JP2004267223A - Method for producing milk beverage - Google Patents
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本発明は、乳飲料の製造方法に関するもので、詳しくは、PETボトル入り飲料に用いられるUHT殺菌を施した際の乳化物の熱安定性および長期間の保存安定性の優れた乳飲料を得ることができる乳飲料の製造方法に関する。 The present invention relates to a method for producing a milk beverage, and more specifically, to obtain a milk beverage having excellent heat stability and long-term storage stability of an emulsion when subjected to UHT sterilization used for a PET bottled beverage. And a method for producing a milk beverage.
ミルクコーヒーなどの乳成分を含む乳飲料は、保存のために加熱殺菌処理を経て製造されるが、生残する耐熱性の強い高温芽胞菌の増殖による変敗を防止するためにショ糖脂肪酸エステルを添加することが広く行われている。また、保存中における脂肪の遊離や蛋白質の凝集の発生を抑え、乳化安定性を長期間保持するために、ポリグリセリン脂肪酸エステルとショ糖脂肪酸エステルを併用する方法が提案されており(特許文献1、特許文献2等)、これらの方法は安定性の面で非常に優れたものである。
ところが、これらの方法はレトルト殺菌では問題ないが、近年、PET飲料の殺菌に利用されているUHT殺菌を施した場合には、含有される乳蛋白質が熱変性を起こして沈殿し易くなり、保存安定性が低下することから効果不十分となる。このため、UHT殺菌の処理時間を最小限に抑え、且つペクチン、カラギーナン等の増粘多糖類を添加する方法が行われているが、長期間の保存安定化には十分とはいえない。 However, these methods have no problem in retort sterilization, but in recent years, when UHT sterilization used for sterilization of PET beverages is performed, the milk protein contained is easily denatured by heat and easily precipitates. The effect is insufficient because the stability is reduced. For this reason, a method of minimizing the treatment time of UHT sterilization and adding a thickening polysaccharide such as pectin and carrageenan has been performed, but it is not sufficient for long-term storage stability.
そこで、本発明者らは、特定の曇点を有するポリグリセリン脂肪酸エステルを含有する乳飲料が、UHT殺菌を施しても長期間の乳化安定性を保持することができることを見出し、本発明に到達した。すなわち、本発明の要旨は、乳飲料を超高温(UHT)殺菌処理を経て製造するにおいて、乳飲料中に、20%塩化ナトリウム水溶液中1重量%濃度で測定した曇点が90℃以上であるポリグリセリン脂肪酸エステルを含有させることを特徴とする乳飲料の製造方法に存する。 Thus, the present inventors have found that a milk beverage containing a polyglycerol fatty acid ester having a specific cloud point can maintain long-term emulsion stability even after being subjected to UHT sterilization, and reached the present invention. did. That is, the gist of the present invention is that when a milk beverage is manufactured through ultra-high temperature (UHT) sterilization, the cloud point measured at a 1% by weight concentration in a 20% aqueous sodium chloride solution in the milk beverage is 90 ° C. or higher. The present invention relates to a method for producing a dairy beverage, comprising a polyglycerin fatty acid ester.
本発明により、乳脂肪分、乳蛋白質を含有し、且つ、UHT殺菌を施しても長期間の乳化安定性を保持することができる乳飲料の製造方法が提供される。 According to the present invention, there is provided a method for producing a milk beverage which contains milk fat and milk protein and which can maintain long-term emulsion stability even when subjected to UHT sterilization.
本発明における乳飲料は、乳成分である乳脂肪、乳蛋白質を含有する飲料であって、具体的には、全脂肪粉乳液、ミルクコーヒー、ミルク紅茶等が挙げられる。乳成分としては、牛乳、全脂粉乳、スキンミルクパウダー、フレッシュクリーム等が挙げられるが、脱脂粉乳などの蛋白質とバターやミルクオイル等の乳脂とを個別に加えて調整してもよい。乳成分の含量は、牛乳換算で5〜60重量%、好ましくは10〜25重量%である。乳飲料のpHとしては、通常、5.5〜7.0の中性または弱酸性であることが好ましい。勿論、この他、砂糖、香料、ビタミンなどの公知の配合剤を加えてもよい。 The milk beverage according to the present invention is a beverage containing milk fat and milk protein as milk components, and specific examples include full fat milk powder, milk coffee, milk tea and the like. Examples of the milk component include milk, whole-fat milk powder, skin milk powder, fresh cream, and the like. Proteins such as skim milk powder and milk fat such as butter and milk oil may be separately added and adjusted. The content of the milk component is 5 to 60% by weight, preferably 10 to 25% by weight in terms of milk. Generally, the pH of the milk drink is preferably 5.5 to 7.0, which is neutral or weakly acidic. Of course, other known ingredients such as sugar, fragrance and vitamin may be added.
