CN100377775C - 微胶囊的制备方法 - Google Patents
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Abstract
本发明涉及一种基于使用B型明胶作为聚阳离子胶体的复合凝聚方法,用于制备“Halal”认证的含香料微胶囊。
Description
技术领域
本发明涉及食品和香料行业。它特别涉及一种用于制备可通过“Halal”认证的含香料微胶囊的复合凝聚方法。本发明所述方法是基于使用一种B型明胶作为正电荷聚合物壁材料。
背景技术
凝聚,也称作水相分离,是一种众所周知的用于包封疏水液体的技术。凝聚方法可允许提供含油的微胶囊,包封材料是一种胶凝亲水胶体,它对油是不可渗透的,并均匀且致密地沉积在作为核心的该油周围。包封材料是一种蛋白质,它可与另一种具有相反电荷的胶体进行配合。
凝聚方法主要包括含水蛋白质溶液,它可通过改变物理化学环境(稀释和/或调节pH)进行操作,根据该蛋白质的分子量、其等电点和与溶剂的相容性,以实现不同程度的该蛋白质从所述溶液的相分离。
凝聚方法可以是“简单的”或“复合的”。前一名称在当进行相分离时使用单一蛋白质来形成胶囊壁时采用。后一术语是指使用第二相反电荷非蛋白质聚合物以进行相分离。复合凝聚方法广泛地用于商业方法中,并且在文献中已有大量描述。特别地,US2,800,457和US2,800,458详细地描述了复合凝聚法。
一般地,凝聚方法包括四个基本步骤,分别是乳化、凝聚、壁形成和壁硬化。在复合凝聚方法中,包围核心材料的壁,如上所述,是由两种相反电荷高分子量胶体构成。在大多数情形中,所用正电荷胶体是明胶,一种通过水解和随后的提取自胶原得到的功能蛋白。存在着两种商业可得食品/药品级明胶,分别以“ A型明胶”和“B型明胶”表示。这两种等级之间的主要差别是由制造工艺引起的。如果胶原源是采用酸进行水解,则最终产物命名为“A”,如果它是采用石灰水(碱)进行水解,则它命名为“B”。从产品角度来看,这两种明胶主要区别在于它们的等电点。A型明胶具有的等电点在8.5-9.0之间,而B型明胶的等电点在4.8-5.5之间变动。在一种主要依赖于体系动电学稳定性的工艺中,例如凝聚,等电点的这种差异对于成功的包封是关键性的。
有关复合凝聚的先有技术,几乎总是描述使用A型明胶作为阳离子蛋白质壁。在涉及A型明胶的工艺过程中,为了使之带正电荷,pH值保持在低于后者等电点的数值。先有技术的一些文献提及使用由碱水获得的明胶(B型)作为阳离子蛋白壁的可能性,但是据我们所知,还未曾有实例描述过这种实施方式,可以确认,当使用B型明胶以其阳离子形式作为蛋白质壁时,先有技术中所述工艺不可制备出令人满意的微胶囊。另一方面,B型明胶有时在先有技术的复合凝聚工艺被提及,用作聚阴离子聚合物,即以其负电形式、与A型明胶结合作为带正电荷胶体。
现在,如同许多食品成分一样,从宗教/种族角度,对于明胶使用也存在着某些规章限制。这包括明胶的“Kosher”(犹太教清洁食品)和“Halal”(伊斯兰教合法食物)资格。通常地,A型明胶制造工艺使用猪皮作为起始原料。其结果是,由这种起始产品制得的微胶囊不可能受到所述“Halal”或“Kosher”资格。另一方面,源自牛或鱼的B型明胶,能获得Halal或Kosher认证。但是,迄今为此,先有技术所述复合凝聚工艺,在技术上还不能允许制备基于B型明胶的微胶囊。
现在,我们能够建立一种新型凝聚工艺,它适合于制备基于B型明胶作为阳离子壁材料的微胶囊。
Varaporn Buraphacheep Junyaprasert等在Drug Developmentand Industrial Pharmacy,27(6),561-566(2001)中,公开了一种用于包封维生素A的复合凝聚工艺,它结合使用阿拉伯树胶和B型明胶作为壁材料。但是,其中公开的该工艺参数不是最佳的,特别是,该微胶囊的药品含量不能超过50%w/w。
本发明所述工艺能够克服先有技术中观察到的缺点,是通过提供一种适合于制备能通过“Halal”认证并含有最多达80%w/w疏水核心材料的微胶囊的最佳复合凝聚工艺而实现。
发明内容
本发明涉及一种新型复合凝聚方法,它特别适合于制备包封有疏水核心材料的高固定(fix)微胶囊,例如,能够被结合到“Halal”认证的食品或香料的微胶囊。本发明方法使用B型明胶作为聚阳离子胶体,与聚阴离子材料结合。所述工艺参数如pH或加工步骤顺序,对于成功包封是关键性的。更特别地,所述方法其特征在于所述pH在乳化或分散步骤之前被调节到3.0-4.7之间的数值。
本发明还涉及由这种方法制得的微胶囊。这些微胶囊可通过“Halal”认证,且它们含有最多达80重量%的疏水核心材料。
本发明还涉及一种用于赋予、改善或改进食品组合物的器官感觉性能的方法,其中,由本发明所述方法制得的微胶囊被添加到所述组合物中,以及含有所述微胶囊作为活性成分的食品组合物。
