JP4876137B2 - Method for producing calcium-containing milk composition - Google Patents
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- JP4876137B2 JP4876137B2 JP2009035299A JP2009035299A JP4876137B2 JP 4876137 B2 JP4876137 B2 JP 4876137B2 JP 2009035299 A JP2009035299 A JP 2009035299A JP 2009035299 A JP2009035299 A JP 2009035299A JP 4876137 B2 JP4876137 B2 JP 4876137B2
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- 210000004080 milk Anatomy 0.000 title claims description 208
- 235000013336 milk Nutrition 0.000 title claims description 207
- 239000008267 milk Substances 0.000 title claims description 207
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims description 177
- 239000011575 calcium Substances 0.000 title claims description 177
- 229910052791 calcium Inorganic materials 0.000 title claims description 177
- 239000000203 mixture Substances 0.000 title claims description 75
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 claims description 74
- 239000012528 membrane Substances 0.000 claims description 52
- 239000005018 casein Substances 0.000 claims description 34
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims description 34
- 235000021240 caseins Nutrition 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 33
- 239000007787 solid Substances 0.000 claims description 32
- 235000013861 fat-free Nutrition 0.000 claims description 30
- 108010046377 Whey Proteins Proteins 0.000 claims description 28
- 102000007544 Whey Proteins Human genes 0.000 claims description 28
- 239000005862 Whey Substances 0.000 claims description 14
- 235000021119 whey protein Nutrition 0.000 claims description 14
- 239000012466 permeate Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000001728 nano-filtration Methods 0.000 claims description 9
- 102000014171 Milk Proteins Human genes 0.000 claims description 8
- 108010011756 Milk Proteins Proteins 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 235000021239 milk protein Nutrition 0.000 claims description 8
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 7
- 239000008101 lactose Substances 0.000 claims description 7
- 235000020189 fortified milk Nutrition 0.000 claims description 6
- 238000001223 reverse osmosis Methods 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 235000013365 dairy product Nutrition 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 description 27
- 239000007864 aqueous solution Substances 0.000 description 24
- 239000000843 powder Substances 0.000 description 18
- 235000020183 skimmed milk Nutrition 0.000 description 15
- 239000000243 solution Substances 0.000 description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 235000014655 lactic acid Nutrition 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 235000013361 beverage Nutrition 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- -1 lactic acid ions Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 235000013351 cheese Nutrition 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- CPGKMLVTFNUAHL-UHFFFAOYSA-N [Ca].[Ca] Chemical compound [Ca].[Ca] CPGKMLVTFNUAHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000020121 low-fat milk Nutrition 0.000 description 1
- 235000008476 powdered milk Nutrition 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000020185 raw untreated milk Nutrition 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 235000008939 whole milk Nutrition 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Dairy Products (AREA)
Description
本発明はカルシウム含有乳組成物の製造方法に関する。 The present invention relates to a method for producing a calcium-containing milk composition.
乳中に含まれるカルシウムは、吸収性が良く、良質のカルシウム供給源として注目されている。しかし、乳からカルシウムを単に分離精製すると、不溶性のリン酸カルシウムとなるため、飲料に配合する際に分散性の悪さが問題となる。
これに対して、特許文献1には、分散性の良い乳カルシウム剤を製造する方法として、乳酸および乳酸イオンを含有する、ホエイを、UF膜又はNF膜処理して透過液を得、該透過液のpHを調整することにより乳カルシウムを沈殿させ、この乳カルシウムを乳蛋白質と混合したものを乳カルシウム剤とする方法が開示されている。
Calcium contained in milk is well absorbed and has attracted attention as a good source of calcium. However, when calcium is simply separated and purified from milk, it becomes insoluble calcium phosphate, so that poor dispersibility becomes a problem when blended into beverages.
On the other hand, in Patent Document 1, as a method for producing a milk calcium preparation with good dispersibility, whey containing lactic acid and lactic acid ions is treated with a UF membrane or NF membrane to obtain a permeate, A method is disclosed in which milk calcium is precipitated by adjusting the pH of the liquid, and a mixture of this milk calcium and milk protein is used as a milk calcium preparation.
特許文献1では、上記の製造方法で得られた乳カルシウム剤を水に分散させたときに、良好な分散性が得られることが確認されているが、本発明者等の知見によれば、該乳カルシウム剤を乳類に配合すると沈殿が生じてしまう場合がある。 In Patent Document 1, it has been confirmed that when the milk calcium preparation obtained by the above production method is dispersed in water, good dispersibility can be obtained, but according to the knowledge of the present inventors, When the milk calcium preparation is blended with milk, precipitation may occur.
本発明は前記事情に鑑みてなされたもので、乳類に乳カルシウム剤を配合してカルシウム強化乳組成物を製造する方法であって、沈殿が生じ難い製造方法を提供することを目的とする。 This invention is made | formed in view of the said situation, It aims at providing the manufacturing method which mix | blends a milk calcium agent with milk and manufactures a calcium fortified milk composition, Comprising: It is hard to produce precipitation. .
