CN106038511A - 一种纳米番茄红素微囊化冷水分散型粉剂的制备方法 - Google Patents
一种纳米番茄红素微囊化冷水分散型粉剂的制备方法 Download PDFInfo
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- CN106038511A CN106038511A CN201610409246.3A CN201610409246A CN106038511A CN 106038511 A CN106038511 A CN 106038511A CN 201610409246 A CN201610409246 A CN 201610409246A CN 106038511 A CN106038511 A CN 106038511A
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- A—HUMAN NECESSITIES
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- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
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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
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- Chemical & Material Sciences (AREA)
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
本发明涉及一种纳米番茄红素微囊化冷水分散型粉剂的制备方法，该方法采用无毒溶剂使番茄红素与复配的非离子表面活性剂等充分溶解均质后达到纳米级，然后加入赋形剂壁材混合均匀，使纳米番茄红素均匀分布在溶融状态的壁材中，经过喷雾干燥或真空干燥后粉碎得到微囊粉剂。这种微囊粉剂番茄红素含量可达10%以上，经过赋形剂壁材包埋，番茄红素稳定性大大提高，采用冷水分散，乳液呈透明或半透明状，并且非常稳定。通过番茄红素的纳米化，使其更加有利于人体吸收，生物活性明显提高，可广泛适用于医药保健的软硬胶囊、片剂、微乳等方面以及食品工业领域。
Description
技术领域
本发明涉及一种纳米番茄红素微囊化冷水分散型粉剂的制备方法。通过该方法可制备一种经过壁材包埋的冷水分散速溶、活性成分高并且稳定的纳米番茄红素微囊粉剂，本工艺克服了以往番茄红素水分散粉剂含量低，易氧化，水分散后容易分层的缺陷。另外，通过番茄红素的纳米化使其更加有利于人体吸收。因此，纳米水分散番茄红素粉剂可以广泛用于医药保健和食品工业领域。
背景技术
番茄红素(Lycopene)分子式C40H56，分子量536.85，一般结构是由11个共轭及2个非共轭碳碳双键组成的直线型碳氢化合物，纯品为针状深红色晶体，不溶于水，难溶于甲醇、乙醇，可溶于乙醚、石油醚、丙酮、乙酸乙酯，易溶于氯仿、苯、二硫化碳等有机溶剂，是一种脂溶性天然色素，是类胡萝卜素的一种。天然番茄红素在470nm有最大吸收峰，可以作为功能性食品着色剂，突出的抗氧化功能使其在作为着色剂时能起到抗氧化作用，是目前国际公认和最有发展前景的复合功能食品添加剂。最新研究结果表明，番茄红素抗氧化性很强，是维生素E的100倍，β-胡萝卜素的2倍以上。而且番茄红素具有多种生物活性，如淬灭单线态氧、清除自由基、诱导细胞间隙连接通讯，调控肿癌增殖。因此，番茄红素是一种很有发展潜力的新型功能性天然色素，作为具有营养与着色双重作用的食品添加剂，广泛应用于保健食品、医药和化妆品领域。但是，番茄红素油树脂在食品的加工过程中不易分散，其高含量的结晶番茄红素由于易被氧化难以保存，也严重影响人体吸收，限制了番茄红素在食品中的应用，使得不溶于水的番茄红素在食品饮料领域几乎无法使用。