CN107105694A - 亚稳、半透明香料纳米乳液和制备其的方法 - Google Patents
亚稳、半透明香料纳米乳液和制备其的方法 Download PDFInfo
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- CN107105694A CN107105694A CN201580067910.4A CN201580067910A CN107105694A CN 107105694 A CN107105694 A CN 107105694A CN 201580067910 A CN201580067910 A CN 201580067910A CN 107105694 A CN107105694 A CN 107105694A
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- lecithin
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- perfumery
- nano emulsion
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Abstract
提供了一种亚稳、半透明香料纳米乳液。纳米乳液含有香料油相、水性相、以及含有第一卵磷脂和第二卵磷脂的表面活性剂体系。纳米乳液不含任何非天然表面活性剂。表面活性剂体系含有15％以下的游离脂肪酸。第一卵磷脂具有1至8的HLB，并且第二卵磷脂具有8至16的HLB并且含有20％以上的磷脂酰胆碱和溶血磷脂酰胆碱。还公开了一种用于制备纳米乳液的方法以及纳米乳液在液体饮料和液体饮料浓缩物中的用途。
Description
相关申请的交叉引用
本申请要求两个美国申请序列号的优先权的权益：(i)2014年10月20日提交的62/065,865和(ii)2015年7月28日提交的62/197,919。两个申请的内容通过整体引用结合。
背景
在饮料制备中的许多调味化合物是精油如橙、柠檬、和葡萄柚或具有有限的水溶解度的相对非极性的混合物。
为了产生含有香料油的光学澄清或透明的饮料，使用水和非水性助溶剂如丙二醇、甘油、或乙醇制备纳米乳液(在直径为0.1至500纳米的平均粒度范围内)。这些纳米乳液需要是视觉上半透明的并且还是亚稳的，以使得由它们制备的饮料是澄清的并且在其中容纳的油相不与水性相分离。
以下专利和申请描述了含有微乳液或纳米乳液的食品组合物：WO 2007/026271、JP 2006-249037、US 2010/0136175、US 6,902,756、US 2013/0004621、US 2009/0285952、US 6,716,473、和US 2007/0087104。
通常使用合成的、非天然表面活性剂制备稳定纳米乳液。当前，消费者需求仅含有天然产品的饮料。
需要仅使用天然表面活性剂制造用于液体饮料浓缩物和即饮饮料的调味纳米乳液。
概述
本发明基于某些仅含有天然表面活性剂如卵磷脂的纳米乳液出乎意料地显示出稳定、半透明、且适用于制备澄清饮料。
因此，本发明的一个方面涉及亚稳、半透明香料纳米乳液，其含有香料油相、水性相、以及具有第一卵磷脂和第二卵磷脂的表面活性剂体系。纳米乳液不含任何非天然表面活性剂。表面活性剂体系含有以表面活性剂体系的重量计15％以下(例如，10％以下和5％以下)的游离脂肪酸。第一卵磷脂具有1至8的亲水-亲脂平衡(“HLB”)，并且第二卵磷脂具有8至16的HLB并且含有20％以上(例如，30％以上、20％至90％、和30％至90％)的磷脂酰胆碱和溶血磷脂酰胆碱。
纳米乳液通常含有以纳米乳液的重量计0.1％至10％的表面活性剂体系和1％至20％的香料油。表面活性剂体系和香料油之间的比率可以是1∶10至2∶1(优选1∶5至1∶1)。
在表面活性剂体系中，第一和第二卵磷脂中的每一种可以是天然的、脱油的、分馏的、或酶改性的，并且选自由下列各项组成的组：大豆卵磷脂、蛋黄卵磷脂、葵花卵磷脂、油菜籽卵磷脂、和它们的组合。在一些实施方案中，第一卵磷脂是酶改性的卵磷脂，并且第二卵磷脂是含有15％以上的溶血磷脂酰胆碱的脱油的、分馏的、和酶改性的卵磷脂。在第一和第二卵磷脂二者中存在磷脂酰胆碱。在表面活性剂体系中，磷脂酰胆碱和溶血磷脂酰胆碱可以以4∶1至1∶5(优选1∶1至1∶4)的重量比存在。
在一些实施方案中，表面活性剂体系还含有第三卵磷脂。第一、第二、和第三卵磷脂之间的重量比是1∶20∶2至1∶5∶1。在某些实施方案中，香料油相含有油溶性维生素、油溶性着色剂、抗氧化剂、或它们的组合。
