CN114886122B - 一种改善性能的维生素e粉的制备方法 - Google Patents

一种改善性能的维生素e粉的制备方法 Download PDF

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CN114886122B
CN114886122B CN202210518283.3A CN202210518283A CN114886122B CN 114886122 B CN114886122 B CN 114886122B CN 202210518283 A CN202210518283 A CN 202210518283A CN 114886122 B CN114886122 B CN 114886122B
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单伟达
刘建刚
丁化
郭阳
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Zhejiang Garden Nutrition Technology Co ltd
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Abstract

本发明涉及一种维生素E粉及其制备方法，通过对制备方法和生产工艺的改进，实现了水溶性和稳定性很好的均衡，明显优于现有技术常用的制备工艺制备的维生素E粉。

Description

一种改善性能的维生素E粉的制备方法
技术领域
本发明涉及生物医药以及食品饲料领域，具体涉及一种改善性能的维生素E粉的制备方法。
背景技术
维生素E(VE)是生育酚类物质的总称，是一种金黄色或者淡黄色的油状物，带有温和的特殊气味。通常维生素E在光照下遇空气易被氧化而呈现暗红色。它可与丙酮、氯仿、乙醚或者植物油混溶，几乎不溶于水。维生素E是最早发现的维生素之一，它是一种人体必需的脂溶性维生素，作为一种优良的抗氧化剂和营养剂，被广泛应用于临床、医药、食品、饲料、保健品和化妆品等行业。前维生素E在饲料添加剂中用量最大。1KG饲料中需200-300g左右VE用于拌料。维生素E添加剂的缺失会导致动物不孕、白肌病、营养性肌萎缩、肝脏坏死、生长不良、营养不足等。
天然存在的维生素E有四种生育酚(tocopherol)和四种生育三烯酚(tocotrienol)共八种类似物，其中α-生育酚含量最高，生理活性也最高。
维生素E具有多种生物活性,对一些疾病有防治作用。它是一种很强的抗氧化剂,可通过中断自由基的连锁反应保护细胞膜的稳定性,防止膜上脂褐素形成而延缓机体衰老；可通过维持遗传物质的稳定和防止染色体结构变异,调节机体代谢活动有条不紊地进行,也起到延缓衰老的作用；可阻止体内各种组织中致癌物的形成,激发机体的免疫系统,杀死新产生的变形细胞,还能将某些恶性肿瘤细胞逆转为正常表现形的细胞；具有维持结缔组织弹性,促进血液循环；调节体内激素正常分泌；控制体内酸素消耗；保护皮肤粘膜等功能,使皮肤滋润健美,从而达到美容护肤的作用；还可改善头发毛囊微循环,保证其营养供应,使头发再生。另研究表明,维生素E还能阻止LDL胆固醇氧化,而避免冠状动脉硬化。此外维生素E可防止白内障发生；延缓早老性痴呆；维持正常的生殖机能；保持肌肉和外周血管结构与功能的正常状态；治疗胃溃疡；保护肝脏；调节血压；辅助治疗II型糖尿病；与其它维生素具有协同等作用。
由于维生素E容易被氧化，目前最常用的维生素E为维生素E醋酸酯，其也叫做乙酸维生素E，是一种干维生素E形式。该醋酸酯形式比未酯化维生素E更稳定。干性维生素E醋酸酯和油脂形式维生素E的不同之处是后者没有即时抗氧化特性。
目前上市的维生素E的制剂有不同的类型，可以是液体或固体。维生素E粉可以用于配置多种固体组合物，常备用于制备食品、饲料、个人护理产品等。
维生素E粉最常见的制备方法为将维生素E与吸附剂在流化床中以含水悬浮液造粒如(EP1018303A)。将维生素E醋酸酯与明胶、淀粉、吐温等成分，以二氧化硅或硬脂酸镁通过超高压微射流分散技术使得乳液粒径更细，喷雾干燥得到干粉(CN106256346A)。在减压条件下将二氧化硅与预热的维生素E油混合搅拌制备得到维生素E粉(CN101346129A.)。
虽然现有技术中有多个研究维生素E粉的制备工艺研究，但是没有研究如何提高维生素E的稳定性和水溶性。
发明内容
本发明提供一种维生素E粉的制备方法，为物理混合，避免了现有技术中一般采用的喷雾制粒的方法、避免了水、有机溶剂的加入，减少了工艺步骤。而且与喷雾制粒方法相比，直接物理混合制粒的方法，可以极大提高水溶性、高湿以及极端情况下(高温高湿)的稳定性。