在医药保健食品仅仅应用在软胶囊方面，而硬胶囊、片剂几乎不能应用。另外油树脂或高含量结晶体保存与运输都存在问题。为了解决番茄红素水分散技术专利公开号CN103229925A提出了采用植物油溶解番茄红素的方法，由于大量植物油的存在，必须使用大量赋形剂掩盖油脂的问题，这种方法获得的粉剂番茄红素含量很低，粉剂不易保存，渗油明显，水分散后乳液不够稳定，无法满足保健食品行业的应用。CN101092521A提出了一种纳米乳液的制备方法，采用溶剂溶解番茄红素，均质后与水相合并制成纳米乳液.目前国内还没有理想的容易保存的纳米分散颗粒粉剂产品和文献报道。
发明内容
本发明的目的是提供一种纳米番茄红素微囊化冷水分散型粉剂的制备方法，该方法采用无毒溶剂使番茄红素与复配的乳化剂等溶解均质后达到纳米级，然后加入赋形剂壁材混合均匀，使纳米番茄红素均匀分布在溶融状态的壁材中，经过喷雾干燥或真空干燥后粉碎得到微囊粉剂。这种微囊粉剂番茄红素含量可达10％以上，经过赋形剂壁材包埋，番茄红素稳定性大大提高，采用冷水分散，乳液呈透明或半透明状，并且非常稳定，生物活性明显提高，可广泛适用于软硬胶囊、片剂、微乳等方面以及食品添加剂及饮料添加成分。
本发明的制备方法是由以下技术方案来实现的。
⑴首先将30-50％的番茄红素油树脂中加入溶剂，溶剂可以是乙醚、石油醚、乙酸乙酯、丙酮、氯仿、苯、二硫化碳等。番茄红素油树脂与溶剂的质量比是1：10～40，要求溶剂温度保持在20-35度之间。
⑵溶液中加入食品或医药级非离子表面活性剂和崩解剂，活性剂可以是蔗糖酯脂肪酸脂、聚甘油脂肪酸脂、山梨醇酐十六酸脂（斯盘40）、聚山梨脂（吐温80）、单双甘油脂、磷脂、卵磷脂等的一种或两种复配，与番茄红素的质量比是0.5-2:5.然后加入番茄红素质量0.5-5％的稳定与分散助剂，本发明的稳定与分散助剂可以是明胶、阿拉伯胶、黄原胶、卡拉胶改性淀粉、大豆分离蛋白、乳清分离蛋白、魔芋胶、海藻酸钠、羧甲基纤维素钠、交联羧甲基淀粉钠的一种和两种以上的混合物。崩解剂是羧甲基纤维素钠、交联羧甲基淀粉钠的一种，用量为番茄红素油树脂的2-10％。
⑶加入番茄红素与表面活性、崩解剂的溶液，浸泡5-10分钟后采用8000-12000转/分的高速剪切机间歇处理5-20分钟，然后再用25-35MHz超声波间歇进行纳米化均质10-35分钟，超声波功率为每千克液体按照50-300W施加，处理过程要求始终保持30-40度的温度，使番茄红素粒经主要分布在50-500nm范围内。
⑷经过纳米化处理的溶液，根据番茄红素含量的要求，在真空条件下添加一定量的赋形剂壁材，赋形剂可以是蔗糖粉、低聚葡萄糖粉、大豆分离蛋白粉、可溶性淀粉、普通淀粉、β-环糊精、糊精、魔芋精粉、番茄粉、葡萄籽提取物等的一种或两种以上任意比例的混合粉末，并在0.08MPa真空条件下，保持30-40度的温度，采用50-200转/分，充分搅拌10-30分钟，使纳米番茄红素均匀分散包埋在浆液中，同时也防止了纳米番茄红素的重新团聚。
⑸将浆液通过喷雾干燥设备形成固体干粉或在具有0.08真空条件下，采用50-100转/分的搅拌转速，温度控制在50-60度搅拌蒸干，直到没有明显溶剂或形成固体粉末状为止。
⑹喷雾干燥后或采用真空搅拌蒸干的纳米番茄红素微囊粉剂，必须在真空干燥箱内必须继续烘干48-72小时，彻底清除溶剂残留，使其达到规定的要求。
⑺经过彻底烘干的纳米番茄红素微囊粉剂，根据需要经过筛分可以获得100目以下的粉剂，或者是100-40目的颗粒。分别采用铝膜包装，填充保护气体封存。
附图说明 图1.纳米番茄红素微囊化冷水分散型粉剂的加速稳定性实验结果。
具体实施方式
实施例1:
