CN108697149A - 振动液滴形成 - Google Patents

振动液滴形成 Download PDF

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CN108697149A
CN108697149A CN201780012640.6A CN201780012640A CN108697149A CN 108697149 A CN108697149 A CN 108697149A CN 201780012640 A CN201780012640 A CN 201780012640A CN 108697149 A CN108697149 A CN 108697149A
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oil
vitamin
dispersion
particle
acid
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K·迈尔-伯姆
T·黑尔加松
K·科尔特
W·多布勒
C·斯塔达格尔
M·舍恩赫尔
K·凯斯滕
N·内斯特勒
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Abstract

本发明涉及制备颗粒的方法，所述颗粒包含类胡萝卜素和/或维生素和/或ω‑3脂肪酸和/或植物甾醇和/或共轭亚油酸，所述颗粒具有窄的粒度分布和均匀的球形形状和密度，并且还涉及通过该方法可获得的颗粒以及其作为食物补充剂、食物、饲料、身体护理产品和药物的用途。与现有技术相比，本发明的颗粒具有改善的储存稳定性。该颗粒通过振动液滴形成制备。

Description

振动液滴形成
本发明涉及制备颗粒的方法，所述颗粒包含类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸，所述颗粒具有窄的粒度分布和均匀的球形形状和密度，并且还涉及通过该方法可获得的颗粒以及其作为食物补充剂、食物、饲料、身体护理产品和药物的用途。与现有技术相比，本发明的颗粒显示出改善的储存稳定性。
通过US 4522743中描述的方法制备的包含类胡萝卜素和/或维生素的颗粒具有高比例的空气夹杂物，其可以占总颗粒体积的>40％腔。由于这些空气夹杂物，颗粒在机械上不如固体颗粒稳定。颗粒可能在进一步加工过程中受损，并且导致产品性能恶化。除了空气夹杂物外，这些颗粒通常具有宽粒度分布的特征，可能与相当不均匀的颗粒形状配对。特别是通过在机械应力下压碎空心球体，但也由于宽的粒度分布和与之相关的细小粉尘含量和不均匀的颗粒形状，这些制剂具有大的表面积，使它们对于氧对颗粒中存在的类胡萝卜素和维生素的氧化攻击敏感。
因此，本发明的目的是提供一种提供不具有现有技术的这些缺点的颗粒的方法。
该目的是通过以下方法来实现的：通过在含有水胶体的溶液中分散类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸来制备球形颗粒，并且由通过振动液滴化方法形成的分散体制备液滴，并且将得到的液滴固化并且通过蒸发溶剂干燥。
在本发明的上下文中，球形表示个体粒子各自具有1至1.2的长宽比。“长宽比”是最大和最小粒径的商。
在本发明的上下文中，分散体既表示乳液又表示悬浮液。
在振动液滴化过程中，喷嘴和/或分散体和/或包含分散体的储存容器和/或供给喷嘴分散体的供给线被振动激发。所使用的振动激发器可以是机械振荡器、磁感应振荡器、气动振荡器、压电换能器或电声换能器。在这种情况下，振动发生器可以作用在喷嘴和/或供给线和/或储存容器上。也有可能直接用超声处理分散体，例如使用电声换能器，或者直接使用振动挡板/柱塞来激发，以便使离开喷嘴的分散体液滴化为均匀的液滴。
这些液滴化过程的优点是获得了已经形成的球形颗粒的单分散分布。
在制备过程中作用于设备或分散体的频率保持恒定，其中优选应用的激发频率为50至10 000Hz，优选范围为100至5000Hz，并且特别优选范围为400至4000Hz。分散体在40℃的粘度为≥80mPas。最后，喷嘴直径范围应当为50至1000μm。
利用这些参数，可以产生具有窄粒度分布的球形颗粒，其中，取决于频率和喷嘴直径，直径在100至1500μm的颗粒是可实现的。
在这种情况下，优选进行这样的方法，以便得到粒径分布在范围为150至600μm的≥75％，优选在范围为150至600μm的≥85％，特别优选在范围为150至600μm的≥95％的球形颗粒。