本発明者等が鋭意研究した結果、カルシウム強化乳組成物を調製する際に、得ようとする組成よりも低濃度の状態で乳類と乳カルシウム剤とを混合した後、該混合物を濃縮して所望の組成とすることにより、かかる濃縮工程を経ないで同じ組成に調製する場合に比べて沈殿が生じ難いことを見出し、本発明に至った。
すなわち、本発明のカルシウム強化乳組成物の製造方法は、カゼインを含有し、無脂乳固形分の含有量が0.03〜2質量%である乳類と、乳カルシウム剤を含み、カルシウム含有量が60mg/100g以下である乳カルシウム剤液とを混合した後に、ナノフィルトレーション膜(NF膜)または逆浸透膜(RO膜)で濃縮する工程を有することを特徴とするカルシウム強化乳組成物の製造方法である。
前記乳類中のカゼイン含有量は0.57質量%以下であることが好ましい。
As a result of intensive studies by the present inventors, when preparing a calcium-fortified milk composition, milk and a milk calcium preparation are mixed at a lower concentration than the composition to be obtained, and then the mixture is concentrated. Thus, the present inventors have found that by setting the desired composition, precipitation is less likely to occur compared to the case of preparing the same composition without going through such a concentration step.
That is, the production method of the calcium enriched milk composition of the present invention contain casein, seen containing a dairy product content of non-fat milk solids is 0.03 to 2 mass%, milk calcium, calcium A calcium-enriched milk comprising a step of concentrating with a nanofiltration membrane (NF membrane) or a reverse osmosis membrane (RO membrane) after mixing with a milk calcium solution having a content of 60 mg / 100 g or less. It is a manufacturing method of a composition.
The casein content in the milk is preferably 0.57% by mass or less.
前記乳カルシウム剤が、乳清蛋白質、乳糖、および乳カルシウムを含有し、全固形分に対する乳清蛋白質の含有量が5〜70質量%、カルシウム含有量が3〜15質量%であることが好ましい。 It is preferable that the milk calcium preparation contains whey protein, lactose, and milk calcium, the whey protein content is 5 to 70% by mass, and the calcium content is 3 to 15% by mass with respect to the total solid content. .
前記乳カルシウム剤が、ホエイを限外濾過膜(UF膜)処理またはナノフィルトレーション膜(NF膜)処理して得られる透過液のpHを6.0〜9.0に調整することにより乳カルシウムを沈殿させ、該乳カルシウムと乳蛋白質とを混合して得られる乳カルシウム剤であることが好ましい。 The milk calcium preparation adjusts the pH of the permeate obtained by treating whey with an ultrafiltration membrane (UF membrane) or a nanofiltration membrane (NF membrane) to 6.0 to 9.0. A milk calcium preparation obtained by precipitating calcium and mixing the milk calcium and milk protein is preferable.
本発明によれば、乳類に乳カルシウム剤を配合してカルシウム強化乳組成物を製造する際に、沈殿を生じ難くすることができる。 ADVANTAGE OF THE INVENTION According to this invention, when mix | blending a milk calcium agent with milk and manufacturing a calcium fortified milk composition, it can make it hard to produce precipitation.
本発明のカルシウム強化乳組成物の製造方法は、乳類と乳カルシウム剤とを混合し、得られた混合物をナノフィルトレーション膜(NF膜)または逆浸透膜(RO膜)で濃縮する工程を有する。 The method for producing a calcium-fortified milk composition of the present invention comprises mixing milk and a milk calcium preparation, and concentrating the obtained mixture with a nanofiltration membrane (NF membrane) or a reverse osmosis membrane (RO membrane). Have
<乳類>
本発明において、乳カルシウム剤と混合する乳類は、少なくともカゼインを含有する。乳類に乳カルシウム剤を配合したときに沈殿が生じる問題は、乳類がカゼインを含む場合に起こりやすいと考えられ、かかる場合に本発明の効果が充分に発揮される。
乳類中のカゼイン含有量は、乳カルシウム剤と混合する直前において、0.57質量%以下が好ましく、0.43質量%以下がより好ましい。該カゼイン含有量が0.57質量%以下であると、乳カルシウム剤と混合した混合液および該混合液を濃縮した組成物において沈殿が生じ難い。かかるカゼイン含有量を達成するために、必要に応じて乳類を希釈する。
乳カルシウム剤と混合する直前の乳類におけるカゼイン含有量の下限値は特に限定されないが、本発明による効果が充分に得られやすい点からは0.01質量%以上が好ましく、0.14質量%以上がより好ましい。
<Milk>
In the present invention, milk mixed with a milk calcium preparation contains at least casein. The problem that precipitation occurs when milk milk is added to milk is considered to occur easily when milk contains casein, and in such a case, the effects of the present invention are sufficiently exhibited.
The casein content in the milk is preferably 0.57% by mass or less, more preferably 0.43% by mass or less immediately before mixing with the milk calcium preparation. When the casein content is 0.57% by mass or less, precipitation is unlikely to occur in the mixed solution mixed with the milk calcium preparation and the composition obtained by concentrating the mixed solution. To achieve such casein content, the milk is diluted as necessary.
The lower limit of the casein content in the milk immediately before mixing with the milk calcium agent is not particularly limited, but is preferably 0.01% by mass or more, and preferably 0.14% by mass from the viewpoint that the effect of the present invention can be sufficiently obtained. The above is more preferable.
一方、濃縮工程を経て最終的に得られるカルシウム強化乳組成物におけるカゼイン含有量は1.43質量%以上が好ましく、2.29質量%以上がより好ましい。該カゼイン含有量が1.43質量%以上のカルシウム強化乳組成物は、濃縮工程を経ずに乳類と乳カルシウム剤とを混合する従来の方法で得ようとすると、沈殿が生じやすいため、本発明の効果が大きい。
該濃縮工程後のカルシウム強化乳組成物におけるカゼイン含有量の上限値は特に限定されないが、風味の点からは4.29質量%以下が好ましく、2.86質量%以下がより好ましい。
On the other hand, the casein content in the calcium-fortified milk composition finally obtained through the concentration step is preferably 1.43% by mass or more, and more preferably 2.29% by mass or more. The calcium-enriched milk composition having a casein content of 1.43% by mass or more is likely to precipitate when it is obtained by a conventional method in which milk and a milk calcium preparation are mixed without going through a concentration step. The effect of the present invention is great.