纳米乳液还可以含有在水性相中的助溶剂如多元醇。其还可以含有单糖、二糖、水胶体、或它们的组合。多元醇的实例包括丙二醇、1，3-丙二醇、甘油、丁二醇、赤藓糖醇、木糖醇、甘露糖醇、山梨糖醇、异麦芽酮糖醇(isomalt)、和它们的组合；适合的单糖包括葡萄糖、果糖、和它们的组合；二糖可以是蔗糖、麦芽糖、或它们的组合；并且水胶体的实例包括黄原胶、瓜尔胶、阿拉伯胶、化学改性阿拉伯胶、果胶、和它们的组合。
在一些实施方案中，助溶剂是丙二醇、甘油和山梨糖醇的混合物。在其他实施方案中，丙二醇以5至25％的水平存在，甘油以0.1至35％的水平存在，并且山梨糖醇以25至65％的水平存在，全部以纳米乳液的重量计。水和助溶剂之间的重量比是1∶95至1∶3，优选1∶40至1∶4，并且更优选1∶20至1∶5。
本发明的另一个方面涉及含有任何上述纳米乳液的液体饮料或液体饮料浓缩物。
也在本发明的范围内的是用于制备亚稳、半透明香料纳米乳液的方法。所述方法包括在表面活性剂体系的存在下将香料油乳化至水性相中的步骤，其中表面活性剂体系含有第一卵磷脂和第二卵磷脂。纳米乳液不含任何非天然表面活性剂，第一卵磷脂具有1至8的HLB，并且第二卵磷脂具有8至16的HLB并且含有以第二卵磷脂的重量计20％以上的磷脂酰胆碱和溶血磷脂酰胆碱。
本发明的一个或多个实施方案的细节在以下描述中给出。根据说明书和权利要求，本发明的其他特征、目标、和优点将会是显而易见的。
详细描述
已经出人意料地发现，可以通过磷脂系表面活性剂体系在不存在合成或非天然助表面活性剂(例如，脂肪酸的糖酯和聚甘油脂肪酸酯，其二者由糖或聚甘油与脂肪酸合成)的情况下制备由油和水组成的亚稳、半透明香料纳米乳液。除了提供优秀的水分散性，根据本发明制备的香料纳米乳液组合物提供高产品收率(例如，90％以上和95％以上)和可以与当前商业纳米乳液香料体系相比的影响感官的香料性能。此外，如在本文中的实例中说明的，在常规蔗糖单棕榈酸酯系乳液和本发明的卵磷脂系纳米乳液之间，感官性能数据未显示出显著性差异。注意，蔗糖单棕榈酸酯是用于使酸性饮料稳定的合成表面活性剂。参见Choi等人，Food Research International，44(9)，3006-12(2011)。
因此，本发明的亚稳、半透明香料纳米乳液不含任何非天然表面活性剂并且包含香料油相、水性相、和表面活性剂体系。表面活性剂体系含有第一卵磷脂和第二卵磷脂，其二者均为天然磷脂。
天然产品或表面活性剂是指自然存在的并且来自自然来源的产品。天然产品/表面活性剂包括它们的衍生物，所述衍生物可以是加盐的、脱盐的、脱油的、分馏的、或使用天然酶或微生物改性的。另一方面，非天然表面活性剂是通过不包括酶改性的化学过程化学合成的表面活性剂。
为了本发明的目的，稳定性被定义为保持对于在最终用途中使用来说可接受的香味品质和强度。优选地，亚稳组合物在室温下在玻璃或塑料容器中具有至少1年至三年的保存限期。
半透明纳米乳液是指通透可见的纳米乳液，尽管光可能会被材料本身漫射。就此而言，本发明的纳米乳液提供澄清的软饮料。术语半透明是指具有小于800比浊测量法浊度单位(Nephelometric Turbidity Unit，“NTU”；例如，小于200NTU和小于100NTU)的浊度的纳米乳液。术语澄清是指具有小于10NTU(例如，5NTU以下和3NTU以下)的浊度的物质。浊度可以按照在本领域内公知的工序测量，例如Fernandez等人，Food Chemistry(2000)，71，563-66；和Christensen等人，Journal-American Water Works Association(2003)，95，179-189。
纳米乳液指的是直径尺寸为200纳米以下(例如，20至150纳米)的脂质液滴。参见Mason等人，2006，J.Physics：Condensed Matter 18，635-66。纳米乳液通过利用高应力机械工艺将水不可溶混油相混合至水性相中来制备。
适用于制备本发明的纳米乳液的香料油含有一种或多种挥发性化合物。可以根据本发明使用各种香料。香料可以选自合成香料、调味油以及来源于植物、叶、花、果实、以及它们的组合的油提取物。代表性的香料油包括，但不限于留兰香油、肉桂油、薄荷油、丁香油、月桂油、百里香油、雪松叶油、肉豆蔻油、鼠尾草油、和苦杏仁油。还可用的是人工、自然或合成水果香料如香草、巧克力、咖啡、可可和柑橘属油(包括柠檬、橙、葡萄、酸橙和葡萄柚)、和水果香精(包括苹果、梨、桃、草莓、西瓜、树莓、樱桃、李子、菠萝、杏等)。这些香料可以单独或混合使用。