因此,本发明第一目的是一种用于制备含疏水核心材料的微胶囊的方法,该方法依次包括以下步骤:a)混合带正电高分子量胶体和带负电高分子量胶体的溶液;b)调节在a)中得到的混合物的pH到3.0-4.7之间的数值;c)在该混合物中乳化或分散一种疏水核心材料;d)对在c)中得到的乳液或分散液进行水稀释和/或pH调节以进行凝聚;e)冷却在d)中得到的凝聚层以提供微胶囊的壁形成;和f)添加一种硬化剂;所述方法其特征在于所述带正电高分子量胶体是B型明胶。
“高分子量”的意思,通常是分子量在40000-100000之间。
术语“疏水核心材料”包括疏水液体材料(它们通常通过凝聚而被包封),以及固体或悬浮在疏水液体中的固体。
虽然先有技术一些文献提及B型明胶作为用于复合凝聚工艺的一种可能起始原料,但是,已经证实,已经公开的方法事实上不能制备出令人满意的基于这种壁形成材料的微胶囊,除非B型明胶是处于其阴离子形式。现在,本发明方法能够制备出非常有效的基于使用阳离子型B型明胶的释放系统,该系统具有含非常高负荷疏水核心材料的优点,另一方面还具有符合宗教/种族规章限制的优点。本发明的更多目的、方面和优点,通过下述的详细说明以及实施例,将会变得更加清楚明了。
在本发明第一步骤中,一方面,一种带正电高分子量胶体溶液,和另一方面的一种带负电高分子量胶体被混合在一起。所述方法其特征在于所述带正电高分子量胶体是B型明胶。使用呈阳离子形式的B型明胶,在这类方法中是非常不同寻常的。它暗示该溶液的pH是设定在低于其等电点的数值,即低于4.8-5.5的数值。
如上所述,B型明胶是从胶原源(例如来自牛或鱼)的碱水解获得的。碱催化水解需要数天时间才能完成。该方法的详细内容是本领域熟练技术人员公知的。
至于所述带负电胶体,任何能与蛋白质反应形成配合凝聚层的阴离子聚合物都适合于本发明方法。特别地,阿拉伯树胶、藻酸钠、琼脂、角叉菜胶、羧甲基纤维素、聚丙烯酸钠或多磷酸是适合用于本发明目的的阴离子聚合物。
在一种特定实施方式中,明胶与所述相反电荷胶体的重量比为3∶2。
本发明步骤b)包括调节在a)中得到的混合物的pH到3.0-4.7之间的数值。典型地,这可通过添加乳酸而实现。在本发明方法中,这个步骤对于特定pH数值、以及从处理阶段角度来说都是非常重要的。事实上,该调节是在添加所述疏水核心材料之前进行操作的,不同于先有技术公开的方式,其中pH通常是在乳化或分散步骤之后进行调节的。现在,已经证实,以一种意外的方式,在所述方法的特定阶段,调节该pH到合适数值,是造成微胶囊有效壁形成的原因。
该pH值一旦得到调节,疏水核心材料就在该混合物中进行乳化或分散。如上所述,这种核心材料由疏水液体、以及固体或悬浮在疏水液体中的固体组成。
在本发明一种特定实施方式中,有待包封的核心材料是一种液体香料成分或组合物。这些术语可限定多种天然和合成来源的香料物质,在当前它们被用于制备食品组合物。它们包括单一化合物或混合物。这类成分的具体实例可在现有文献中找到,例如,在Fenaroli’s Handbook of Flavor Ingredients,1975,CRC Press;M.B.Jacobs的Synthetic Food Adjuncts,1947(由Van Nostrand所编);或S.Arctander的Perfume and Flavor Chemicals,1969,Montclair,N.J.(USA)。这些物质对于调味和/或芳香化消费品领域的技术人员来说是已知的,即赋予传统调味的消费品一种风味或味道,或改进消费品的味道。
天然提取物也可被包封到本发明系统之中;这些包括例如柑橘提取物如柠檬、橙子、酸橙、柚子或橘皮油,或咖啡、茶、薄荷、可可、香草或草药和香料的香精油,等等。
疏水核心材料的含量,为所用明胶重量的35-90wt%。
本发明方法当然还适合用于包封其它不是调味成分的核心材料,例如,加香成分、药物或化妆品成分。
本发明下述步骤分别是通过水稀释/或pH调节的凝聚,接着是冷却该凝聚层以提供壁形成。该冷却必须要达到一定温度,胶体在该温度时发生胶凝。在一种特定实施方式中,冷却速率是在0.25-0.5℃/分钟之间。
最后,为了交联在该疏水核心材料周围形成的壁,添加一种硬化剂。适用于本发明目的的硬化剂的典型实例,包括甲醛、乙醛、乙二醛、戊二醛、铬矾等。
由本发明方法获得的微胶囊,构成本发明的另一目的。这些释放系统具有通过潜在“Halal”认证的优点,因此,它能用于为这类指定的最终消费品调味。
另一方面,本发明微胶囊负荷有非常高的疏水核心材料。特别地,该微胶囊可含最多达80重量%的疏水核心材料,而先有技术公开的方法在胶囊中仅允许具有最多达35重量%的活性成分。
该最终产品具有非常令人满意的壁厚和形态,并且在相同固定水平(fix level)上与由A型明胶开始制得的微胶囊的壁厚和形态是可比的,这可由图1和图2中所示的显微图片看出。