The upper limit of the casein content in the calcium-fortified milk composition after the concentration step is not particularly limited, but is preferably 4.29% by mass or less and more preferably 2.86% by mass or less from the viewpoint of flavor.
乳類中の無脂乳固形分の含有量は、上記カゼイン含有量の好ましい範囲が得られる範囲であればよく、特に限定されない。例えば、乳カルシウム剤と混合する直前の乳類における無脂乳固形分含有量は、0.03〜2質量%が好ましく、0.5〜1.5質量%がより好ましい。また濃縮工程を経て最終的に得られるカルシウム強化乳組成物における無脂乳固形分含有量は5〜15質量%が好ましく、8〜10質量%がより好ましい。 The content of the non-fat milk solid content in the milk is not particularly limited as long as the preferable range of the casein content can be obtained. For example, the non-fat milk solid content in the milk immediately before mixing with the milk calcium agent is preferably 0.03 to 2% by mass, and more preferably 0.5 to 1.5% by mass. Moreover, 5-15 mass% is preferable and, as for the non-fat milk solid content in the calcium fortified milk composition finally obtained through a concentration process, 8-10 mass% is more preferable.
乳類の具体例としては、生乳、牛乳、無脂肪牛乳、低脂肪牛乳、成分調整牛乳、濃縮乳または脱脂濃縮乳を必要に応じて水で希釈した希釈液;全粉乳または脱脂粉乳の水溶液等が挙げられる。
乳類は1種でもよく、2種以上を混合して用いてもよい。
Specific examples of milk include raw milk, milk, non-fat milk, low-fat milk, ingredient-adjusted milk, concentrated milk or skim-concentrated milk diluted with water as necessary; whole milk powder or skim milk aqueous solution, etc. Is mentioned.
One kind of milk may be used, or two or more kinds of milk may be mixed and used.
<乳カルシウム剤>
本発明において用いられる乳カルシウム剤は、乳由来のカルシウム、すなわち乳カルシウムを含有する組成物であり、カゼインを含まないものである。乳カルシウム剤は、乳カルシウムの他に、乳清蛋白質および乳糖を含むことが好ましい。
乳カルシウム剤におけるカルシウム含有量は、全固形分に対して3〜15質量%が好ましく、3〜10質量%がより好ましい。3質量%未満であるとカルシウム強化剤として不適当であり、15質量を超えるとカルシウムの分散性が悪くなる。
なお、本発明におけるカルシウム含有量は、ICP発光分光分析法により得られる値である。
<Milk calcium preparation>
The milk calcium agent used in the present invention is a composition containing calcium derived from milk, that is, milk calcium, and does not contain casein. The milk calcium preparation preferably contains whey protein and lactose in addition to milk calcium.
3-15 mass% is preferable with respect to the total solid, and, as for the calcium content in a milk calcium preparation, 3-10 mass% is more preferable. If it is less than 3% by mass, it is unsuitable as a calcium fortifier, and if it exceeds 15% by mass, the dispersibility of calcium will be poor.
The calcium content in the present invention is a value obtained by ICP emission spectroscopic analysis.
乳カルシウム剤における乳清蛋白質の含有量は、全固形分に対して5〜70質量%が好ましく、8〜40質量%がより好ましい。5質量%未満であるとカルシウムの分散性が悪くなり、70質量%を超えると好ましくない風味が増大する。
乳カルシウム剤における乳糖の含有量は全固形分に対して15〜92質量%が好ましい。
The content of whey protein in the milk calcium preparation is preferably 5 to 70 mass%, more preferably 8 to 40 mass%, based on the total solid content. When the amount is less than 5% by mass, the dispersibility of calcium deteriorates, and when it exceeds 70% by mass, an unfavorable flavor increases.
The content of lactose in the milk calcium preparation is preferably 15 to 92% by mass with respect to the total solid content.
乳カルシウム、乳清蛋白質および乳糖を上記の好ましい範囲で含有する乳カルシウム剤は、ホエイを限外濾過膜(UF膜)処理またはナノフィルトレーション膜(NF膜)処理して透過液を得、該透過液のpHを6.0〜9.0に調整することにより乳カルシウムを沈殿させ、該乳カルシウムと乳蛋白質とを混合する方法で製造できる。
例えば、上記特許文献1に記載の製造方法で製造することができる。ただしホエイは、乳酸および乳酸イオンを含有するものに限られない。
すなわち、限外濾過膜(UF膜)処理またはナノフィルトレーション膜(NF膜)処理に供するホエイとしては、乳を乳酸発酵させた乳酸ホエイのほか、チーズホエイ、塩酸ホエイ等を用いることができる。また前記透過液のpHを6.0〜9.0に調整して乳カルシウムを沈殿させる工程における、該透過液の温度は30〜80℃が好ましい。乳カルシウムと乳蛋白質とを混合する工程においては、透過液中の沈殿を回収して得られるスラリー状の沈殿と、乳蛋白質を含有する水溶液とを混合することが好ましい。乳蛋白質として乳清蛋白質を用いることが好ましい。乳蛋白質を含有する水溶液は、乳清蛋白質および乳糖を含むものが好ましい。例えば、ホエイパウダーの水溶液、蛋白質濃縮ホエイパウダーの水溶液等が用いられる。
A milk calcium preparation containing milk calcium, whey protein and lactose in the above preferred range is obtained by treating whey with an ultrafiltration membrane (UF membrane) or a nanofiltration membrane (NF membrane) to obtain a permeate, By adjusting the pH of the permeate to 6.0 to 9.0, milk calcium can be precipitated, and the milk calcium and milk protein can be mixed.