在香料油中的挥发性化合物可以包括，但不限于乙醛、二甲基硫醚、乙酸乙酯、丙酸乙酯、丁酸甲酯、和丁酸乙酯。含有挥发性醛或酯的香料包括，例如，乙酸肉桂基酯、肉桂醛、柠檬醛、二乙缩醛、乙酸二氢香芹酯、甲酸丁香酚酯、和对甲基苯甲醚。可以在本香料油中存在的挥发性化合物的另外的实例包括乙醛(苹果)；苯甲醛(樱桃、杏仁)；肉桂醛(肉桂)；柠檬醛，即α柠檬醛(柠檬、酸橙)；橙花醛，即β柠檬醛(柠檬、酸橙)；癸醛(橙、柠檬)；乙基香兰素(香草、奶油)；洋茉莉醛，即胡椒醛(香草、奶油)；香兰素(香草、奶油)；α-戊基肉桂醛(香辛水果香料)；丁醛(黄油、奶酪)；戊醛(黄油、奶酪)；香茅醛(改性剂，多种类型)；癸醛(柑橘属水果)；醛C-8(柑橘属水果)；醛C-9(柑橘属水果)；醛C-12(柑橘属水果)；2-乙基丁醛(浆果)；己醛，即反式-2(浆果)；甲苯基醛(樱桃、杏仁)；藜芦醛(香草)；2，6-二甲基-5-庚醛，即甜瓜醛(甜瓜)；2-6-二甲基辛醛(绿色水果)；和2-十二醛(柑橘属，桔)；樱桃；或葡萄以及它们的混合物。组合物还可以含有味道调节剂和人造增甜剂。
所选择的挥发性化合物的物理、化学、和气味性质在表1中给出。
表1
*Good Scents Company和默克索引(Merck Index)第12版
通常，本发明的香料纳米乳液含有20％以下的香料油。在某些实施方案中，香料纳米乳液含有0.1％至10％之间的香料油。在其他实施方案中，香料纳米乳液含有1％至5％之间的香料油。
除了香料油之外，香料纳米乳液还包含由第一卵磷脂和第二卵磷脂组成的表面活性剂体系。在一些实施方案中，包含可以具有1至16的HLB的第三卵磷脂。通常，在不存在任何非天然助表面活性剂(例如，脂肪酸的糖酯、甘油脂肪酸酯、聚甘油脂肪酸酯、聚山梨糖醇酯、或短链醇)的情况下使用卵磷脂。卵磷脂可以是脱油的(即，具有3％以下的残油)，分馏的(即，分离溶剂(可以为醇如乙醇或乙醇-水混合物)中的可溶性组分和不溶性组分)，或酶改性的(即磷脂的酶水解，得到磷脂分子的较高极性，从而提高卵磷脂的水溶解度)。在某些实施方案中，第一卵磷脂是天然卵磷脂(例如，标准流体卵磷脂)，其未脱油和酶改性。在其他实施方案中，第一卵磷脂是酶改性的卵磷脂。其还可以是分馏的和/或脱油的。第一卵磷脂具有在1至8的范围内、优选在4至8的范围内的HLB值。第二卵磷脂可以是脱油的、分馏的、和/或酶改性的，并且具有在8至16、优选12至15的范围内的HLB值。第一和第二卵磷脂的重量比可以是1∶30至10∶1(优选1∶20至5∶1；更优选1∶10至1∶1；并且甚至更优选、1∶10至1∶3.5)。在表面活性剂体系中的游离脂肪酸的总量被控制在15％以下的水平。在不受任何理论约束的情况下，游离脂肪酸降低亚稳、半透明香料纳米乳液和最终饮料产品的澄清度。
如在本文中所使用的术语“HLB”是指分子的“亲水-亲脂平衡”。HLB数字表示在1-40的范围内的分子的极性，并且最常用的乳化剂具有1至20之间的值。在增加亲水性的情况下，HLB数字增加。如由Griffin，“借助‘HLB’的表面-活性剂的分类(Classification ofSurface-Active Agents by′HLB′)”，Journal of the Society of Cosmetic Chemists 1(1949)，311-26；和Griffin，“非离子表面活性剂的HLB值的计算”，Journal of theSociety of Cosmetic Chemists 5(1954)，249-56描述的，可以通过对分子的不同区域计算数值来确定表面活性剂的HLB。
术语“游离脂肪酸”是指含有游离羧基(-COOH)的脂肪酸。游离脂肪酸包括它们的盐和溶剂化物。
当使用第三卵磷脂时，第一、第二、和第三卵磷脂之间的重量比可以是1∶20∶2至1∶5∶1。已经意外地发现，当由在以上范围内的上述卵磷脂制备时，在不需要加入非天然表面活性剂的情况下，纳米乳液是亚稳、半透明的。
优选地，在本发明的纳米乳液中使用的卵磷脂是食品级或GRAS(通常被认为是安全的)。可商购获得的卵磷脂的实例包括但不限于蛋黄卵磷脂、大豆磷脂、和99％纯蛋黄或大豆磷脂酰胆碱。在其他实施方案中，已经将卵磷脂酶改性以形成溶血卵磷脂。
卵磷脂是两种主要组分即磷脂和甘油三酯与少量如植物糖脂、植物固醇、生育酚、和游离脂肪酸的其他成分的混合物。在卵磷脂中的磷脂包括磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇、磷脂酸。在某些实施方案中，在卵磷脂中的磷脂酰胆碱的水平在5至80％、优选40至80％、或更优选50至80％的范围内。如在本文中所使用的术语“卵磷脂”是指单一类型的卵磷脂(例如，脱油的、或分馏的、或酶改性的)以及卵磷脂的混合物。卵磷脂通过提取并且纯化来源于自然存在的产品(包括但不限于大豆、蛋类、葵花籽或油菜籽(菜籽))的磷脂而制备。
