CN104135871A - 用于生产包含具有皂树皂苷的纳米乳的澄清饮料的组合物和方法 - Google Patents
用于生产包含具有皂树皂苷的纳米乳的澄清饮料的组合物和方法 Download PDFInfo
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- CN104135871A CN104135871A CN201380010948.9A CN201380010948A CN104135871A CN 104135871 A CN104135871 A CN 104135871A CN 201380010948 A CN201380010948 A CN 201380010948A CN 104135871 A CN104135871 A CN 104135871A
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/38—Other non-alcoholic beverages
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L2/52—Adding ingredients
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A—HUMAN NECESSITIES
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/68—Acidifying substances
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
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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
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
制备澄清饮料浓缩物的方法,其包含液体香料油在水相中的纳米乳,该方法包括在乳化剂的存在下将香料油乳化到水中,所述乳化剂由至少5%重量的皂树皂苷组成,任选地包含至少一种其他的乳化剂;其特征在于在乳化前,将水相的pH调整至4.0的最大值。该方法使得能够制备这样的饮料,其不仅是透明似水晶的,而且还基本上具有原始香料油的更饱满的香味。
Description
本说明书涉及澄清饮料及其制备方法。
澄清饮料、特别是具有水果香味的那些饮料需要香料为纳米乳的形式,即粒度小到不产生可辨别浊度的乳剂。这种乳剂的粒度小于可见光的波长,即具有约150nm、理想地小于100nm的最大直径。
自然需要乳化剂制备这种乳剂,并且如果产品是可消费的,则它们必须服从涉及这种产品的政府规章。因此,希望使用天然的乳化剂。这种类型的一些传统的乳化剂包括阿拉伯树胶、印度树胶、黄蓍树胶、胡芦巴树胶、豆胶树树胶和甜菜果胶。这些能够达到约200nm的最小粒度。因此,使用基于树胶的乳剂制备的饮料具有约200-400NTU(即比浊法浊度单位,众所周知并且广泛应用于本领域的且例如用Hach2100N浊度计(获自Hach Company)、按照指令使用该仪器测定的浊度单位)的浊度。在这种水平上,一些浊度仍然是可以觉察的,并且使用这种方法未得到或无法得到“透明似水晶的”期望之物。
最近,已经发现并且例如在日本公布的申请2010-142205中公开了一些皂树提取物可以有助于提供可以产生纳米乳和澄清饮料的乳化剂。皂树提取物是获自美洲土生土长的皂树(Quillaja)种类(皂皮树科(Quillajaceae))的许多树的提取物。一种这样的树是皂树(Quillajasaponaria Molina),其天然产于智利。提取物是商购的且是皂苷的丰富来源(典型的提取物包含约14%重量的皂苷)。已知这些提取物是许多应用中的天然起泡剂,包括食品和饮料(例如,参见San Martín andBriones in J.Sci.Food Agric 80:2063-2068(2000))。它们通常以与其他更廉价的皂苷来源的混合物的形式销售,例如西地格丝兰(Yucca schidigera)和肥皂草(Saponaria officinalis)。皂树皂苷也作为干燥提取物商购,即皂苷含量为50%或以上的水溶性固体粉末。