For example, it can be manufactured by the manufacturing method described in Patent Document 1. However, whey is not limited to those containing lactic acid and lactic acid ions.
That is, as whey used for ultrafiltration membrane (UF membrane) treatment or nanofiltration membrane (NF membrane) treatment, in addition to lactic acid whey obtained by lactic fermentation of milk, cheese whey, hydrochloric acid whey, and the like can be used. . The temperature of the permeate is preferably 30 to 80 ° C. in the step of precipitating milk calcium by adjusting the pH of the permeate to 6.0 to 9.0. In the step of mixing milk calcium and milk protein, it is preferable to mix a slurry-like precipitate obtained by collecting the precipitate in the permeate and an aqueous solution containing the milk protein. It is preferable to use whey protein as the milk protein. The aqueous solution containing milk protein preferably contains whey protein and lactose. For example, an aqueous solution of whey powder, an aqueous solution of protein concentrated whey powder, or the like is used.
本発明で用いられる乳カルシウム剤は、液体であっても、粉末等の固体であってもよいが、乳類と混合する際は、乳カルシウム剤を含む液状の乳カルシウム剤液とする。乳カルシウム剤が液体である場合は、そのまま乳カルシウム剤液として使用できるが、希釈して用いることが好ましい。乳カルシウム剤液は乳カルシウム剤の溶液でもよく、分散液でもよい。好ましくは乳カルシウム剤の水溶液が用いられる。
乳類と混合する直前の乳カルシウム剤液における、カルシウム含有量は、60mg/100g以下であることが好ましい。該カルシウム含有量が60mg/100g以下であると、乳類と乳カルシウム剤液を混合した混合液、および該混合液を濃縮した組成物において沈殿の生成が良好に抑えられる。
The milk calcium preparation used in the present invention may be a liquid or a solid such as a powder, but when mixed with milk, a liquid milk calcium preparation containing a milk calcium preparation is used. When the milk calcium preparation is a liquid, it can be used as it is as a milk calcium preparation liquid, but it is preferably diluted. The milk calcium preparation solution may be a milk calcium preparation solution or a dispersion. Preferably, an aqueous solution of a milk calcium preparation is used.
The calcium content in the milk calcium preparation immediately before mixing with milk is preferably 60 mg / 100 g or less. When the calcium content is 60 mg / 100 g or less, the formation of precipitates is satisfactorily suppressed in a mixed solution obtained by mixing milk and a milk calcium solution, and a composition obtained by concentrating the mixed solution.
また、濃縮工程を経て最終的に得られるカルシウム強化乳組成物におけるカルシウム含有量は、100mg/100g以上が好ましい。該カルシウム含有量が100mg/100g以上であるカルシウム強化乳組成物は、濃縮工程を経ずに乳類と乳カルシウム剤とを混合する従来の方法で得ようとすると沈殿が生じやすいため、本発明の効果が大きい。 Further, the calcium content in the calcium-fortified milk composition finally obtained through the concentration step is preferably 100 mg / 100 g or more. Since the calcium-enriched milk composition having a calcium content of 100 mg / 100 g or more tends to precipitate when it is obtained by a conventional method in which milk and a milk calcium preparation are mixed without going through a concentration step, the present invention The effect is great.
<混合工程>
乳類と乳カルシウム剤液との混合は、液温10℃以下で行うことが好ましい。
<濃縮工程>
乳類と乳カルシウム剤液との混合液の濃縮は、ナノフィルトレーション膜(NF膜)または逆浸透膜(RO膜)を用いて行う。NF膜またはRO膜を用いることにより、固形分の組成を変化させずに濃縮することができる。
該混合液の濃縮は、液温10℃以下で行うことが好ましい。
濃縮倍率は、混合直前の乳類および乳カルシウム剤液における各成分の好ましい含有量と、濃縮後のカルシウム強化乳組成物における各成分の好ましい含有量に応じて設定され、特に限定されない。例えば5〜10倍程度が好ましく、5〜7倍程度がより好ましい。
<Mixing process>
The mixing of the milk and the milk calcium solution is preferably performed at a liquid temperature of 10 ° C. or lower.
<Concentration process>
Concentration of the mixture of milk and milk calcium solution is performed using a nanofiltration membrane (NF membrane) or a reverse osmosis membrane (RO membrane). By using the NF membrane or the RO membrane, it is possible to concentrate without changing the composition of the solid content.
The concentration of the mixed solution is preferably performed at a liquid temperature of 10 ° C. or lower.
The concentration ratio is set according to the preferable content of each component in the milk and milk calcium preparation immediately before mixing and the preferable content of each component in the calcium-enriched milk composition after concentration, and is not particularly limited. For example, about 5 to 10 times is preferable, and about 5 to 7 times is more preferable.