食品级卵磷脂以液体、颗粒或粉末从商业来源获得并且包括，例如，由美国卵磷脂公司(American Lecithin Company(Oxford，CT))销售的ALCOLEC Lecithins和由CARGILL(Mechelen，比利时)销售的TOPCITHIN、LECIPRIME、LECISOY、EMULFLUID、METARIN、EMULPUR、LECIGRAN、EPIKURON、LECIMULTHIN、EMULTOP、和OVOTHIN Lecithins，以及由杜邦营养与健康(DuPont Nutrition&Health(St.Louis，MO))销售的SOLEC Lecithins。
通常，本发明的香料纳米乳液含有0.1％至20％之间的表面活性剂体系。在其他实施方案中，本发明的香料纳米乳液含有0.1％至10％之间的表面活性剂体系。优选地，香料纳米乳液包含1％至10％之间的第一卵磷脂和0.1％至10％之间的第二卵磷脂。所使用的卵磷脂的量可以取决于制剂所需的香料油的性质和水平以及纳米乳液的所需的影响感官和澄清度性能。
根据本发明，将香料油相乳化至水性相中，其可以占以纳米乳液的重量计65％至99％。水性相可以具有30％至95％(例如，50％至95％和70％和95％)的助溶剂如甘油、丙二醇、甘油、和/或乙醇。还可以将糖醇作为助溶剂加入至水性相中。糖醇的实例包括山梨糖醇、甘露糖醇、木糖醇、乳糖醇、麦芽糖醇、赤藓糖醇、和它们的组合。在具体的实施方案中，在纳米乳液组合物中使用水和丙二醇、甘油和糖醇中的至少一种的组合。可以使用丙二醇和糖醇、丙二醇和甘油、甘油和糖醇、或所有三者一起作为助溶剂。水和助溶剂之间的重量比通常是1∶95至1∶4(例如，1∶20至1∶5)。
在某些实施方案中，水性相进一步含有0.01％至20％的载体材料，其包括单糖和二糖，如葡萄糖、乳糖、左旋糖、海藻糖、果糖、麦芽糖、核糖、蔗糖、或它们的组合。在其他实施方案中，水性相进一步含有蛋白质、胶、和/或水胶体。适合的蛋白质包括大豆蛋白分离物、大豆蛋白浓缩物、乳清蛋白分离物、乳清蛋白浓缩物、明胶、豌豆蛋白、和蛋白水解产物。胶和水胶体的实例包括黄原胶、瓜尔胶、阿拉伯胶(gum acaia)、化学改性阿拉伯胶、果胶、和海藻酸盐。
本发明的香料纳米乳液通过在卵磷脂的存在下使用常规技术将香料油乳化为水性相而制备。简而言之，纳米乳液通常通过混合水性相和油相并且对混合物进行均质化数次(或者在本领域的术语中，进行多于一“遍(pass)”)而制备。根据本发明，预乳液步骤(即高剪切混合步骤)对于在高压均质化之前设定初始粒度来说是重要的。高剪切混合的速度可以在3,000rpm至20,000rpm的范围内并且混合的时间可以在5至30分钟的范围内。随后使用高压均化器(例如，可商购获得的Niro Panda 2000)或其他类型的均化器(例如，可商购自Microfluidics的MICROFLUIDIZER或可商购自Avestin的EMULSIFLEX)以制备纳米乳液。均质化可以在3,000/300psi至10,000/1,000psi下使用二级均化器进行二、三、或更多遍；或在6,500/500psi至20,000/2,000psi下进行一、二或更多遍。
速溶的亚稳、半透明香料纳米乳液可以用于各种消费品、食品、或药品中。尤其是，亚稳、半透明香料纳米乳液发现了在下列各项中的应用：口香糖、糕点、口腔护理产品、饮料、零食、乳制品、汤、酱汁、调味品、洗涤剂、织物软化剂和其他织物护理产品、防汗剂、除臭剂、滑石、猫砂、头发护理和造型产品、个人护理产品、空气清新剂、谷物、烘焙产品和清洁剂。
在具体实施方案中，速溶的亚稳、半透明香料纳米乳液在饮料和澄清饮料液体浓缩物中使用。因此，除了亚稳、半透明香料纳米乳液之外，本发明还提供含有本发明的亚稳、半透明香料纳米乳液的光学澄清的最终饮料产品或液体饮料浓缩物。
在一些实施方案中，速溶的亚稳、半透明香料乳液以基于最终饮料产品的重量在1ppm至60％(例如，1ppm至20％和5ppm至5％)之间的水平加料，以使得产品含有0.01ppm至10％(0.1ppm至5％、0.5ppm至1％、和1ppm至100ppm)的香料油。在使用本发明的香料乳液的情况下，由此制备的最终饮料产品是澄清的，具有10比浊测量法浊度单位(“NTU”)以下的浊度。