本発明における乳飲料に含有されるポリグリセリン脂肪酸エステルは、ポリグリセリンと脂肪酸との反応により得られるエステル体と未反応ポリグリセリンの混合物であり、この混合物特性は、ポリグリセリンの重合度、脂肪酸の種類、脂肪酸のエステル化率(未反応ポリグリセリン量)、エステル化の内訳比率(モノ体、ジ体、トリ体などの割合)などにより決定されるが、これら全ての要件の特定は極めて難しい。また、この特性は一般的に界面活性剤の特性を規定するために、用いられるHLBだけでは規定することができない。そこで、本発明では、近年、新たな規定法として提唱されている「曇点」での特定を行うものである。 The polyglycerin fatty acid ester contained in the milk beverage in the present invention is a mixture of an ester and an unreacted polyglycerin obtained by a reaction between polyglycerin and a fatty acid. It is determined by the type, the esterification ratio of fatty acids (the amount of unreacted polyglycerin), the breakdown ratio of esterification (the ratio of mono-, di-, and tri-forms), but it is extremely difficult to specify all of these requirements. In addition, since this property generally defines the property of the surfactant, it cannot be defined only by the HLB used. Therefore, in the present invention, identification is performed at a “cloud point” which has been recently proposed as a new regulation method.
「曇点」とは水和している非イオン性界面活性剤が高温で脱水和して水から分離してくる現象であり、ポリオキシエチレン系の界面活性剤ではよく知られている。曇点はポリグリセリン脂肪酸エステルの構造・組成に鋭敏であり、脂肪酸石鹸の影響をも反映するので、親水性の程度や組成の違いをより正確に識別することができる。さらに、簡便に測定できることから、ポリグリセリン脂肪酸エステルの特徴を代表する物性として最も優れている。従って、ポリグリセリン脂肪酸エステルにおいては、曇点はHLB(親水性と疎水性のバランス)よりも有用な指標となる。ポリグリセリンは多数の水酸基を持つために、ポリオキシエチレン系の界面活性剤と比較すると、全般に曇点が高く、水の沸点を超えるものも多いので、そのような場合適当な塩水溶液を用いることにより簡易に測定することができる(特開平9−157386号公報参照)。通常、親水性が強いほど曇点は高くなる。また、エステル化率が同じであってもモノエステル含量が多いエステル組成の方がより親水性が高く、曇点も高くなる。 The "cloud point" is a phenomenon in which a hydrated nonionic surfactant is dehydrated at a high temperature and separated from water, and is well known among polyoxyethylene-based surfactants. The cloud point is sensitive to the structure and composition of the polyglycerin fatty acid ester and reflects the effect of the fatty acid soap, so that the difference in the degree of hydrophilicity and the composition can be identified more accurately. Furthermore, since it can be easily measured, it is the most excellent physical property representative of the characteristics of polyglycerin fatty acid ester. Therefore, in polyglycerin fatty acid esters, the cloud point is a more useful index than HLB (balance between hydrophilicity and hydrophobicity). Since polyglycerin has a large number of hydroxyl groups, compared to polyoxyethylene-based surfactants, it generally has a higher cloud point and often exceeds the boiling point of water, so in such cases, use an appropriate salt aqueous solution Thus, the measurement can be easily performed (see Japanese Patent Application Laid-Open No. 9-157386). Usually, the stronger the hydrophilicity, the higher the cloud point. Further, even if the esterification rate is the same, an ester composition having a higher monoester content has higher hydrophilicity and a higher cloud point.