本発明の製造方法にあっては、乳類と乳カルシウム剤を混合する際に、通常、混合だけで所望の組成が得られるように乳類と乳カルシウム剤を調製するところ、両者を希釈するなどして低濃度の状態に調製して混合した後、ナノフィルトレーション膜(NF膜)または逆浸透膜(RO膜)で濃縮して所望の組成にすることにより、沈殿が生じるのを防止できる。
かかる効果が得られる理由は明確ではないが、例えば特許文献1に記載されているような、水への分散性が改善された乳カルシウム剤であっても、乳類と混合すると沈殿を生じるのは、乳類中のカゼインとカルシウムとが反応して不溶性の反応物が生成するからであり、かかる反応は、カゼインおよびカルシウムの濃度が高い場合に生じ易いためと考えられる。
In the production method of the present invention, when mixing milk and milk calcium preparation, usually milk and milk calcium preparation are prepared so that a desired composition can be obtained only by mixing, and both are diluted. After preparing and mixing in a low concentration state, etc., it is concentrated with a nanofiltration membrane (NF membrane) or reverse osmosis membrane (RO membrane) to obtain the desired composition, thereby preventing precipitation. it can.
The reason why such an effect is obtained is not clear, but, for example, even a milk calcium agent with improved water dispersibility, as described in Patent Document 1, causes precipitation when mixed with milk. This is because casein and calcium in milk react with each other to produce an insoluble reactant, and this reaction is considered to occur easily when the concentrations of casein and calcium are high.
以下に実施例を用いて本発明をさらに詳しく説明するが、本発明はこれら実施例に限定されるものではない。以下において「%」は、特に断りのない限り「質量%」を意味する。
[調製例1:乳カルシウム剤の調製]
乳酸ホエイ300kgを分画分子量10kDaのUF膜(DK3840C:Desalination社製)で10倍まで濃縮し、透過液270kgを得た。次にこの透過液をRO膜で3倍に濃縮し、濃縮液85kgを得た。この濃縮液を50℃に昇温し、1N水酸化ナトリウムを添加してpH7.0に調整した。1時間後、クラリファイヤーで処理して、沈殿4.4kgを回収した。このようにして得られた沈殿と乳清蛋白質濃縮物(組成;乳清蛋白質35%、乳糖55%、脂肪2%、灰分5%及び水分3%)の15質量%水溶液とを、全固形分当りのカルシウム量が5質量%となるように混合し、均質圧500kg/cm2で均質処理した後、噴霧乾燥して乳カルシウム剤とした。得られた乳カルシウム剤における乳清蛋白質含有量は28.7%、カルシウム含有量は4.77%であった。
Hereinafter, the present invention will be described in more detail using examples, but the present invention is not limited to these examples. In the following, “%” means “% by mass” unless otherwise specified.
[Preparation Example 1: Preparation of milk calcium preparation]
300 kg of lactic acid whey was concentrated up to 10 times with a UF membrane (DK3840C: manufactured by Desalination) having a molecular weight cut off of 10 kDa to obtain 270 kg of a permeate. Next, this permeate was concentrated three times with an RO membrane to obtain 85 kg of a concentrate. The concentrated solution was heated to 50 ° C., and adjusted to pH 7.0 by adding 1N sodium hydroxide. After 1 hour, it was treated with a clarifier to recover 4.4 kg of precipitate. Thus obtained precipitate and a whey protein concentrate (composition: whey protein 35%, lactose 55%, fat 2%, ash content 5% and water content 3%) in a 15% by mass aqueous solution The mixture was mixed so that the amount of calcium per unit was 5% by mass, homogenized at a homogeneous pressure of 500 kg / cm 2 , and then spray-dried to obtain a milk calcium preparation. The whey protein content in the obtained milk calcium preparation was 28.7%, and the calcium content was 4.77%.
[調製例2:乳カルシウム剤の調製]
チーズホエイ200kgを調製例1と同じUF膜で10倍まで濃縮し、透過液180kgを得た。次にこの透過液を50℃に昇温し、1N水酸化ナトリウムを添加してpH7.0に調整した。1時間後、クラリファイヤーで処理して、沈殿2.6kgを回収した。このようにして得られた沈殿と、調製例1と同じ乳清蛋白質濃縮物の15質量%水溶液とを、全固形分当りのカルシウム量が5質量%となるように混合し、均質圧500kg/cm2で均質処理した後、噴霧乾燥して乳カルシウム剤とした。得られた乳カルシウム剤における乳清蛋白質含有量は28.7%、カルシウム含有量は4.77%であった。
[Preparation Example 2: Preparation of milk calcium preparation]
200 kg of cheese whey was concentrated 10 times with the same UF membrane as in Preparation Example 1 to obtain 180 kg of permeate. Next, this permeate was heated to 50 ° C., and adjusted to pH 7.0 by adding 1N sodium hydroxide. After 1 hour, it was treated with a clarifier to recover 2.6 kg of precipitate. The precipitate thus obtained and a 15% by mass aqueous solution of the same whey protein concentrate as in Preparation Example 1 were mixed so that the amount of calcium per total solid content was 5% by mass, and a homogeneous pressure of 500 kg / After homogeneous treatment at cm 2 , it was spray-dried to obtain a milk calcium preparation. The whey protein content in the obtained milk calcium preparation was 28.7%, and the calcium content was 4.77%.