如在本文中所使用的，术语“液体饮料浓缩物”意指可以用另一种液体(如水性饮用液体)稀释以提供最终饮料或者在食用之前加入至食品中的液体组合物。短语“液体”是指在室温(即70°F)下非气体的、可流动的、流体组合物。如在本文中所使用的术语“最终饮料”意指已经通过标准软饮料(即，即饮的)制备工序或者通过稀释浓缩物以提供饮用、消费形式的饮料而制备的饮料。在一些方面中，由于酸化剂含量和/或香味强度，浓缩物是非饮用的。通过阐明术语“浓度”而举例的方式，75倍(即“75X”)的浓度将会等同于1份浓缩物对应74份水(或其他饮用液体)以提供最终饮料。换句话说，当确定液体饮料浓缩物的适当的稀释水平以及因此的浓度时，考虑最终饮料的香味特征。浓缩物的稀释因数还可以被表示为提供一份浓缩物所需的量。
术语“纳米乳液”和“乳液”在本文中可互换地使用。
浓缩物的粘度、pH、和配方将会至少部分取决于预期的稀释因数。在一种方法中，可以将适度浓缩的产品配制为以至少5倍的因数稀释以提供最终饮料，其可以是，例如8盎司饮料。在一个方面中，将浓缩物配制为以5至15倍的因数稀释以提供最终饮料。在这种形式下，液体浓缩物具有1.8至4或者更具体1.8至2.9、2至3.1、或2至2.5的pH；以及使用心轴S00在50rpm和20℃下利用Brookfield DVII+Pro粘度计测量的7.5至100cP、10至100cP、15至100cP、10至50cP、或10至20cP的粘度。在一些实施方案中，浓缩物至少包含基于浓缩物的重量0.1至15百分比的酸化剂。如果需要，可以使用任何可食用的、食品级有机或无机酸，如，但不限于，柠檬酸、苹果酸、琥珀酸、乙酸、盐酸、己二酸、酒石酸、富马酸、磷酸、乳酸、酸式焦磷酸钠、它们的盐、以及它们的组合。酸化剂的选择可以至少部分取决于浓缩物的所需pH和/或酸化剂赋予稀释的最终饮料的味道。在另一个方面中，在浓缩物中包含的酸化剂的量可以取决于酸的强度。例如，与更强的酸如磷酸相比，在浓缩物中将会需要更大量的乳酸以降低最终饮料中的pH。在一些实施方案中，可以将缓冲液加入至浓缩物中以在所需pH下提供增加的酸含量。适合的缓冲液包括，例如，酸的共轭碱、葡萄糖酸盐、乙酸盐、磷酸盐或酸的任何盐(例如，柠檬酸钠和柠檬酸钾)。在其他实例中，酸的未解离的盐可以使浓缩物缓冲。
本发明的饮料或浓缩物可以包含来自用于大块固体加入的水果或蔬菜的一种或多种果汁或果汁浓缩物(如至少4X浓缩产品)。在一个方面中，果汁或果汁浓缩物可以包括，例如，椰子汁(还通常被称为椰子水)、苹果、梨、葡萄、橙、马铃薯、蜜柑、柠檬、酸橙、番茄、胡萝卜、甜菜、芦笋、芹菜、羽衣甘蓝、菠菜、南瓜、草莓、树莓、香蕉、蓝莓、芒果、百香果、桃、李子、木瓜、和组合。如果需要，果汁或果汁浓缩物还可以作为糊状物(puree)加入。
如指出的，可以将加入至饮用液体中以形成调味饮料。在一些方面中，浓缩物可以是非饮用的(如由于高的酸含量和香味强度)。例如，可以使用饮料浓缩物以为水、可乐、碳酸水、茶、咖啡、赛尔脱兹矿泉水(seltzer)、苏打水(club soda)等提供香味，并且还可以用于增强果汁的香味。在一个实施方案中，可以使用饮料浓缩物以为酒精饮料提供香味，所述酒精饮料包括但不限于调味香槟、起泡葡萄酒(sparkling wine)、葡萄汽酒(winespritzer)、鸡尾酒、马提尼酒(martini)等。在具体的实施方案中，浓缩物在光学澄清饮料中使用。
饮料浓缩物还可以与各种食品组合以为食品增加香味。例如，可以使用浓缩物为各种固体、半固体、和液体食品提供香味，所述食品包括但不限于燕麦片、谷物、酸奶、脱乳清酸奶、白软干酪(cottage cheese)、奶油奶酪、霜状白糖、沙拉酱、酱汁、以及甜点如冰淇淋、果汁冻(sherbet)、果汁冰糕(sorbet)、和意大利冰淇淋(Italian ice)。饮料浓缩物与食品或饮料的适当的比率可以由本领域普通技术人员方便地确定。
本发明的其他修改对本领域技术人员来说将会是显而易见的。应理解这样的修改在本发明的范围内。另外，除非另外指定，所有份数、百分数、比例、和比率在本文中和在权利要求中通常是指基于重量。
在本文中所公开的值和尺寸不应被理解为被严格限制为所叙述的确切数值。反而，除非另外指定，每个这样的值意在表示所叙述的值和在该值附近的功能上等同的范围二者。例如，作为“50％”公开的值意在表示“约50％”。
在本文中引用的所有出版物通过整体引用结合。
通过以下非限制性实施例更详细地描述了本发明。
实施例1-2：含有两种卵磷脂的纳米乳液的制备
使用以下工序制备本发明的两种纳米乳液，即样品A和B。