可以理解已经对皂树皂苷与其他材料组合作为乳化剂产生了相当的关注。例如,上述举出的日本公开号2010-142205描述了皂树提取物与聚氧化乙烯失水山梨糖醇脂肪酸酯的组合的应用。其他实例是PCT公布的申请WO2011/089249,其描述了皂树皂苷+大比例的卵磷脂作为乳化剂在澄清饮料中的应用,且EP2359702描述了皂树皂苷与聚合物乳化剂组合在乳化固体、微溶于水的多酚、类黄酮和二萜葡糖苷类中的应用。
目前令人意外地发现,能够更有效地提供透明似水晶的用液体香料油加香的饮料,而无需另外的乳化剂。本说明书由此提供了制备澄清饮料浓缩物的方法,其包含液体香料油在水相中的纳米乳,所述方法包括在乳化剂的存在下将香料油乳化到水中,所述乳化剂由至少5%重量的皂树皂苷组成,任选地包含至少一种其他的乳化剂,其特征在于在乳化前,将水相的pH调整至4.0的最大值。
该方法的应用能够维持香味特性的完全可靠性。这是因为该方法可以与原始香料一起使用,与本领域常用的“洗涤过的”香料相反。所谓“洗涤过的香料”是指来自大部分乃至全部水不溶性物质(例如单萜类)的香味已经被除去。尽管这种“洗涤”保持了基本的香味,但是它缺乏许多其他原始的属性,例如原始的“果皮香”、体香、饱满、圆和的香质。本说明书的香料浓缩物保持了全部这些特性且由此提供了更真实的香味。
乳化剂由至少5%重量的皂树皂苷组成。它们作为提取物商购,例如来自National Starch的Q-NaturaleTM范围的产品,这种提取物典型地包含14%重量的皂苷。尽管能够分离皂树皂苷,但是它是昂贵的,且实际上更通常地使用提取物自身,对所用的提取物的量进行选择以提供期望比例的皂树皂苷。
在具体的实施方案中,乳化剂由25、50、75和100%的皂树皂苷组成。
在那些使用其他乳化剂的情况中,这些其他乳化剂以占总乳化剂最大重量95%的程度存在。然而,正如上述所解释的,它们可以选自那些已知的并且为本领域使用的乳化剂。这些其他乳化剂的非限制性实例包括聚山梨醇酯类、蔗糖酯类和脂肪酸和卵磷脂的聚甘油酯类。可以使用一种以上这种非皂树的乳化剂。
皂树皂苷(和由此的提取物)的必需的比例根据应用与应用的不同而改变,且本领域技术人员易于仅使用简单实验就能够确定适合的用量。作为一般指定原则,皂树皂苷与香料基质的重量比约为0.1-3.0。尽管添加超出这一比例的皂苷没有效果(例如高于3,皂苷的苦味可能变得显著),但是可能存在特定的系统并且应用,其中超出这一范围的比例可能是有用的,且尽管最佳结果一般使用该范围内的比例得到,但是不应将它们视为绝对的限制。
在乳化前进行的pH调整可以通过添加酸实现。所用的酸可以是任意经批准的食用酸,即其用于食品和饮料的用途是经官方批准的任意酸。因此,不仅能够使用常用的有机酸,例如柠檬酸、苹果酸、乙酸和乳酸,而且作为在一些可乐型饮料中使用的,可以使用例如磷酸这样的无机酸。
在典型的非限制性实例中,向调整至适当pH的饮料基质(典型地为水、蔗糖或其他甜味剂、柠檬酸和防腐剂、有时是维生素和其他成分)中添加本说明书的香料浓缩物,其包含5%重量的皂树提取物,该提取物包含14%的皂苷(即在浓缩物中有0.7%的皂苷)与3%的橙香料基质,这种添加得到了澄清的橙饮料,其具有小于10NTU的浊度,即为透明的。增加皂树提取物至7.5%仅轻微地并且是以裸眼几乎不能感觉到的方式改善了NTU值。
为了生产浓缩物,必需对香味材料、水和皂树提取物的掺合物进行高剪切掺合,使得得到期望的纳米乳粒度。这一结果通过高压均化实现。这是一种众所周知的且本领域常用的技术,并且设备易于得到。在一个具体的实施方案中,对香味材料、水和提取物的掺合物首先进行高剪切预均化步骤,然后使其充分通过高剪切均化器,以得到期望的结果。预均化可以典型地使用转子-定子混合器或韦林搅切器进行。得到的浓缩物典型地具有1-10%、特别是2-5%重量的香味材料。
不能在单一均化步骤中使用标准乳化设备生产期望粒度的纳米乳,且始终必需进行几次均化,或在本领域的措辞中,使其“通过(pass)”一次以上。为了商业化目的,通过次数越少,则越好,且大量的通过次数是完全不可接受的。已经发现对上述方法的一些改变可以显著地减少通过的次数。在一些情况中,仅需通过3次就可以生产澄清的纳米乳。
在第一种变型中,可以向浓缩物中加入至少一种单糖或二糖。典型实例包括葡萄糖、果糖和蔗糖。由WO2008/039564已知,蔗糖用于与蔗糖单酯类组合,但令人意外地这种单独使用的糖应对皂树提取物具有某些影响。添加这种糖(其可以是单一的糖或两种或多种这样的糖的混合物)能够使用减少的通过次数得到期望的纳米乳大小。典型地以10-50wt%纳米乳的浓度添加所述的糖。
在第二种变型中,可以向浓缩物中加入一些溶剂。它们选自丙二醇(PG)和甘油。这些是众所周知的饮料溶剂,而再次令人意外的是,其应用具有减少通过次数这样的效果。可以典型地以10-95%纳米乳的浓度使用它们。