[試験例1:従来法]
濃縮工程を経ずに、所望の組成が得られるように乳類と乳カルシウム剤とを混合する従来の方法でカルシウム強化乳組成物を調製した。
乳類としては、脱脂粉乳の水溶液を用い、混合前の無脂乳固形分濃度が10質量%(カゼイン濃度2.86質量%)と20質量%(カゼイン濃度5.72質量%)の2種を用意した。乳カルシウム剤としては、調製例1で得られた乳カルシウム剤(カルシウム含有量4.77%)の水溶液を用い、混合前のカルシウム濃度が100、200、250、300、400、500、600(単位:mg/100g)の7種を用意した。
[Test Example 1: Conventional method]
A calcium-fortified milk composition was prepared by a conventional method in which milk and a milk calcium preparation were mixed so that a desired composition was obtained without going through a concentration step.
As the milk, an aqueous solution of skim milk powder is used, and the non-fat milk solid content concentration before mixing is 10% by mass (casein concentration 2.86% by mass) and 20% by mass (casein concentration 5.72% by mass). Prepared. As the milk calcium preparation, the aqueous solution of the milk calcium preparation (calcium content 4.77%) obtained in Preparation Example 1 was used, and the calcium concentration before mixing was 100, 200, 250, 300, 400, 500, 600 ( Seven types (unit: mg / 100 g) were prepared.
表1に示す組み合わせで、脱脂粉乳の水溶液と、乳カルシウム剤の水溶液を、等量混合し、混合物(カルシウム強化乳組成物)中に生じた沈殿の量を測定した。該混合物中における、無脂乳固形分濃度、カルシウム濃度、および沈殿量を表1に示す。
混合は、10℃の脱脂粉乳水溶液をプロペラ式攪拌装置を用いて、60rpmで攪拌し、その中に10℃の乳カルシウム剤水溶液1kgを10ml/秒の速度で添加した。
沈殿量(単位:ml/30ml)の測定は、容量50mlの遠心管に30mlの混合物(カルシウム強化乳組成物)を入れ、遠心機(himac CT5DL、日立工機社製)を用いて、回転半径16.2cmで2000rpm、10分間の遠心分離を行い、遠心管の容量目盛により沈殿量を測定する方法で行った(以下、同様。)
In the combinations shown in Table 1, an equal amount of an aqueous solution of skim milk powder and an aqueous solution of a milk calcium preparation were mixed, and the amount of precipitate produced in the mixture (calcium-enriched milk composition) was measured. Table 1 shows the solid content of non-fat milk, the calcium concentration, and the amount of precipitation in the mixture.
Mixing was performed by stirring a 10 ° C. skimmed milk powder aqueous solution at 60 rpm using a propeller type stirring device, and adding 1 kg of a 10 ° C. milk calcium agent aqueous solution at a rate of 10 ml / second.
The amount of precipitation (unit: ml / 30 ml) was measured by putting 30 ml of the mixture (calcium-enriched milk composition) into a 50 ml capacity centrifuge tube and using a centrifuge (himac CT5DL, manufactured by Hitachi Koki Co., Ltd.). Centrifugation was performed at 16.2 cm at 2000 rpm for 10 minutes, and the amount of precipitation was measured with a volumetric scale of the centrifuge tube (the same applies hereinafter).
カルシウム強化乳組成物が飲料として用いられる場合、カルシウム強化乳組成物中の沈殿は、飲料をプレート式殺菌機で殺菌する際にプレートへの付着物の原因となりやすい。また飲料の保存中に沈殿が生成するのは好ましくない。これらの点からカルシウム強化乳組成物における沈殿量は、0.10ml/30ml以下が望ましい。沈殿量が0.10ml/30ml以下のものを「適」、これを超えるものを「否」と評価して表1に示す。 When the calcium fortified milk composition is used as a beverage, precipitation in the calcium fortified milk composition tends to cause deposits on the plate when the beverage is sterilized with a plate sterilizer. In addition, it is not preferable that a precipitate is formed during storage of the beverage. From these points, the amount of precipitation in the calcium enriched milk composition is preferably 0.10 ml / 30 ml or less. Table 1 shows that the amount of precipitation is 0.10 ml / 30 ml or less is evaluated as “appropriate” and the amount exceeding this is evaluated as “no”.
[試験例2:本発明の製造方法]
得ようとする組成よりも低濃度の状態で乳類と乳カルシウム剤とを混合した後、該混合物を濃縮して所望の組成とする方法でカルシウム強化乳組成物を調製した。
混合前の乳類として、無脂乳固形分濃度が2質量%(カゼイン濃度0.57質量%)の脱脂粉乳水溶液を用意した。乳カルシウム剤としては、試験例1と同じ乳カルシウム剤の水溶液を用い、混合前のカルシウム濃度が40、50、60(単位:mg/100g)の3種を用意した。
該脱脂粉乳水溶液と3種の乳カルシウム剤水溶液を、それぞれ等量混合し、脱脂粉乳由来の無脂乳固形分濃度が1質量%(カゼイン濃度0.29質量%)で、乳カルシウム剤由来のカルシウム濃度が20、25、30(単位:mg/100g)の3種の混合物を得た。混合条件は試験例1と同様である。得られた混合物(濃縮前)中の沈殿量を試験例1と同様にして測定した。混合前における無脂乳固形分濃度およびカルシウム濃度を表2に示す。
[Test Example 2: Production method of the present invention]
After mixing the milk and the milk calcium preparation in a concentration lower than the composition to be obtained, a calcium-fortified milk composition was prepared by a method of concentrating the mixture to obtain a desired composition.
As milk before mixing, the skim milk powder aqueous solution whose nonfat milk solid content density | concentration is 2 mass% (casein density | concentration 0.57 mass%) was prepared. As the milk calcium preparation, the same aqueous solution of milk calcium preparation as in Test Example 1 was used, and three kinds of calcium concentrations before mixing, 40, 50 and 60 (unit: mg / 100 g) were prepared.
