17 | 2009-07-23 | ベリトロン・リミテッド | Calcium absorption promoter |
| JP2010187595A (en) * | 2009-02-18 | 2010-09-02 | Morinaga Milk Ind Co Ltd | Method for producing calcium-containing milk composition |
| JP2011055811A (en) * | 2009-09-14 | 2011-03-24 | Ogawa & Co Ltd | Method for producing plant extract powder |
| FR3046525A1 (en) * | 2016-01-11 | 2017-07-14 | Cie Laitiere Europeenne | DAIRY CALCIUM IN DISPERSIBLE POWDER, PROCESS FOR PREPARING SAME AND USE THEREOF FOR ENHANCING CALCIUM FOOD |
| WO2018016120A1 (en) * | 2016-07-22 | 2018-01-25 | 一般社団法人 Ｕｎｉｃａｌ | Food product containing calcium salt granules and dietary fiber |
| JP2018078870A (en) * | 2016-11-18 | 2018-05-24 | 一般社団法人 Ｕｎｉｃａｌ | Food product containing the granule of calcium salt and dietary fiber |
| WO2023209603A1 (en) * | 2022-04-29 | 2023-11-02 | Fonterra Co-Operative Group Limited | Dairy product and process |
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| KR101689287B1 (en) * | 2014-10-28 | 2016-12-23 | 조향현 | Preparation method for milk protein with high content of organic mineral using nucleotide as an catalyst |
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2003
- 2003-09-01 KR KR1020030060910A patent/KR20030078050A/en not_active Application Discontinuation
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2004
- 2004-03-01 JP JP2004055659A patent/JP2005073695A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009526748A (en) * | 2006-02-17 | 2009-07-23 | ベリトロン・リミテッド | Calcium absorption promoter |
| JP2010187595A (en) * | 2009-02-18 | 2010-09-02 | Morinaga Milk Ind Co Ltd | Method for producing calcium-containing milk composition |
| JP2011055811A (en) * | 2009-09-14 | 2011-03-24 | Ogawa & Co Ltd | Method for producing plant extract powder |
| FR3046525A1 (en) * | 2016-01-11 | 2017-07-14 | Cie Laitiere Europeenne | DAIRY CALCIUM IN DISPERSIBLE POWDER, PROCESS FOR PREPARING SAME AND USE THEREOF FOR ENHANCING CALCIUM FOOD |
| WO2017121726A1 (en) * | 2016-01-11 | 2017-07-20 | Compagnie Laitiere Europeenne | Milk calcium in dispersible powder form, method of preparation thereof and use of same to enrich food with calcium |
| WO2018016120A1 (en) * | 2016-07-22 | 2018-01-25 | 一般社団法人 Ｕｎｉｃａｌ | Food product containing calcium salt granules and dietary fiber |
| JP2018078870A (en) * | 2016-11-18 | 2018-05-24 | 一般社団法人 Ｕｎｉｃａｌ | Food product containing the granule of calcium salt and dietary fiber |
| WO2023209603A1 (en) * | 2022-04-29 | 2023-11-02 | Fonterra Co-Operative Group Limited | Dairy product and process |
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