在一个具体的实施方案中,PG、甘油和蔗糖的至少两种的组合产生了特别有益的效果。能够使用PG-蔗糖、甘油-蔗糖、PG-甘油和所有它们三种的混合物。典型实例为10%-25%的PG-甘油。另一个具体实例为40-24-27和10-25-35的PG-甘油-蔗糖。
在第三种变型中,用能够应用较高压力(超过100MPa且至多几百MPa)的均化设备替代具有至多50MPa的典型压力的标准均化设备。这种设备是众所周知的,而一般不应用于饮料香料工业,因为高压不被视为是必需或有用的─实际上在一些情况中,它们可能存在缺点(它们可能损害阿拉伯树胶或改性淀粉)。这种设备的实例包括MicrofluidizerTM(Microfluidics Corp.)和EmulsiFlexTM(Avestin)。
由此提供了加香的澄清饮料浓缩物,其可以通过如上所述的方法制备。
通过掺合由此制备的浓缩物与澄清饮料基质制备澄清饮料,所述澄清饮料基质即以公认比例包含除所述浓缩物以外的任意本领域公知的标准成分的组合物。典型地,消费品中的香料浓度可以占消费品重量的0.0005-0.05%,特别是0.001-0.02%。终产品是具有饱满香味的完全透明的消费品。
在另一个实施方案中,可以将上述浓缩物转化成固体形式。在这种形式中,它是贮存稳定的且可以用于生产澄清消费品,简单地通过将其溶于水或以本领域公认比例包含任意本领域已知的标准成分的消费品基质来进行。可以通过向浓缩物中添加载体水溶液且然后喷雾干燥得到的混合物进行该方法。产物是非粘性的粉末,其可以以这种形式使用,或如果需要,将其与其他本领域公认成分一起混合成片剂形式。溶解固体形式得到有饱满香味的完全透明的消费品。
载体是喷雾干燥领域众所周知的,但并非都适用于与这种系统相关的应用。已经发现高MW阿拉伯树胶是特别适合的。
本说明书由此进一步提供了固体形式的澄清饮料产品浓缩物,其可以通过取如上所述的浓缩物并且将其如上所述进行加工来制备。
该方法进一步参照下列非限制性实施例描述。
对比例1
通过掺合去离子水、丙二醇、甘油和糖浆至均匀来制备具有表1中所示组成的纳米乳(对比例1)。加入皂树提取物,再次将该掺合物搅拌至均匀。在使用安装分配聚集物的PT-DA 3030-6060的PolytronPT6100系统进行高剪切条件下,将橙香料基质添加到水相中。以18000rpm持续高剪切掺合5分钟。使得到的粗乳剂通过APV60高剪切均化器以400/50巴(5600/700psi)加工3次。用Zetasizer HAS(Malvern Instruments)、按照指令使用该设备测定流体动力学直径。给出的数值是3次测量的平均值。
乳剂的pH:4.8
3次均化通过后的流体动力学直径:134nm
表1
成分名称 | 对比例1 |
g/kg | |
去离子水 | 27.5 |
丙二醇 | 150.0 |
甘油99.5% | 200.0 |
皂树提取物* | 50.0 |
糖浆65Brix | 538.5 |
橙香料基质** | 34.0 |
*Q-NaturaleTM 200(National Starch Food Innovation)
**产品代码96584505(Givaudan)
实施例1-4
根据对对比例1所述的方法制备纳米乳,区别仅在于首先将表2中给出的柠檬酸的量溶于去离子水,然后加入溶剂和糖浆。从对比例1中给出的水量中扣除加入的酸量。pH值和流体动力学直径如表2中所示。全部流体直径均显著地低于均化前不加入酸的对比例1中相应的值。pH越低,则纳米乳滴的尺寸越小。
表2
实施例 | 加入的柠檬酸的量(g/kg乳剂) | pH | 流体直径(nm) |
1 | 1.65 | 3.8 | 111 |
2 | 4.00 | 3.2 | 109 |
3 | 6.34 | 2.9 | 105 |
4 | 12.00 | 2.6 | 100 |
实施例5-12
根据对对比例1所述的方法制备纳米乳,区别仅在于首先将表3中给出的有机酸的量溶于去离子水,然后加入溶剂和糖浆。从对比例1中给出的水量中扣除加入的酸量。pH值和流体动力学直径如表3中所示。全部流体动力学直径均显著地低于均化前不加入酸的对比例1中相应的值。酸越强,则达到特定pH所需加入的酸的量越少。
表3
实施例 | 所用的酸 | 加入的酸的量(g/kg乳剂) | pH | 流体动力学直径(nm) |
5 | 抗坏血酸 | 12.00 | 3.6 | 110 |
6 | 酒石酸 | 1.65 | 3.4 | 112 |
7 | 酒石酸 | 4.00 | 2.9 | 105 |
8 | 酒石酸 | 6.34 | 2.7 | 103 |
9 | 苹果酸 | 1.65 | 3.6 | 119 |
10 | 苹果酸 | 4.00 | 3.2 | 110 |