The same amount of the skim milk powder aqueous solution and the three types of milk calcium agent aqueous solutions are mixed, and the non-fat milk solid content concentration derived from skim milk powder is 1% by mass (casein concentration 0.29% by mass). Three types of mixtures having calcium concentrations of 20, 25, and 30 (unit: mg / 100 g) were obtained. The mixing conditions are the same as in Test Example 1. The amount of precipitation in the obtained mixture (before concentration) was measured in the same manner as in Test Example 1. Table 2 shows the non-fat milk solid content concentration and calcium concentration before mixing.
こうして得られた混合物を、NF膜を用い10倍、又は5倍に濃縮し、6種類のカルシウム強化乳組成物を得た。NF膜はNTR−7450HG(日東電工社製)を用い、10℃にて、入口圧力2.65MPa、出口圧力2.58MPaの条件で濃縮を行った。
得られたカルシウム強化乳組成物中の沈殿量を試験例1と同様にして測定した。濃縮後のカルシウム強化組成物中における、無脂乳固形分濃度、カルシウム濃度、および沈殿量を表2に示す。
The mixture thus obtained was concentrated 10 times or 5 times using an NF membrane to obtain six types of calcium-fortified milk compositions. As the NF membrane, NTR-7450HG (manufactured by Nitto Denko Corporation) was used, and concentration was performed at 10 ° C. under conditions of an inlet pressure of 2.65 MPa and an outlet pressure of 2.58 MPa.
The amount of precipitation in the obtained calcium-enriched milk composition was measured in the same manner as in Test Example 1. Table 2 shows the non-fat milk solid content concentration, the calcium concentration, and the precipitation amount in the calcium fortified composition after concentration.
表1に示されるように、無脂乳固形分が10質量%(カゼイン濃度2.86質量%)または5質量%(カゼイン濃度1.43質量%)で、カルシウム濃度が100mg/100g以上であるカルシウム強化乳組成物を、従来法で製造すると沈殿量が多く、評価は「否」となる。
これに対して、表2に示されるように、無脂乳固形分が10質量%(カゼイン濃度2.86質量%)で、カルシウム濃度が200、250、300(mg/100g)であるカルシウム強化乳組成物、または無脂乳固形分が5質量%(カゼイン濃度1.43質量%)で、カルシウム濃度が100、125、150(mg/100g)であるカルシウム強化乳組成物であっても、本発明の方法で製造すると沈殿量はいずれも0.05ml/30mlであり、ほとんど沈殿は生じない。
また、表1の結果より、無脂乳固形分が10質量%または5質量%であっても、カルシウム濃度が50mg/100gであるカルシウム強化乳組成物は、従来法で製造しても沈殿量は少ないことがわかる。
As shown in Table 1, the solid content of non-fat milk is 10% by mass (casein concentration 2.86% by mass) or 5% by mass (casein concentration 1.43% by mass), and the calcium concentration is 100 mg / 100 g or more. When a calcium-enriched milk composition is produced by a conventional method, the amount of precipitation is large, and the evaluation is “No”.
On the other hand, as shown in Table 2, the calcium fortification with non-fat milk solid content of 10% by mass (casein concentration 2.86% by mass) and calcium concentration of 200, 250, 300 (mg / 100 g) Even a milk composition or a calcium-fortified milk composition having a non-fat milk solid content of 5% by mass (casein concentration of 1.43% by mass) and a calcium concentration of 100, 125, 150 (mg / 100 g), When produced by the method of the present invention, the amount of precipitation is 0.05 ml / 30 ml, and almost no precipitation occurs.
In addition, from the results of Table 1, even if the non-fat milk solid content is 10% by mass or 5% by mass, the calcium-enriched milk composition having a calcium concentration of 50 mg / 100 g can be precipitated even if produced by the conventional method. You can see that there are few.