本发明方法制得的微胶囊,可用于食品和香料领域的许多种应用之中。因此,含有本发明所述微胶囊和其它调味辅料的食品组合物,也是本发明的目的。
附图说明
图1和图2是分别采用A型(图1)和B型(图2)明胶作为阳离子聚合物制得的复合凝聚层放大10倍的显微图片。
实施本发明的方式
现在,将以更详细方式在下述实例中对本发明进行描述,其中,温度以摄氏度表示,缩写词具有本领域通常的意思。
实施例1
按照本发明所述方法制备微胶囊-与其它方法进行对比
使用B型明胶(250 Bloom,源自:SKW Biosystems,USA)、阿拉伯树胶、冷压橙皮油、柠檬油精、丁香酚和乙酸辛酯,用于制备微胶囊。改变胶体浓度、体系pH、稀释水数量、处理步骤顺序和明胶与阿拉伯树胶间的比率,进行多个试验。
表1给出了每个试验中所用成分的量。
表1:在5个试验中本发明方法中明胶、水、阿拉伯树胶、水、香料和稀释水的数量
试验号 | 1 | 2 | 3 | 4 | 5 |
明胶(g) | 9 | 9 | 7.5 | 9 | 9 |
水(g) | 100 | 100 | 100 | 100 | 100 |
阿拉伯树胶(g) | 6 | 6 | 7.5 | 6 | 6 |
水(g) | 150 | 150 | 150 | 150 | 150 |
香料(g) | 60 | 60 | 60 | 60 | 60 |
稀释水(g) | 200 | 400 | 400 | 200 | 200 |
制备过程
所有微胶囊都是通过一种包括乳化或分散、凝聚(水稀释)、壁形成(冷却)和交联的基本步骤的方法制得的。但是,每个试验相互之间,在所述方法中的成分含量和/或pH调节的阶段是变化的。在所有试验中,胶体溶液是在37-40°的温度进行混合。体系最终温度为22-24°。通过添加乳酸调节pH值。冷却速率是在0.25-0.5°/分钟之间。在冷却批料到该最终温度之后,添加0.14重量%的戊二醛溶液(25%),以交联该蛋白质壁。
试验#1:以下述顺序对这些成分进行混合:在明胶溶液和阿拉伯树胶溶液的混合物中乳化香料(冷压橙皮油)。添加稀释水。以递减方式调节批料pH值从4.64到2.82,但实际上没有壁形成。
试验#2:本试验除采用两倍稀释水之外,与试验1相同。试验是不成功的。
试验#3:除了胶体溶液浓度随着该比率变化之外,与试验2相同。试验是不成功的。
试验#1-3表明了本发明方法中进行的步骤的顺序的重要作用。当该pH值在乳化/分散步骤之后进行调节时,没有发生壁形成。
试验#4:其配方与试验1相同。添加顺序发生改变。在混合胶体溶液之后,于添加香料油之前,采用乳酸调节pH值到3.0。发现了极好的壁的形成。此试验证实了在所述方法中pH调节阶段的重要性。
试验#5:除了香料是柠檬油精、丁香酚和乙酸辛酯的60∶20∶20混合物组成之外,所有事情都是按试验#4进行。试验是成功的。
从上述实验可以得出结论:采用B型明胶制备微胶囊是成功的,只要该胶体溶液的pH值得到合适的调节,且只要该调节是在添加疏水核心材料之前进行的。
Claims (8)
1.一种用于制备含疏水核心材料的微胶囊的方法,该方法依次包括以下步骤:
a)混合带正电高分子量胶体和带负电高分子量胶体的溶液;
b)调节在a)中得到的混合物的pH到3.0-4.7之间的数值;
c)在该混合物中乳化或分散一种疏水核心材料;
d)对在c)中得到的乳液或分散液进行水稀释和/或pH调节以进行凝聚;
e)冷却在d)中得到的凝聚层以提供微胶囊的壁形成;和
f)添加一种硬化剂;
所述方法其特征在于所述带正电高分子量胶体是B型明胶。
2.如权利要求1所述的方法,其特征在于B型明胶与所述带负电高分子量胶体间的重量比为3∶2。
3.如权利要求1所述的方法,其特征在于所述冷却步骤是以0.25-0.5℃/分钟的速率进行的。
4.如权利要求1所述的方法,其特征在于所述疏水核心材料是一种香料成分或组合物。
5.能够由权利要求1所述方法制得的微胶囊。
6.如权利要求5所述的微胶囊,含有最多达80重量%的疏水核心材料。
7.一种食品组合物,含有权利要求5所述微胶囊作为活性成分以及香料辅剂。
8.一种用于赋予、改善或改进调味组合物的器官感觉性能的方法,包括添加权利要求5所述微胶囊到所述组合物之中。
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US20040032036A1 (en) * | 2002-08-19 | 2004-02-19 | Anandaraman Subramaniam | Process for the preparation of flavor or fragrance microcapsules |