油和水性相的制备。为了制备油相，在混合的情况下将6克的标准流体卵磷脂(GIRALEC，可商购自Lasenor，Barcelona，Spain；HLB为4)与30克的酸橙香料油(国际香料和香精公司(International Flavors and Frances)，Union Beach，NJ)合并，直到均匀溶解。为了制备水性相，在分离容器中，在使用高架混合机混合的情况下，将600克的70％山梨糖醇水溶液、254克的甘油、和100克的丙二醇合并，直到均匀。在使用Silverson高剪切混合机(Model L4RT(SILVERSON))以6,500rpm高剪切混合5分钟的情况下，将十克的分馏卵磷脂(来自American Lecithin Company，Oxford，CT的ALCOLEC PC 50；HLB为8；脱油的，含有50％磷脂酰胆碱)逐渐加入至水性相中，直到完全溶解。
半透明乳液的形成。通过将油相和以上在使用Silverson高剪切混合机(型号L4RT)以6,500rpm高剪切混合3分钟的情况下制备的水性相混合，形成预乳液。在高压NiroPanda 2000均化器(Niro Soavi，Hudson，WI)中在7,000/700psi下对预乳液进一步处理三遍。根据该实施例制造的样品被称为“样品A”，以用于实施例5和6。通过Malvern Zetasizer(Malvern Instruments Ltd，Worcestershire，UK)测量乳液的粒度。将乳液在水中以1重量％稀释，以用于粒度测量。
根据上述相同工序制备样品B，不同之处在于使用6克的SOLECK-EML溶血卵磷脂(HLB为8)代替标准卵磷脂并且使用20克的ALCOLEC C LPC20脱油溶血卵磷脂(HLB为12)代替10克的ALCOLEC PC50。
实施例3-4：含有三种卵磷脂的澄清乳液的制备
油和水性相的制备。为了制备油相，在混合的情况下将3克的标准液体卵磷脂(GIRALEC，可商购自Lasenor，Barcelona，Spain；HLB为4)与30克的酸橙香料油(国际香料和香精公司(International Flavors and Frances)，Union Beach，NJ)合并，直到均匀溶解。为了制备水性相，在分离容器中，在使用高架混合机混合的情况下，将600克的70％山梨糖醇水溶液、254克的甘油、和100克的丙二醇合并，直到均匀。在使用Silverson高剪切混合机(Model L4RT(SILVERSON))以6,500rpm高剪切混合5分钟的情况下，将来自AmericanLecithin Company(Oxford，CT，USA)的十克的分馏卵磷脂(ALCOLEC PC 50)和来自Cargill的3克的EMULPUR SF标准脱油卵磷脂(Decatur，IL；HLB为7)逐渐加入至水性相中，直到完全溶解。
半透明乳液的形成。通过将油相和以上在使用Silverson高剪切混合机(型号L4RT)以6,500rpm高剪切混合3分钟的情况下制备的水性相混合，形成预乳液。在高压NiroPanda 2000均化器(Niro Soavi，Hudson，WI)中在7,000/700psi下对预乳液进一步处理3遍。根据该实施例制造的样品被称为“样品C”，以用于实施例5和6。通过Malvern Zetasizer(Malvern Instruments Ltd，Worcestershire，UK)测量乳液的粒度。将乳液在去离子水中以1重量％稀释，以用于粒度测量。
在实施例1-2中描述的预乳液步骤和高压均化器二者的处理参数的范围也适用于实施例3-4。
利用在实施例中描述的相同工序制备样品D，不同之处在于使用SOLEC K-EML溶血卵磷脂代替相同量的标准卵磷脂并且使用ALCOLEC C LPC20脱油溶血卵磷脂代替相同量的ALCOLEC PC50。
实施例5：卵磷脂系纳米乳液的表征
使用浊度计以由美国环保局规定的NTU的单位得到浊度程度测量。对于饮料来说，具有高于15的NTU值将会被认为是模糊和不澄清的。对于澄清饮料来说，优选的范围是0.1至10，并且更优选的范围是0.1至5。将在实施例1-4中制备的纳米乳液A-D应用于根据表2的饮料配方的最终饮料。
表2
| 最终饮料 | g/L |
| 纳米乳液 | 1 |
| 糖浆67°白利糖度(Brix) | 150 |
| 柠檬酸50％溶液 | 3 |
| 水 | 最终适量至1L |
在表3中包括四种纳米乳液的平均粒度、微乳液的浊度、最终饮料的浊度。所有纳米乳液都是半透明的。所有最终饮料都是光学澄清的。通常，较高的表面活性剂浓度得到较小的平均粒度，其因此得到最终饮料的较低的浊度值，在样品A和B中显示出来。相反，在相同浓度下的表面活性剂的选择可能会得到最终饮料的不同的粒度和浊度值，在样品C和D中显示出来。