曇点測定法としては、通常、1〜30%の塩化ナトリウム又は硫酸ナトリウム溶液にポリグリセリン脂肪酸エステルを溶解した後、測定する必要があり、その条件は対象となる試料の溶解性により異なるが、本発明の場合の測定法について説明する。本発明の場合、先ず、ポリグリセリン脂肪酸エステルを1重量%となるように20重量%塩化ナトリウム水溶液に分散し、加熱しながら撹拌し、均一な水溶液とする。そして得られたポリグリセリン脂肪酸エステル均一水溶液を、0℃以上100℃以下の任意の温度で2〜5℃刻みに振とう撹拌・静置し、ポリグリセリン脂肪酸エステルが油状あるいはゲル状の如く分離し、不均一水溶液となった状態の温度を「曇点」として測定する。0℃未満では氷の融点以下、100℃を越えると水の沸点以上となるために、正確な水溶液状態の観察が難しく曇点測定が困難となるので好ましくない。 As a cloud point measurement method, it is usually necessary to measure the polyglycerol fatty acid ester after dissolving it in a 1 to 30% sodium chloride or sodium sulfate solution, and the conditions vary depending on the solubility of the target sample. The measuring method in the case of the present invention will be described. In the case of the present invention, first, a polyglycerin fatty acid ester is dispersed in a 20% by weight aqueous sodium chloride solution so as to be 1% by weight, and stirred while heating to obtain a uniform aqueous solution. The obtained homogeneous aqueous solution of polyglycerin fatty acid ester is shaken, stirred and allowed to stand at an arbitrary temperature of 0 ° C. or more and 100 ° C. or less in steps of 2 ° C. to separate the polyglycerin fatty acid ester into an oil or a gel. The temperature in the state of a non-uniform aqueous solution is measured as the “cloud point”. If the temperature is lower than 0 ° C., the temperature is lower than the melting point of ice, and if it is higher than 100 ° C., the temperature is higher than the boiling point of water.
本発明で用いるポリグリセリン脂肪酸エステルの曇点範囲は90℃以上であり、曇点がこの温度より低いと効果が不十分となる。なお、従来、曇点の高いものとして、例えば、親水性銘柄としてデカグリセリンモノステアレート(阪本薬品工業社製MSW−750)が市販されているが、この曇点は約82℃である。従って、これを仮りに乳飲料に配合した場合には、高温長期保存によるオイルオフを完全に抑制することができず、本発明で目標とする乳化剤として十分な機能を発揮することができない。しかし、本発明の曇点90℃以上のものを用いた場合には、UHT殺菌をしても良好な乳化安定性が長期間保持可能である。 The cloud point range of the polyglycerol fatty acid ester used in the present invention is 90 ° C. or higher. If the cloud point is lower than this temperature, the effect becomes insufficient. Conventionally, as a high cloud point, for example, decaglycerin monostearate (MSW-750, manufactured by Sakamoto Yakuhin Kogyo Co., Ltd.) is marketed as a hydrophilic brand, and the cloud point is about 82 ° C. Therefore, if this is blended in a milk drink, oil-off due to long-term storage at high temperature cannot be completely suppressed, and a sufficient function as an emulsifier targeted in the present invention cannot be exhibited. However, when the cloud point of the present invention of 90 ° C. or higher is used, good emulsion stability can be maintained for a long time even after UHT sterilization.