特别地，该方法的特征在于，以粒径分布的跨度(X90-X10除以X50)测量的多分散性小于1.0，优选小于0.8，并且特别优选小于0.6，其中X50值代表平均粒径分布，并且差X90-X10代表粒径分布的宽度。
球形颗粒的含量由水胶体基质组成，其中类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸呈现均匀分布。这些颗粒的特征在于，封闭在颗粒中的空腔体积为≤40％，优选≤30％，贝亲特别优选≤20％的颗粒总体积。
在本发明的上下文中，在这种情况下，类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸被理解为表示维生素A、D、E或K或其衍生物，例如维生素A和维生素E的酯，例如乙酸视黄酯或乙酸生育酚酯、生育三烯酚(tocotrienol)、维生素K1、维生素K2，以及类胡萝卜素，例如β-胡萝卜素、斑蝥黄、虾青素、桔黄质(citranaxanthin)和酯衍生物、玉米黄质和酯衍生物、叶黄素和酯衍生物、番茄红素和阿朴胡萝卜素醛(apocarotenal)。
根据本发明的合适的水胶体是植物胶、改性植物胶、明胶、改性明胶、改性淀粉、木素磺酸盐、壳聚糖、角叉菜胶、酪蛋白、酪蛋白酸盐、乳清蛋白质、玉米醇溶蛋白、改性纤维素、果胶、改性果胶、植物蛋白质和改性植物蛋白质或其混合物。
在这种情况下，植物胶包括琼脂、海藻酸、海藻酸盐、糖胶树胶、玛树脂、药用蜀葵提取物、结冷胶、瓜尔豆籽粕(guar seed meal)、***胶、来自车前子壳的胶、来自云杉树汁液(sap)的胶、角豆籽粉、刺梧桐胶、魔芋粉、乳香(mastic)、他拉豆胶、黄蓍胶、黄原胶。
根据本发明，优选作为水胶体的是明胶和/或植物胶和/或改性植物胶，并且特别是植物胶中的***胶。
此外，在添加类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸之前或之后，可以将抗氧化剂添加到水胶体溶液中，以提高其对氧化降解的稳定性。在这种情况下，抗氧化剂选自dl-α-生育酚、d-α-生育酚、β-生育酚、γ-生育酚、δ-生育酚、丁基羟基甲苯(BHT)、丁基羟基茴香醚、没食子酸丙酯、没食子酸辛酯、没食子酸十二酯、迷迭香提取物、绿茶提取物和其它没食子酸衍生物、叔丁基羟基喹啉、乙氧喹啉、鼠尾草酚、鼠尾草酸、抗坏血酸棕榈酸酯和抗坏血酸硬脂酸酯或其混合物。
抗氧化剂在颗粒组合物中的比例为0.1至10％重量，优选0.5至8.5％重量，基于颗粒组合物(不含粉剂(powdering agent))的干质量，所述颗粒组合物包含类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸，其中各组分的百分比合计为100％。
为了提高球形颗粒的机械稳定性，在水胶体中添加软化剂，例如糖或糖醇也是合适的，所述的糖或糖醇例如蔗糖、葡萄糖、葡萄糖糖浆、乳糖、转化糖和其它葡萄糖-果糖组合物、山梨醇、甘露醇、甘油、麦芽糊精、异麦芽糖或异麦芽酮糖醇(isomalt)。名称异麦芽酮糖醇表示糖替代品，它也用商品名(Südzucker,Germany)提供。异麦芽酮糖醇是氢化异麦芽糖，它由大约等比例的6-O-α-D-吡喃葡萄糖基-D-山梨醇和1-O-α-D-吡喃葡萄糖基-D-甘露醇组成。优选使用的软化剂是蔗糖、葡萄糖糖浆、山梨醇和乳糖。
通常选择保护胶体和软化剂与类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸的比例，从而获得固体制剂，其包含0.01至50％重量的类胡萝卜素和/或维生素，10至65％重量、优选15至60％重量的保护胶体和5至60％重量、优选10至50％重量的软化剂，其中所有百分比指的是颗粒组合物的干质量(没有粉剂)并且各组分的百分比合计为100％。
此外，可以使用乳化剂，例如抗坏血酸棕榈酸酯、聚甘油脂肪酸酯、山梨醇脂肪酸酯、丙二醇脂肪酸酯或卵磷脂，其浓度为0至200％重量，优选5至150％重量，特别优选为10至80％重量，基于所用的类胡萝卜素和/或维生素。
此外，使用另外的生理上可耐受的油也是可能有利的，例如芝麻油、玉米胚芽油、棉籽油、大豆油、花生油、葵花籽油、菜籽油、椰子油、棕榈油、橄榄油、动物脂肪、猪油、牛油、改性油或其混合物，其浓度为0至500％重量，优选10至300％重量，特别优选20至100％重量，基于类胡萝卜素和/或维生素。
除了指定的组分之外，还可以将其它常规助剂和添加剂例如无机盐和有机盐有利地添加到分散体中，以制备含有类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸的颗粒组合物。