表3
| 特征 | 样品A | 样品B | 样品C | 样品D |
| 平均粒度(nm) | 137 | 90 | 140 | 94 |
| 纳米乳液的浊度(NTU) | 107 | 120 | 112 | 143 |
| 最终饮料的浊度(NTU) | 10.1 | 2.8 | 8.4 | 4.1 |
实施例6：卵磷脂系纳米乳液的感官性能
为了确立卵磷脂系纳米乳液的消费者益处，在根据表2制备的饮料中，选择在实施例1和3中制备的两种香料纳米乳液(样品A和C)与参考样品(蔗糖单棕榈酸酯系纳米乳液)进行比较。采用由12名评价者组成的专家组评价酸橙香气和香味二者的强度以及不正常的气味和不正常的味道，显示在表4中。统计学分析未显示出蔗糖单棕榈酸酯系纳米乳液(对照)和本发明的卵磷脂系纳米乳液之间的显著性差异(p＝0.05)，表明卵磷脂系纳米乳液能够提供与含有非天然、合成表面活性剂蔗糖单棕榈酸酯的常规蔗糖单棕榈酸酯系体系可比的香料质量和特征的全部益处。
表4
实施例7-11：具有不同的卵磷脂比率的纳米乳液的制备
根据在以上实施例1-2中描述的相似工序制备本发明的五种纳米乳液，不同之处在于使用不同量的卵磷脂。参见以下表5。根据在实施例5中描述的工序制备各自含有纳米乳液的最终饮料。测量它们的浊度。意外地，所有最终饮料都是光学澄清的，具有低于10的浊度。随着标准液体卵磷脂与ALCOLEC C LPC20(HLB＝12；含有20％以上的溶血磷脂酰胆碱和40％的磷脂酰胆碱+溶血磷脂酰胆碱)的比率增加以及磷脂酰胆碱与溶血磷脂酰胆碱的比率增加，浊度值增加。参见表5和6。
表5
| 样品 | 样品E | 样品F | 样品G | 样品H | 样品I |
| 标准液体卵磷脂(克) | 2.4 | 6 | 13 | 20 | 23.6 |
| ALCOLEC C LPC20的重量(克) | 23.6 | 20 | 13 | 6 | 2.4 |
| 最终饮料的浊度(NTU) | 1.9 | 2.5 | 2.7 | 7 | 9.9 |
表6
实施例12-15：具有不同的卵磷脂量的纳米乳液的制备
根据在实施例1-2中描述的工序制备另外四种纳米乳液，其中卵磷脂的总重量相对于恒定重量的香料(30克)增加。参见表7。根据在实施例5中描述的工序制备各自含有纳米乳液的最终饮料，并且测量饮料的浊度。除了在表面活性剂体系中含有高游离脂肪酸水平的样品M之外，结果显示，最终饮料的浊度值随着总卵磷脂水平的增加而降低。
表7
实施例16-18：含有不同的游离脂肪酸量的纳米乳液的制备
根据在实施例1-2中描述的工序制备两种额外的本发明的纳米乳液和比较的纳米乳液，其中使用26克的游离脂肪酸水平不同的不同类型的卵磷脂。根据在实施例5中描述的工序制备各自含有纳米乳液的最终饮料。测量它们的浊度。参见表8。分别使用含有小于10％的游离脂肪酸的表面活性剂体系制备本发明的样品N和O。使用含有28％的游离脂肪酸的表面活性剂体系制备比较的纳米乳液。意外地，样品N和O各自具有6以下的浊度，而比较的P具有高至24NTU的浊度，表示是非澄清的。
表8
| 样品 | 样品N | 样品O | 比较的P |
| 游离脂肪酸(％) | 6.9 | 9.8 | 28 |
| 最终饮料的浊度(NTU) | 5.3 | 6 | 24.1 |
其他实施方案
本说明书中所公开的全部特征可以以任何组合方式进行组合。本说明书中所公开的各个特征可以被提供相同、等价、或类似目的的备选特征替换。因此，除非另外明确指出，所公开的各个特征仅是一系列等价或类似特征的一个实例。
实际上，为了制备半透明、亚稳香料纳米乳液，实现制备澄清液体饮料的目的，本领域技术人员可以通过使用不同香料和卵磷脂、改变香料和卵磷脂的浓度来设计并且制备纳米乳液，以在澄清饮料或浓缩物中实现所需的影响感官的特征或释放特征。此外，香料、卵磷脂、和水之间的比率也可以由技术人员通过本领域中已知的制备具有所需性质的纳米乳液的试验来确定。
根据以上描述，技术人员可以容易地确定本发明的基本特征，并且在不背离其精神和范围的情况下，可以做出本发明的多种变化和修改以使其适应多种用途和情况。因此，其他实施方案也在权利要求的范围内。
Claims (16)
1.一种亚稳、半透明香料纳米乳液，所述亚稳、半透明香料纳米乳液包含香料油相、水性相、以及含有第一卵磷脂和第二卵磷脂的表面活性剂体系，其中所述纳米乳液不含任何非天然表面活性剂，所述表面活性剂体系含有15％以下的游离脂肪酸，所述第一卵磷脂具有1至8的HLB，并且所述第二卵磷脂具有8至16的HLB并且含有20％以上的磷脂酰胆碱和溶血磷脂酰胆碱。