11 | 苹果酸 | 8.00 | 3.0 | 103 |
12 | 苹果酸 | 12.00 | 2.8 | 100 |
实施例13
根据对对比例1所述的方法制备纳米乳,区别仅在于首先将表4中给出的磷酸的量溶于去离子水,然后加入溶剂和糖浆。从对比例1中给出的水量中扣除加入的酸量。pH值和3次通过高压均化后的流体动力学直径如表4中所示。流体动力学直径显著地低于均化前不加入酸的对比例1中相应的值。
表4
实施例 | 加入的酸的量(g/kg乳剂) | pH | 流体动力学直径(nm) |
13 | 1.5 | 3.0 | 110 |
对比例2-3和实施例14-16
使用不同的橙和柠檬香料基质制备与上述那些相当的纳米乳。表5展示了香料基质、加入的柠檬酸的量和3次均化通过后的流体动力学直径。
表5
实施例 | 香料基质 | 加入的酸的量(g/kg乳剂) | 流体动力学直径(nm) |
CE2 | 橙* | 142 | |
14 | 橙* | 3.00(+1.50苯甲酸钠) | 117 |
15 | 橙* | 1.65 | 118 |
CE3 | 柠檬** | 148 | |
16 | 柠檬** | 1.65 | 122 |
*产品代码96584506(Givaudan)
**产品代码96584510(Givaudan)
对比例4和实施例17(与实施例1相同)
根据对对比例1所述的方法制备纳米乳(对比例4)。然而,改变水、溶剂和皂树提取物的量以便能够将另外的乳化剂(阿拉伯树胶)溶于水相,然后均化。根据EP2359702中公开的实施例选择皂树提取物与阿拉伯树胶之比,以便显示与如EP2359702中乳化聚合物的组合不会起到实现足够低直径的作用。为了对比,对比例4和实施例1的组成与1、2和3次通过高压均化器后测定的流体动力学直径如表6中所示。皂树提取物与阿拉伯树胶的组合导致液滴直径显著地大于对比例1(不加酸)和甚至在柠檬酸存在下的实施例1(加入酸)中相应的值。还发现在2次通过高压均化后,流体动力学直径没有进一步减小。
表6
*阿拉伯树胶Instant AA(CNI)
**Q-NaturaleTM 200(National Starch Food Innovation)
***产品代码96584505(Givaudan)
Claims (8)
1.制备澄清饮料的方法,该澄清饮料包含液体香料油在水相中的纳米乳,该方法包括在乳化剂的存在下将香料油乳化到水中,所述乳化剂由至少5%重量的皂树皂苷组成,任选地包含至少一种其他的乳化剂,其特征在于,在乳化前,将水相的pH调整至4.0的最大值。
2.权利要求1的方法,其中通过添加经批准的食用酸调整pH。
3.权利要求1的方法,其中皂树皂苷在乳化剂中的比例选自25、50、75和100%。
4.香味澄清饮料浓缩物,可通过权利要求1的方法制备。
5.制备固体形式的澄清饮料浓缩物的方法,包括将载体添加到权利要求1的浓缩物中并且喷雾干燥,所述载体包含分子量大于100kDa的阿拉伯树胶。
6.固体形式的澄清饮料浓缩物,可通过权利要求5的方法制备。
7.澄清饮料,包含澄清饮料基质和权利要求4的澄清饮料浓缩物。
8.澄清饮料,包含澄清饮料基质和溶解的权利要求6的固体形式的澄清饮料浓缩物。
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JP6472245B2 (ja) | 2019-02-20 |
US20150030748A1 (en) | 2015-01-29 |
EP2825060A1 (en) | 2015-01-21 |
JP2015509731A (ja) | 2015-04-02 |
SG11201404534TA (en) | 2014-09-26 |
US11666079B2 (en) | 2023-06-06 |
KR20140138159A (ko) | 2014-12-03 |
BR112014020967B1 (pt) | 2020-07-28 |
WO2013135759A1 (en) | 2013-09-19 |
EP2825060B1 (en) | 2017-12-27 |
KR102187394B1 (ko) | 2020-12-07 |
CN104135871B (zh) | 2018-01-02 |
KR20200005750A (ko) | 2020-01-16 |
GB201204377D0 (en) | 2012-04-25 |
ES2663000T3 (es) | 2018-04-10 |
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