助剂和添加剂的比例通常为0.2至20％重量，优选0.3至15％重量，特别优选0.4至10％重量，特别优选0.5至5％重量，基于颗粒组合物的干质量(没有粉剂)，其中各组分的百分比合计为100％。
根据DE2534091中的细节，例如，通过喷雾干燥或通过喷雾冷却或通过包封颗粒、分离和干燥，可以在流化床中以本身已知的方式从分散体制备粉末制剂。
在这种情况下，形成的液滴被粉剂包封，所述粉剂可以选自疏水性二氧化硅、亲水性二氧化硅、淀粉、改性淀粉、玉米淀粉、纤维素、改性纤维素、硅酸钙、硅酸钙镁、碳酸钙、磷酸三钙、己二酸钙、己二酸镁、二氧化钛、木质素、高度分散的果胶、改性果胶、植物蛋白质、改性的植物蛋白质和它们的组合。
本发明的方法的特征在于，所产生的液滴在10℃至80℃的温度被粉剂包裹，随后在40℃至120℃的进料空气温度固化和干燥。
优选以下加工方案：其中将包含类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸的分散体喷入充满疏水二氧化硅或玉米淀粉粉剂的惰性气体气氛中。
特别地，优选以下加工方案：其中在喷雾之后，将粉末干燥成残留含水量低于10％重量，优选低于6％重量。
本发明进一步涉及颗粒组合物，除所述组分之外，其还包含相对于活性成分的重量比例为0.025倍至4倍的粉剂或粉剂混合物。另外，还要求保护本发明的制剂形式作为食物补充剂、食物、饲料、身体护理产品和药物的用途。
附图：
图1：根据1A制备的颗粒的扫描电子显微照片
图2：根据1B制备的颗粒的扫描电子显微照片
图3：试验1A和1B的粒度分布
在下面的实施例中，更详细地解释了本发明的颗粒的制备。
非创造性实施例1A
将30g的斑蝥黄以及0.6g抗坏血酸棕榈酸酯和8g乙氧喹啉一起悬浮于240g异丙醇中，并且在将限压阀设置为30bar时，在混合室A中继续与390g异丙醇混合。在悬浮液侧的6L/h和溶剂侧的9L/h的计量速率下，混合室A中设定170℃的混合温度。停留时间0.3秒后，分子分散的溶液在混合室B中与32g明胶和120g葡萄糖糖浆在4000g水中混合，流速为100L/h异丙醇。在蒸馏装置中减压除去溶剂后，获得活性成分分散体，其可以通过喷雾干燥转化为稳定的水溶性干燥粉末。在水中溶解后，测量粒径为150nm。将制备的乳液通过25bar的喷嘴喷入喷雾塔，其中疏水二氧化硅在60℃流态化。将仍然潮湿的颗粒在60℃的空气入口温度，在流化床内进一步干燥5小时。确定了颗粒的宽的粒径分布(图3)，在约500μm具有最大值，以及高比例的空腔，基于颗粒的总体积。
实施例1A中空心球体比例的测定
在15mL离心管中装入4mL制备的颗粒。然后将正戊烷加入到管中，直到达到12mL的体积。将管密封并且摇动直到颗粒从底部完全搅拌上来。然后将管放置在直立位置，并且在5分钟后测量测量值。
空心球体的量以毫米级读出，并且以毫米表示。
对于实施例1A，一式三份测量，平均值为6.2mm。
创造性实施例1B
实施例1B类似于实施例1A进行，区别在于在0.5bar的压力下使用振动喷嘴。所用的装置是具有200μm的喷嘴开口的Buchi Encapsulator B-390，频率为1400Hz。通过喷嘴实现的流速为每小时30g。确定了颗粒的窄的粒径分布(图3)，在约400μm具有最大值，以及非常低比例的空腔，基于颗粒的总体积。
实施例1B中空心球体比例的测定
根据实施例1A的试验方法确定了实施例1B的空心球体的量。
对于实施例1B，一式三份测量，平均值为0mm。
斑蝥黄稳定性试验
在预混合应力试验中试验了由此制备的颗粒的稳定性。对于该目的，将每种情况下制备的25mg颗粒和4g预混合的混合物的试验样品称重到50mL玻璃瓶中。预混合的混合物由20％的小麦粗粉麸皮、20％的在二氧化硅上负载的50％氯化胆碱和10％的微量元素混合物组成。微量元素混合物由46.78％的FeSO4×7H2O、37.43％的CuSO4×5H2O、11.79％的ZnO、3.61％的MnO和0.39％的CoCO3组成。加入所有成分后，将试验样品小心地用手混合。这些试验样品在40℃和70％的气候室中储存4周。在储存开始前和储存完成后，测定试验样品的斑蝥黄含量。从储存后和储存前的斑蝥黄含量的比例计算保留。
实施例的保留值在下图中显示。
名称 保留(％)
1A 25
1B 86
保留越高，颗粒或其制剂的稳定性越好。如果将本发明实施例的颗粒的稳定性与相应的非创造性实施例进行比较，则稳定性的改善是非常明显的。