ポリグリセリン脂肪酸エステルは、一般的にはポリグリセリンと脂肪酸をアルカリ触媒存在下に、180〜260℃の温度で反応させることにより得られるが、市場に流通しているポリグリセリン脂肪酸エステルには、ポリグリセリンと脂肪酸の反応仕込み比率によりHLB値の異なる各種の銘柄がある。ポリグリセリンに対して脂肪酸の仕込み比率が大きいと親水性の低い(曇点の低い)銘柄が得られ、逆の場合は親水性の高い(曇点の高い)銘柄が得られる。従って、親水性の高い銘柄を得ようとする場合、脂肪酸に対してポリグリセリンを等モルまたは過剰にする必要がある。しかし、このような仕込み比率であっても、通常のアルカリ触媒による反応では、モノエステル体の多いポリグリセリン脂肪酸エステルを得ることは困難であり、未反応のポリグリセリンとジエステル体以上の高置換度のポリグリセリン脂肪酸エステルを比較的多く含んだものが得られることになる。 Polyglycerin fatty acid ester is generally obtained by reacting polyglycerin and a fatty acid at a temperature of 180 to 260 ° C. in the presence of an alkali catalyst. There are various brands having different HLB values depending on the reaction charge ratio of glycerin and fatty acid. If the ratio of the charged fatty acid to polyglycerin is large, a brand having low hydrophilicity (low cloud point) is obtained, and if the reverse is true, a brand having high hydrophilicity (high cloud point) is obtained. Therefore, in order to obtain a brand with high hydrophilicity, it is necessary to make polyglycerin equimolar or excess with respect to the fatty acid. However, even with such a charging ratio, it is difficult to obtain a polyglycerol fatty acid ester having a large amount of a monoester compound in a reaction with a normal alkali catalyst, and a high degree of substitution of unreacted polyglycerin and a diester compound or more is obtained. Is obtained containing a relatively large amount of polyglycerin fatty acid ester.
本発明の特定曇点のポリグリセリン脂肪酸エステルを得るためには、通常、アルカリ触媒の量を減じ、2段階反応で後半の温度を高める方法、例えば、反応温度180〜260℃でのエステル化反応後に、さらに反応温度を10〜50℃上昇させて1〜4時間反応させる方法を用いることができる(特開平7−145104号公報参照)。従って、特定の曇点を示すポリグリセリン脂肪酸エステルを得るためには、このような特定の反応条件で製造することが望ましい。例えば、前記特許文献2記載の公知の製造法であっても、得られるポリグリセリン脂肪酸エステルの曇点は、たとえ水酸基価が同様であっても全く異なるものとなる。 In order to obtain the polyglycerol fatty acid ester having a specific cloud point of the present invention, a method of reducing the amount of an alkali catalyst and raising the latter half temperature in a two-stage reaction is usually used, for example, an esterification reaction at a reaction temperature of 180 to 260 ° C. Thereafter, a method in which the reaction temperature is further raised by 10 to 50 ° C. and the reaction is carried out for 1 to 4 hours can be used (see JP-A-7-145104). Therefore, in order to obtain a polyglycerol fatty acid ester having a specific cloud point, it is desirable to produce under such specific reaction conditions. For example, even with the known production method described in Patent Document 2, the cloud point of the obtained polyglycerin fatty acid ester is completely different even if the hydroxyl value is the same.
反応させるポリグリセリンが過剰の場合には、未反応のポリグリセリンを製品中に多く含むことになる。未反応のポリグリセリン量が多いほどポリグリセリン脂肪酸エステルの親水性は高くなるが、実質のポリグリセリン脂肪酸エステル量は少なくなるために、乳化剤としての機能が劣る。従って、ポリグリセリン脂肪酸エステル中に残存するポリグリセリンの量は70重量%以下が好ましく、更に好ましくは60重量%以下のものである。 If the amount of polyglycerin to be reacted is excessive, the product will contain a large amount of unreacted polyglycerin. As the amount of unreacted polyglycerin increases, the hydrophilicity of the polyglycerol fatty acid ester increases, but the actual amount of polyglycerin fatty acid ester decreases, so that the function as an emulsifier is inferior. Therefore, the amount of polyglycerin remaining in the polyglycerin fatty acid ester is preferably 70% by weight or less, more preferably 60% by weight or less.