[実施例1]
無脂乳固形分濃度が2%(カゼイン濃度0.57質量%)となるように水に溶解した脱脂粉乳(森永乳業社製)の水溶液150kgと、調製例1で得られた乳カルシウム剤を、カルシウム濃度が60mg/100gとなるように水に溶解した乳カルシウム剤水溶液150kgを混合した。混合後、NF膜(製品名:NTR−7450HG、日東電工社製)で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が300mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物における沈殿量は0.05ml/30mlであった。
[Example 1]
150 kg of an aqueous solution of skim milk powder (manufactured by Morinaga Milk Industry Co., Ltd.) dissolved in water so that the non-fat milk solid content concentration is 2% (casein concentration 0.57% by mass), and the milk calcium preparation obtained in Preparation Example 1 Then, 150 kg of an aqueous milk calcium preparation solution dissolved in water so as to have a calcium concentration of 60 mg / 100 g was mixed. After mixing, it is concentrated up to 10 times with an NF membrane (product name: NTR-7450HG, manufactured by Nitto Denko Corporation), the non-fat milk solid content derived from skim milk powder is 10% (casein concentration: 2.86% by mass), milk calcium preparation A calcium-fortified milk composition having a calcium content derived from 300 mg / 100 g was obtained. The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例2]
実施例1と同じ脱脂粉乳水溶液150kgと、調製例1で得られた乳カルシウム剤を、カルシウム濃度が40mg/100gとなるように水に溶解した乳カルシウム剤水溶液150kgを混合した。混合後、実施例1と同じNF膜で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が200mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物における沈殿量0.05ml/30mlであった。
[Example 2]
150 kg of the same nonfat dry milk aqueous solution as in Example 1 and 150 kg of an aqueous milk calcium preparation obtained by dissolving the milk calcium preparation obtained in Preparation Example 1 in water so that the calcium concentration is 40 mg / 100 g were mixed. After mixing, it was concentrated up to 10 times with the same NF membrane as in Example 1, the nonfat milk solid content derived from skim milk powder was 10% (casein concentration 2.86% by mass), and the calcium content derived from the milk calcium preparation was 200 mg / 100 g of calcium enriched milk composition was obtained. The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例3]
無脂乳固形分濃度が2%(カゼイン濃度0.57質量%)となるように水で希釈した脱脂濃縮乳(森永乳業社製)の希釈液150kgと、実施例1と同じカルシウム濃度60mg/100gの乳カルシウム剤水溶液150kgを混合した。混合後、実施例1と同じNF膜で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が300mg/100gのカルシウム強化乳組成物を得た。
濃縮後のカルシウム強化乳組成物における沈殿量は0.05ml/30mlであった。
[Example 3]
150 kg of dilute concentrated milk (manufactured by Morinaga Milk Industry Co., Ltd.) diluted with water so that the non-fat milk solids concentration is 2% (casein concentration 0.57% by mass), and the same calcium concentration as in Example 1 60 mg / 150 kg of a 100 g milk calcium preparation aqueous solution was mixed. After mixing, it was concentrated up to 10 times with the same NF membrane as in Example 1, the nonfat milk solid content derived from skim milk powder was 10% (casein concentration 2.86% by mass), and the calcium content derived from the milk calcium preparation was 300 mg / 100 g of calcium enriched milk composition was obtained.
The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例4]
実施例1と同じ脱脂粉乳水溶液150kgと、実施例1と同じカルシウム濃度60mg/100gの乳カルシウム剤水溶液150kgを混合した。混合後、RO膜(製品名:NTR−759HG、日東電工社製)で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が300mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物における沈殿量は0.05ml/30mlであった。
[Example 4]
150 kg of the same nonfat dry milk aqueous solution as in Example 1 and 150 kg of an aqueous milk calcium preparation solution having the same calcium concentration of 60 mg / 100 g as in Example 1 were mixed. After mixing, it is concentrated up to 10 times with RO membrane (product name: NTR-759HG, manufactured by Nitto Denko Corporation), non-fat milk solid content derived from skim milk powder is 10% (casein concentration 2.86% by mass), milk calcium preparation A calcium-fortified milk composition having a calcium content derived from 300 mg / 100 g was obtained. The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例5]
実施例3と同じ脱脂濃縮乳の希釈液150kgと、実施例2と同じカルシウム濃度40mg/100gの乳カルシウム剤水溶液150kgを混合した。混合後、実施例1と同じNF膜で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が200mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物における沈殿量は0.05ml/30mlであった。
[Example 5]
150 kg of the same non-fat concentrated milk dilution as in Example 3 and 150 kg of an aqueous calcium calcium solution having a calcium concentration of 40 mg / 100 g as in Example 2 were mixed. After mixing, it was concentrated up to 10 times with the same NF membrane as in Example 1, the nonfat milk solid content derived from skim milk powder was 10% (casein concentration 2.86% by mass), and the calcium content derived from the milk calcium preparation was 200 mg / 100 g of calcium enriched milk composition was obtained. The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例6]
実施例1と同じ脱脂粉乳水溶液150kgと、実施例2と同じカルシウム濃度40mg/100gの乳カルシウム剤水溶液150kgを混合した。混合後、実施例4と同じRO膜で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が200mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物における沈殿量は0.05ml/30mlであった。
[Example 6]
150 kg of the same nonfat dry milk aqueous solution as in Example 1 and 150 kg of an aqueous milk calcium preparation solution having the same calcium concentration of 40 mg / 100 g as in Example 2 were mixed. After mixing, it was concentrated up to 10 times with the same RO membrane as in Example 4, the non-fat milk solid content derived from skim milk powder was 10% (casein concentration 2.86% by mass), and the calcium content derived from the milk calcium preparation was 200 mg / 100 g of calcium enriched milk composition was obtained. The amount of precipitation in the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
[実施例7]
実施例1と同じ脱脂粉乳水溶液150kgと、調製例2で得られた乳カルシウム剤を、カルシウム濃度が60mg/100gに水に溶解した乳カルシウム剤水溶液150kgを混合した。混合後、実施例1と同じNF膜で10倍まで濃縮し、脱脂粉乳由来の無脂乳固形分が10%(カゼイン濃度2.86質量%)、乳カルシウム剤由来のカルシウム含有量が300mg/100gのカルシウム強化乳組成物を得た。濃縮後のカルシウム強化乳組成物の沈殿量は0.05ml/30mlであった。
[Example 7]
150 kg of the same nonfat dry milk aqueous solution as in Example 1 and 150 kg of the aqueous milk calcium preparation obtained by dissolving the milk calcium preparation obtained in Preparation Example 2 in water at a calcium concentration of 60 mg / 100 g were mixed. After mixing, it was concentrated up to 10 times with the same NF membrane as in Example 1, the nonfat milk solid content derived from skim milk powder was 10% (casein concentration 2.86% by mass), and the calcium content derived from the milk calcium preparation was 300 mg / 100 g of calcium enriched milk composition was obtained. The amount of precipitation of the calcium enriched milk composition after concentration was 0.05 ml / 30 ml.
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