2.权利要求1所述的亚稳、半透明香料纳米乳液，其中所述纳米乳液含有0.1％至20％的所述表面活性剂体系和1％至20％的所述香料油。
3.权利要求1所述的亚稳、半透明香料纳米乳液，其中所述第一和第二卵磷脂中的每一种是天然的、脱油的、分馏的、或酶改性的，选自由下列各项组成的组：大豆卵磷脂、蛋黄卵磷脂、葵花卵磷脂、油菜籽卵磷脂、和它们的组合；并且所述第一和第二卵磷脂之间的重量比是1∶30至10∶1，优选1∶20至5∶1，或更优选1∶10至1∶1。
4.权利要求3所述的亚稳、半透明香料纳米乳液，其中所述第二卵磷脂是含有15％以上的溶血磷脂酰胆碱和15％以下的游离脂肪酸的脱油的、分馏的、和酶改性的卵磷脂。
5.权利要求1所述的亚稳、半透明香料纳米乳液，所述亚稳、半透明香料纳米乳液还包含在所述水性相中作为助溶剂的多元醇，其中水和所述助溶剂之间的重量比是1∶95至1∶4，或优选1∶20至1∶5。
6.权利要求5所述的亚稳、半透明香料纳米乳液，其中所述多元醇是丙二醇、1，3-丙二醇、甘油、丁二醇、赤藓糖醇、木糖醇、甘露糖醇、山梨糖醇、异麦芽酮糖醇、或它们的组合。
7.权利要求1所述的亚稳、半透明香料纳米乳液，所述亚稳、半透明香料纳米乳液还包含在所述水性相中的单糖、二糖、水胶体、和它们的组合。
8.权利要求7所述的亚稳、半透明香料纳米乳液，其中所述单糖是葡萄糖、果糖、或它们的组合，所述二糖是蔗糖、麦芽糖、或它们的组合，并且所述水胶体是黄原胶、瓜尔胶、阿拉伯胶、化学改性阿拉伯胶、果胶、或它们的组合。
9.权利要求1所述的亚稳、半透明香料纳米乳液，其中所述香料油相含有油溶性维生素、油溶性着色剂、抗氧化剂、或它们的组合。
10.权利要求1所述的亚稳、半透明香料纳米乳液，其中所述表面活性剂体系还含有第三卵磷脂，并且所述第一、第二、和第三卵磷脂之间的重量比是1∶20∶2至1∶5∶1。
11.权利要求3所述的亚稳、半透明香料纳米乳液，其中所述第一卵磷脂是酶改性的卵磷脂，并且所述第二卵磷脂是含有15％以上的溶血磷脂酰胆碱和15％以下的游离脂肪酸的脱油的、分馏的、和酶改性的卵磷脂。
12.权利要求11所述的亚稳、半透明香料纳米乳液，所述亚稳、半透明香料纳米乳液还包含在所述水性相中的多元醇、单糖、二糖、水胶体、或它们的组合，其中所述多元醇是丙二醇、1，3-丙二醇、甘油、丁二醇、赤藓糖醇、木糖醇、甘露糖醇、山梨糖醇、异麦芽酮糖醇、或它们的组合，所述单糖是葡萄糖、果糖、或它们的组合，所述二糖是蔗糖、麦芽糖、或它们的组合，并且所述水胶体是黄原胶、瓜尔胶、阿拉伯胶、化学改性阿拉伯胶、果胶、或它们的组合。
13.权利要求12所述的亚稳、半透明香料纳米乳液，其中所述纳米乳液含有0.1％至20％的所述表面活性剂体系和1％至20％的所述香料油相，并且所述香料油相含有油溶性维生素、油溶性着色剂、抗氧化剂、或它们的组合。
14.权利要求13所述的亚稳、半透明香料纳米乳液，其中所述表面活性剂体系和所述香料油的重量比是1∶10至2∶1，或优选1∶5至1∶1，并且所述表面活性剂体系含有(i)10％以下、或优选5％以下的游离脂肪酸和(ii)4∶1至1∶5、或优选1∶1至1∶4的重量比的磷脂酰胆碱和溶血磷脂酰胆碱。
15.一种包含权利要求1所述的亚稳、半透明香料纳米乳液的液体饮料或液体饮料浓缩物。
16.一种用于制备权利要求1的亚稳、半透明香料纳米乳液的方法，所述方法包括在表面活性剂体系的存在下将香料油乳化至水性相中，其中所述表面活性剂体系含有第一卵磷脂和第二卵磷脂，所述纳米乳液不含任何非天然表面活性剂，所述表面活性剂体系含有15％以下的游离脂肪酸，所述第一卵磷脂具有1至8的HLB，并且所述第二卵磷脂具有8至16的HLB并且含有20％以上的磷脂酰胆碱和溶血磷脂酰胆碱。
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| CN115397252A (zh) * | 2020-12-18 | 2022-11-25 | 弗门尼舍有限公司 | 用于饮料和个人护理应用的风味剂组合物 |
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| CN107105708A (zh) | 2017-08-29 |
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| EP3209137B1 (en) | 2019-12-18 |
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