ポリグリセリン脂肪酸エステルを構成する脂肪酸の具体例としては、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘン酸、オレイン酸などの炭素数14〜22の飽和または不飽和の脂肪酸が挙げられるが、炭素数が小さい方が好ましい。中でも、ミリスチン酸、パルミチン酸、ステアリン酸が好ましく、特にミリスチン酸が好ましい。ポリグリセリン脂肪酸エステルを構成するポリグリセリンの重合度としては、平均重合度が4〜20、好ましくは平均重合度が4〜12である。ポリグリセリン脂肪酸エステルの含量は、一般に、乳飲料中0.01〜0.1重量%であり、好ましくは0.025〜0.1重量%である。 Specific examples of the fatty acid constituting the polyglycerin fatty acid ester include a saturated or unsaturated fatty acid having 14 to 22 carbon atoms such as myristic acid, palmitic acid, stearic acid, behenic acid, and oleic acid. A smaller one is preferred. Among them, myristic acid, palmitic acid and stearic acid are preferable, and myristic acid is particularly preferable. The degree of polymerization of the polyglycerol constituting the polyglycerin fatty acid ester is 4-20, preferably 4-12. The content of the polyglycerin fatty acid ester is generally 0.01 to 0.1% by weight, preferably 0.025 to 0.1% by weight in the milk beverage.
本発明における乳飲料には、上記のポリグリセリン脂肪酸エステルの他に、各種の成分を含有することが出来るが、本発明では特に、ショ糖脂肪酸エステルを併用すると乳飲料自体の安定性が一層向上するので好ましい。そのショ糖脂肪酸エステルとしては、通常、モノエステル含量が50%以上であり、構成脂肪酸の70%以上がパルミチン酸またはステアリン酸のもの、特に、モノエステル含量が70%以上であり、構成脂肪酸の80%以上がパルミチン酸であるショ糖脂肪酸エステルが好ましい。これらショ糖脂肪酸エステルの配合は殺菌効果の面からも好ましい。ショ糖脂肪酸エステルの含量は、例えば、0.03〜0.1重量%が好ましく、ポリグリセリン脂肪酸エステルとショ糖脂肪酸エステルの比率は重量比で、1/1〜7/3が好ましい。その他の乳化剤成分としては、レシチン、リゾレシチン、モノグリセライド、有機酸モノグリセライド、ジグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル等が挙げられる。 The milk beverage of the present invention may contain various components in addition to the above-mentioned polyglycerin fatty acid ester. In the present invention, the use of sucrose fatty acid ester in particular further improves the stability of the milk beverage itself. Is preferred. The sucrose fatty acid ester usually has a monoester content of 50% or more, and 70% or more of the constituent fatty acids is palmitic acid or stearic acid, particularly, a monoester content of 70% or more. Sucrose fatty acid esters in which at least 80% is palmitic acid are preferred. Mixing of these sucrose fatty acid esters is also preferable from the viewpoint of the bactericidal effect. The content of the sucrose fatty acid ester is preferably, for example, 0.03 to 0.1% by weight, and the ratio of the polyglycerin fatty acid ester to the sucrose fatty acid ester is preferably 1/1 to 7/3 by weight. Other emulsifier components include lecithin, lysolecithin, monoglyceride, organic acid monoglyceride, diglycerin fatty acid ester, sorbitan fatty acid ester and the like.
本発明の乳飲料の製造方法は、殺菌処理、特に、UHT殺菌を施しても殺菌直後の乳化物の耐熱性が高く、さらに長期間の乳化安定性を保持することができる。通常レトルト殺菌は、121℃、20〜40分の条件で行われるが、PETボトル用飲料などに用いられるUHT殺菌は、より高温、例えば、殺菌温度130〜150℃で、且つ、121℃での殺菌価(Fo)が10〜50に相当する超高温殺菌である。UHT殺菌は飲料に直接水蒸気を吹き込むスチームインジェクション式や飲料を水蒸気中に噴射して加熱するスチームインフュージョン式などの直接加熱方式、プレートやチューブなど表面熱交換器を用いる間接加熱方式など公知の方法で行うことができ、例えばプレート式殺菌装置を用いることができる。 According to the method for producing a milk beverage of the present invention, even when sterilization treatment, in particular, UHT sterilization is performed, the heat resistance of the emulsion immediately after sterilization is high, and the emulsion stability can be maintained for a long period of time. Normally, retort sterilization is performed under the conditions of 121 ° C and 20 to 40 minutes, but UHT sterilization used for PET bottle beverages and the like is performed at a higher temperature, for example, at a sterilization temperature of 130 to 150 ° C and at 121 ° C. It is an ultra-high temperature sterilization having a sterilization value (Fo) of 10 to 50. UHT sterilization is a known method such as a direct heating method such as a steam injection method in which steam is directly blown into a beverage or a steam infusion method in which a beverage is injected into steam and heated, and an indirect heating method using a surface heat exchanger such as a plate or a tube. For example, a plate-type sterilizer can be used.