将含量为30％的番茄红素油树脂10g加入到250ml乙酸乙酯中，加热到30度，采用8000转/分的剪切机间歇剪切15分钟，再加入斯盘40,5g，吐温80，6g，羧甲基纤维素钠1g，浸泡10分钟，继续间歇剪切10分钟，然后转移到25MHz，80W超声波均质器中，间歇均质30分钟，温度保持30-35度，完成纳米化处理，然后转移到具有搅拌器的真空釜中，利用真空吸入38g番茄粉，采用100转/分的搅拌速度搅拌20分钟，完成番茄多糖、果胶、纤维素浆液对纳米番茄红素的包埋，将真空釜温度提高到60度，真空度保持0.08MPa,进行蒸干，形成块状，然后放入真空干燥箱继续烘干48小时，取出粉碎，经过筛分，分别获得100目以下的粉剂和100目以上颗粒形状的纳米番茄红素微囊化冷水分散型颗粒粉剂，番茄红素含量≥6%。
实施例2:
将含量为30％的番茄红素油树脂10g加入到300ml氯仿中，在25度温度下，采用12000转/分的剪切机间歇剪切10分钟，再加入蔗糖酯脂肪酸脂6g，大豆分离蛋白8g，羧甲基淀粉钠1g，浸泡10分钟，继续间歇剪切10分钟，然后转移到28MHz，100W超声波均质机中，间歇均质35分钟，温度保持30-35度，完成纳米化处理，然后转移到具有搅拌器的真空釜中，利用真空吸入24g蔗糖粉与魔芋精粉，比例为1；1，温度保持40度，采用60转/分的搅拌速度搅拌25分钟，完成浆液对纳米番茄红素的包埋，然后采用喷雾干燥器喷雾干燥，所的颗粒粉剂放入真空干燥箱继续烘干24小时，得到番茄红素含量≥10％的纳米番茄红素微囊化冷水分散型颗粒粉剂。
实施例3:
将含量为40的番茄红素油树脂50g加入到2000ml乙酸乙酯中，加热到30度，采用12000转/分的恒温剪切机剪切10分钟，再加入斯盘40,25克，卵磷脂50g，羧甲基纤维素钠5克，浸泡5分钟，继续间歇剪切15分钟，然后转移到28MHz，500W超声波恒温均质机中，温度保持30-40度，完成番茄红素纳米化处理，然后转移到真空搅拌釜中，利用真空吸入150g蔗糖粉，100gβ-环糊精，300g魔芋精粉，温度保持38度，采用60转/分的搅拌速度搅拌20分钟，完成浆液对番茄红素的包埋，液体浆液通过喷雾干燥机干燥，所得的颗粒粉剂放入真空干燥箱继续烘干48小时，得到番茄红素含量大于≥6％的微囊化冷水分散型颗粒粉剂。
实施例1的纳米番茄红素冷水分散型颗粒粉剂，室温下加入50倍去离子水，15秒全部分散，溶液呈透明或半透明状，室温下避光放置7天无见分层，溶液稳定性极佳。
由图1所示，用本发明的方法，实施例1制备的纳米番茄红素冷水分散型颗粒粉剂，在60度环境下，置于开口容器内，每天取样检测，15天番茄红素基本能保持原有含量。
Claims (6)
1.一种纳米番茄红素微囊化冷水分散型粉剂的制备方法，包括以下步骤:
a)将番茄红素、非离子表面活性剂、崩解剂溶于溶剂中，经过高速剪切后再进行超声波均质。
b)在步骤a）中加入赋形剂壁材，充分搅拌均匀后通过喷雾干燥或真空干燥获得固体粉末产品。
2.根据权利要求1所述的非离子表面活性剂，活性剂可以是蔗糖酯脂肪酸脂、聚甘油脂肪酸脂、山梨醇十六酸脂、聚山梨脂、单双甘油脂、磷脂、卵磷脂的一种或两种以上复配。表面活性剂与番茄红素油树脂的质量比是0.5-2:5。崩解剂是交联羧甲基淀粉钠、羧甲基纤维素钠的一种，用量为番茄红素油树脂的2-10％。
3.根据权利要求1所述的高速剪切机转速采用8000-12000转/分，并且采用间歇工作，防止温度超过40度。
4.根据权利要求1所述的超声波均质，超声波频率为25-35MHz,超声波功率按照每公斤液体50-200W进行施加，同时保证均质温度不超过40度。
5.根据权利要求1所述的赋形剂壁材，壁材可以是蔗糖粉、低聚葡萄糖、大豆分离蛋白、可溶性淀粉、普通淀粉、β-环糊精、糊精、魔芋精粉、番茄粉、葡萄籽提取物的一种或两种以上的混合粉末。
6.根据权利要求1所述的充分搅拌均匀后通过喷雾干燥获得粉剂或者经过真空干燥，温度为50-60度，搅拌条件下进行蒸干，直到成为固体粉末为止，然后放入真空干燥箱继续烘干48小时以上，取出粉碎，经过筛分，分别获得100目以上的粉剂和100-40目以下的颗粒状产品。
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Application publication date: 20161026 |