WO2007113706A1 (en) | 2006-04-04 | 2007-10-11 | Firmenich Sa | Method for preparing microcapsules by coacervation |
WO2008063158A2 (en) * | 2006-10-31 | 2008-05-29 | William Marsh Rice University | Method for nanoencapsulation |
JP2008206420A (ja) * | 2007-02-23 | 2008-09-11 | Fuji Oil Co Ltd | 食品水分移動防止用ポリイオンコンプレックス膜 |
US20100086651A1 (en) * | 2007-05-21 | 2010-04-08 | Dardelle Gregory | Large coacervated capsules |
US9186640B2 (en) * | 2007-08-28 | 2015-11-17 | Pepsico, Inc. | Delivery and controlled release of encapsulated lipophilic nutrients |
US20100028503A1 (en) * | 2008-07-30 | 2010-02-04 | Jimbay Peter Loh | Simultaneous Multiple Acervation Process |
EP2292102A1 (en) * | 2009-09-02 | 2011-03-09 | Lipofoods, S.L. | Microcapsules containing salts for food products |
US9743688B2 (en) | 2010-03-26 | 2017-08-29 | Philip Morris Usa Inc. | Emulsion/colloid mediated flavor encapsulation and delivery with tobacco-derived lipids |
JP5931859B2 (ja) | 2010-06-30 | 2016-06-08 | フイルメニツヒ ソシエテ アノニムFirmenich Sa | 固形コアコアセルベート化したカプセル |
US20140106032A1 (en) | 2011-06-07 | 2014-04-17 | Firmenich Sa | Core-shell capsules |
CN102441354A (zh) * | 2011-10-27 | 2012-05-09 | 天津大学 | 一种黑白电泳显示微胶囊的制备方法 |
US20130251855A1 (en) * | 2012-03-21 | 2013-09-26 | Pepsico, Inc. | Aqueous product comprising oil-containing microcapsules and method for the manufacture thereof |
US10092023B2 (en) | 2012-05-24 | 2018-10-09 | Firmenich Sa | Hybrid coacervate capsules |
TWI605870B (zh) * | 2012-10-25 | 2017-11-21 | 奇華頓公司 | 方法 |
SG11201705845VA (en) | 2015-02-06 | 2017-08-30 | Firmenich & Cie | Microcapsules imparting intense vanilla odor note |
CN108697591B (zh) | 2016-02-18 | 2022-06-17 | 国际香料和香精公司 | 聚脲胶囊组合物 |
ES2950434T3 (es) | 2016-09-16 | 2023-10-10 | Int Flavors & Fragrances Inc | Composiciones de microcápsula estabilizadas con agentes de control de la viscosidad |
CN109645555A (zh) * | 2019-01-30 | 2019-04-19 | 湖北中烟工业有限责任公司 | 一种用于新型加热不燃烧烟草中的果香香线的制备方法和应用 |
JP2021106507A (ja) * | 2019-12-27 | 2021-07-29 | 小林製薬株式会社 | ゼラチン含有組成物及び吸湿抑制方法 |
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