以下、本発明を実施例により更に具体的に説明するが、本発明は、その要旨を超えない限り、以下の実施例に限定されるものではない。また、比、%および部はいずれも重量比、重量%および重量部を表す。 Hereinafter, the present invention will be described more specifically with reference to examples, but the present invention is not limited to the following examples as long as the gist of the present invention is not exceeded. Further, all ratios, percentages and parts represent weight ratios, weight percentages and parts by weight.
実施例1〜3および比較例1
焙煎コーヒー豆40gを95℃の脱塩水400gで抽出し、コーヒー抽出液を得た。コーヒー抽出液313g、牛乳375g、グラニュー糖84g及び表1記載の乳化剤を全量に対して、0.1%配合し、これに脱塩水を加えて全量を1500gとした。重曹を加えてpHを6.8に調整し、これを高圧ホモジナイザーを用いて60〜70℃の温度で150kg/50kgの圧力で均質化後、プレート式UHT殺菌装置により殺菌温度137℃、殺菌時間(ホールド時間)60秒の条件で殺菌し、無菌状態で30g試験管に採取し冷却することによりミルクコーヒーを得た。次に、得られたミルクコーヒーを40℃で2週間保存し、FormalAction社製、TurbiscanMA2000によりクリームオフ量を測定した。評価結果を表1に示した。
Examples 1 to 3 and Comparative Example 1
40 g of roasted coffee beans were extracted with 400 g of demineralized water at 95 ° C. to obtain a coffee extract. 313 g of coffee extract, 375 g of milk, 84 g of granulated sugar, and 0.1% of the emulsifier shown in Table 1 were blended with respect to the total amount, and desalted water was added thereto to make the total amount to 1500 g. The pH was adjusted to 6.8 by adding baking soda, and the mixture was homogenized using a high-pressure homogenizer at a temperature of 60 to 70 ° C. at a pressure of 150 kg / 50 kg. (Holding time) It was sterilized under the condition of 60 seconds, collected in a 30 g test tube in an aseptic state, and cooled to obtain milk coffee. Next, the obtained milk coffee was stored at 40 ° C. for 2 weeks, and the amount of cream-off was measured using Turbiscan MA2000 manufactured by FormalAction. Table 1 shows the evaluation results.
<TurbiscanMA2000によるクリームオフ量の測定>
光源を一定時間間隔でサンプル管の上下方向にスキャンすることにより、サンプルからの後方散乱光を検出し、測定時間に対して後方散乱光強度の変化率を観測することにより、クリームオフの状態を把握することができる。サンプル管上部の測定により、クリームオフ量の情報が得られる。時間とともに後方散乱光強度の変化率が正に大きくなるほどクリームオフ量が多く、乳化安定性は劣る。そこで、表1における乳化安定性(クリーミング)を次のように評価した。
◎:400分での後方散乱光強度の変化率が3%未満
○:400分での後方散乱光強度の変化率が3%〜4%未満
△:400分での後方散乱光強度の変化率が4%以上
<Measurement of cream-off amount by Turbiscan MA2000>
By scanning the light source up and down the sample tube at regular time intervals, the backscattered light from the sample is detected, and the change rate of the backscattered light intensity with respect to the measurement time is observed. I can figure it out. Measurement of the upper part of the sample tube provides information on the amount of cream off. As the rate of change of the backscattered light intensity increases with time, the cream-off amount increases and the emulsion stability deteriorates. Then, the emulsion stability (creaming) in Table 1 was evaluated as follows.