Claims (18)

1.制备球形颗粒的方法，所述球形颗粒包含类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸，其中类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸分散在包含至少一种水胶体的溶液中，并且液滴由喷嘴形成的分散体制备，其中分散体液滴由振动激发产生，并且将液滴通过蒸发溶剂固化和干燥。
2.权利要求1的方法，其中喷嘴和/或分散体和/或包含分散体的储存容器和/或供给分散体给喷嘴的供给线被振动激发。
3.权利要求1或2的方法，其中振动激发是范围为50至10 000Hz，优选范围为100至5000Hz并且特别优选范围为400至4000Hz的振动的叠加频率。
4.上述权利要求中任一项的方法，其中被液滴化的分散体在40℃具有≥80mPas的粘度。
5.上述权利要求中任一项的方法，其中类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸均匀地分布在颗粒的水胶体基质中。
6.上述权利要求中任一项的方法，其中封闭在颗粒中的空腔体积为≤40％，优选≤30％，并且特别优选≤20％的颗粒总体积。
7.上述权利要求中任一项的方法，其中颗粒的粒度分布在范围为150至600μm大于75％，优选在范围为150至600μm大于85％，并且特别优选在范围为150至600μm大于95％。
8.上述权利要求中任一项的方法，其中以X90-X10除以X50测量的多分散性小于1.0，优选小于0.8，并且特别优选小于0.6。
9.上述权利要求中任一项的方法，其中水胶体选自植物胶、改性植物胶、明胶、改性明胶、改性淀粉、木素磺酸盐、壳聚糖、角叉菜胶、酪蛋白、酪蛋白酸盐、乳清蛋白质、玉米醇溶蛋白、改性纤维素、果胶、改性果胶、植物蛋白质和改性植物蛋白质或其混合物。
10.上述权利要求中任一项的方法，其中类胡萝卜素和/或维生素和/或ω-3脂肪酸和/或植物甾醇和/或共轭亚油酸选自维生素A、D、E或K或其衍生物，例如维生素A和维生素E的酯，例如乙酸视黄酯或乙酸生育酚酯、生育三烯酚、维生素K1、维生素K2，以及类胡萝卜素，例如β-胡萝卜素、斑蝥黄、虾青素、桔黄质和酯衍生物、玉米黄质和酯衍生物、叶黄素和酯衍生物、番茄红素和阿朴胡萝卜素醛。
11.上述权利要求中任一项的方法，其中被液滴化的分散体包含至少一种抗氧化剂，所述的抗氧化剂选自dl-α-生育酚、d-α-生育酚、β-生育酚、γ-生育酚、δ-生育酚、丁基羟基甲苯(BHT)、丁基羟基茴香醚、没食子酸丙酯、没食子酸辛酯、没食子酸十二酯、迷迭香提取物、绿茶提取物和其它没食子酸衍生物、叔丁基羟基喹啉、乙氧喹啉、鼠尾草酚、鼠尾草酸、抗坏血酸棕榈酸酯和抗坏血酸硬脂酸酯或其混合物。
12.上述权利要求中任一项的方法，其中被液滴化的分散体包含油，所述的油选自芝麻油、玉米胚芽油、棉籽油、大豆油、花生油、葵花籽油、菜籽油、椰子油、棕榈油、橄榄油和动物脂肪、猪油和牛油、改性油或其混合物。
13.上述权利要求中任一项的方法，其中被液滴化的分散体包含至少一种软化剂，所述的软化剂选自糖或糖醇，例如蔗糖、葡萄糖、葡萄糖糖浆、乳糖、海藻糖、转化糖和其它葡萄糖-果糖组合物、山梨醇、甘露醇、甘油、麦芽糊精、异麦芽糖或异麦芽酮糖醇。
14.上述权利要求中任一项的方法，其中通过振动激发产生的液滴被粉剂包裹，随后固化并且干燥。
15.上述权利要求中任一项的方法，其中产生的液滴在温度为10至80℃被粉剂包裹，随后在40至120℃的进料空气温度固化并且干燥。
16.权利要求14或15的方法，其中粉剂选自疏水性二氧化硅、亲水性二氧化硅、淀粉、改性淀粉、玉米淀粉、纤维素、改性纤维素、硅酸钙、硅酸钙镁、碳酸钙、磷酸三钙、己二酸钙、己二酸镁、二氧化钛、木质素、高度分散的果胶、改性果胶、植物蛋白质、改性的植物蛋白质和它们的组合。
17.通过权利要求1至16的方法可获得的制剂形式。
18.权利要求17的制剂形式作为食物补充剂、食物、饲料、身体护理产品和药物的用途。
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