:: Change rate of backscattered light intensity at 400 minutes is less than 3% ○: Change rate of backscattered light intensity at 400 minutes is less than 3% to less than 4% Δ: Change rate of backscattered light intensity at 400 minutes Is 4% or more
実施例4および比較例2〜3
全脂粉乳49.5g、グラニュー糖90g及び乳化剤として表2に示す曇点を有するデカグリセリンステアリン酸エステルを全量に対して0.05%となるように配合し、これを脱塩水に溶解し、1規定乳酸水溶液によりpHを6.6に調整して全量を1500gとした。これを高圧ホモジナイザーを用いて60〜70℃の温度で150kg/50kgの圧力で均質化後、プレート式UHT殺菌装置により殺菌温度132℃、殺菌時間(ホールド時間)90秒の条件で殺菌し、無菌状態で30g試験管に採取し冷却することにより全脂肪粉乳液を得た。殺菌直後および55℃で2ヶ月間保存した後の全脱脂粉乳液について、メジアン粒径(粒径の出現頻度の合計が50%となる粒径)測定および目視観察を行い、乳化安定性について評価した。なお、粒径測定はHORIBA社製、LA−500を用いた。評価結果を表2にまとめて示した。
Example 4 and Comparative Examples 2-3
49.5 g of whole fat milk powder, 90 g of granulated sugar and decaglycerin stearate having a cloud point shown in Table 2 as an emulsifier were blended so as to be 0.05% based on the total amount, and this was dissolved in deionized water. The pH was adjusted to 6.6 with a 1N aqueous lactic acid solution to make the total amount 1500 g. This was homogenized using a high-pressure homogenizer at a temperature of 60 to 70 ° C. at a pressure of 150 kg / 50 kg, and then sterilized by a plate-type UHT sterilizer under the conditions of a sterilization temperature of 132 ° C. and a sterilization time (hold time) of 90 seconds. In this state, 30 g was collected in a test tube and cooled to obtain a whole fat powder emulsion. Immediately after sterilization and after storage at 55 ° C. for 2 months, the median particle size (particle size at which the total frequency of particle size is 50%) is measured and visually observed to evaluate the emulsion stability. did. The particle size was measured using LA-500 manufactured by HORIBA. The evaluation results are summarized in Table 2.
なお、表2におけるオイルオフの状態は以下のように評価した。
<オイルオフ評価基準>
○:オイルオフがまったく観察されない
△:極僅かなオイルオフが観察される
×:オイルオフにより生じる凝集物が観察される
The oil-off state in Table 2 was evaluated as follows.
<Oil-off evaluation criteria>
:: No oil-off is observed at all △: Very slight oil-off is observed ×: Aggregates generated by oil-off are observed
製造例1
デカグリセリン(平均重合度9.15、平均分子量695、水酸基価900)188g(0.27モル)とミリスチン酸(純度99%、平均分子量228)62g(0.27モル)を加熱ジャケット付き攪拌型反応槽に仕込み、25%水酸化ナトリウム0.025g(対原料合計0.0025%)を加えて、窒素気流下、240℃に昇温して3時間反応させた後、更に260℃で4時間反応させてデカグリセリンミリスチン酸エステル234gを得た。
Production Example 1
188 g (0.27 mol) of decaglycerin (average degree of polymerization 9.15, average molecular weight 695, hydroxyl value 900) and 62 g (0.27 mol) of myristic acid (purity 99%, average molecular weight 228) were stirred with a heating jacket. The reaction vessel was charged, 0.025 g of 25% sodium hydroxide (0.0025% of the total amount of the raw material) was added, and the temperature was raised to 240 ° C. in a nitrogen stream, followed by a reaction for 3 hours, and further at 260 ° C. for 4 hours. The reaction was performed to obtain 234 g of decaglycerin myristate.
製造例2
デカグリセリン(平均重合度9.15、平均分子量695、水酸基価900)183g(0.26モル)とパルミチン酸(純度96%、平均分子量257)67g(0.25モル)を用い、製造例1と同様に反応を行い、デカグリセリンパルミチン酸エステル229gを得た。
Production Example 2
Production Example 1 using 183 g (0.26 mol) of decaglycerin (average degree of polymerization 9.15, average molecular weight 695, hydroxyl value 900) and 67 g (0.25 mol) of palmitic acid (purity 96%, average molecular weight 257). The reaction was carried out in the same manner as described above to obtain 229 g of decaglycerin palmitic acid ester.
実施例5〜8および比較例4
紅茶葉(ティンブラ茶)100gを80℃の脱塩水1000gで抽出し、紅茶抽出液を得た。続いて、紅茶抽出液250g、牛乳500g、砂糖150gを混合し、続いて表3記載の乳化剤2.5gを脱塩水497.5gに溶解した乳化剤水溶液500gを加え、さらに脱塩水を加えて全量を2500gとした。これを高圧ホモジナイザーを用いて60〜70℃の温度で150kg/50kgcm-2の圧力で均質化後、プレート式UHT殺菌装置により殺菌温度137℃、殺菌時間(ホールド時間)60秒の条件で殺菌し、無菌状態で殺菌済みの500mLPETボトルに充填し、冷却することによりミルク紅茶を得た。殺菌直後および40℃で2ヶ月間保存した後のミルク紅茶について、メジアン粒径(粒径の出現頻度の合計が50%となる粒径)測定を行った。また、40℃で2ヶ月間保存した後のミルク紅茶について、FormalAction社製、TurbiS can MA2000によるクリームオフ量測定を行った。さらに、PETボトルの目視観察により、40℃で2週間保存後および2ヶ月保存後の、クリームの再分散性、オイルオフについて評価した。評価結果を表3にまとめて示した。
Examples 5 to 8 and Comparative Example 4
100 g of black tea leaves (Timbra tea) were extracted with 1000 g of demineralized water at 80 ° C. to obtain a black tea extract. Subsequently, 250 g of black tea extract, 500 g of milk, and 150 g of sugar were mixed, and subsequently, 500 g of an emulsifier aqueous solution obtained by dissolving 2.5 g of the emulsifier shown in Table 3 in 497.5 g of demineralized water was added. 2500 g. This was homogenized using a high-pressure homogenizer at a temperature of 60 to 70 ° C. at a pressure of 150 kg / 50 kg cm −2 , and then sterilized by a plate-type UHT sterilizer at a sterilizing temperature of 137 ° C. and a sterilizing time (hold time) of 60 seconds. Then, it was filled into a sterilized 500 mL PET bottle and cooled to obtain milk black tea. For the black tea immediately after sterilization and after storage at 40 ° C. for 2 months, the median particle size (particle size at which the total appearance frequency of the particle size becomes 50%) was measured. The cream-off amount of milk tea after storage at 40 ° C. for 2 months was measured by TurbiScan MA2000 manufactured by FormalAction. Further, the redispersibility of the cream and the oil-off after storage at 40 ° C. for 2 weeks and after storage for 2 months were evaluated by visual observation of the PET bottle. Table 3 summarizes the evaluation results.
なお、表3におけるクリームオフ量、クリーム再分散性、オイルオフは以下のように評価した。
<クリームオフ量評価基準>
◎:600分での後方散乱光強度の変化率が3%未満
○:600分での後方散乱光強度の変化率が3%〜4%未満
△:600分での後方散乱光強度の変化率が4%〜5%未満
×;600分での後方散乱光強度の変化率が5%以上
<クリーム再分散性評価基準>
◎:軽く揺らしただけで分散する
○:暫く揺らすと分散する
△:クリームが壁面に付着し分散しにくい
×:クリームが塊が浮遊する
<オイルオフ評価基準>
○:オイルオフが観察されない
△:少量のオイルオフが観察される
×:多量のオイルオフが観察される
××:オイルオフにより生じる凝集物が観察される
The cream-off amount, cream redispersibility, and oil-off in Table 3 were evaluated as follows.
<Cream off amount evaluation criteria>
:: Change rate of backscattered light intensity at 600 minutes is less than 3% :: Change rate of backscattered light intensity at 600 minutes is 3% to less than 4% Δ: Change rate of backscattered light intensity at 600 minutes : Less than 4% to 5% ×; change rate of backscattered light intensity at 600 minutes is 5% or more <Cream redispersibility evaluation criteria>
◎: Dispersed only by slightly shaking ○: Dispersed when shaked for a while △: Cream adhered to the wall surface and hardly dispersed ×: Cream lump floating <Oil-off evaluation criteria>
:: No oil-off is observed Δ: A small amount of oil-off is observed X: A large amount of oil-off is observed XX: Aggregates generated by oil-off are observed
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