本发明提供一种维生素E粉的制备方法，其特征在于在溶油釜中加入300-500质量份DL-α-生育酚乙酸酯、30-60质量份的PEG4000和10-20质量份聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与350-500质量份二氧化硅在机械化学力的作用下实现有效地吸附；之后，将100-200质量份DL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉；所述维生素E粉90％可以通过孔径为0.84mm分析筛；DL-a-生育酚乙酸酯含量≥50.0％；重金属≤10mg/kg；总砷(As)≤3mg/kg。
如上所述的制备方法，其特征在于：PEG4000与PVPK90的比例为3:1.
如上所述的制备方法，其特征在于：非氧气体为氮气、惰性气体、二氧化碳中的一种或多种。
如上所述的制备方法，其特征在于还包括检测和包装步骤，取样检测合格后进行混批，检测合格后经过金属探测、包装、入库。
如上所述的制备方法，其特征在于在溶油釜中加入400质量份DL-α-生育酚乙酸酯、45质量份的PEG4000和15质量份聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与403质量份二氧化硅在机械化学力的作用下实现有效地吸附；之后，将137质量份DL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉。
如上所述的制备方法，其特征在于在溶油釜中加入400kgDL-α-生育酚乙酸酯、45kg的PEG4000和15kg聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与403kg二氧化硅在机械化学力的作用下实现有效地吸附；之后，将剩余的137kgDL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉。
本发明还提供了一种维生素E粉，其特征在于由以上制备工艺制备得到。
本发明中的维生素E粉，为物理混合，避免了现有技术中一般采用的喷雾制粒的方法、避免了水、有机溶剂的加入，减少了工艺步骤。而且与喷雾制粒方法相比，直接物理混合制粒的方法，可以极大提高水溶性、高湿以及极端情况下(高温高湿)的稳定性。而且通过工艺的改进，将DL-α-生育酚乙酸酯分成2批，大部分与增溶成分PEG4000和聚乙烯吡咯烷酮K90混合；最后再加入剩余的DL-α-生育酚乙酸酯进行吸附。通过该操作，可以提升维生素E粉的稳定性。可以在保证提高水溶性的前提下，保持高湿以及极端情况下(高温高湿)的稳定性。
附图说明
图1：工艺流程图
具体实施方式
实施例1：
在溶油釜中加入537kgDL-α-生育酚乙酸酯，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与463kg二氧化硅在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉，取样按维生素E粉质量标准进行检测，粒度为90％通过孔径为0.84mm分析筛。
对比实施例1：
在溶油釜中加入537kgDL-α-生育酚乙酸酯，在氮气保护下搅拌升温预热，达到熔融状态；将二氧化硅加入流化床中，温度升高到50-60℃，通过喷嘴将预热过的DL-α-生育酚乙酸酯喷到流化床的二氧化硅上，并混合干燥得到最终的维生素E粉。经检测粒度为90％通过孔径为0.84mm分析筛。
对实施例1和对比实施例1的维生素E粉进行检测，得到如下数据：
通过上述实验可以看出，采用本专利中的机械化学方法制备得到的维生素E粉高温稳定性以及强光照稳定性与常规喷雾方法相仿，略有优势。在高湿环境下(90％±5％，10天)和破坏性实验(90％±5％，10天)中，稳定性更好。因此，具有显著优势。采用本专利中的机械化学方法制备得到的维生素E粉与常规制备方法制备得到的维生素E粉水溶性稍有提升，但是不是非常明显。因此，采用本专利中的机械化学方法，可以很好改善维生素E粉对抗高湿和极端高温高湿的环境，且其水溶性也具有一定的改善。
实施例2：改善维生素E粉的水溶性实验
改善物质水溶性的一般性方法为加入增溶性物质，如PEG4000、环糊精或者将其制备成固体分散体等。为此，进行文献查询，CN101084880A中通过将维生素烟酸酯与PEG4000或者PVP制备成固体分散体，从而可以改善维生素烟酸酯的体外溶出速率和体内吸收程度。但是其实施例1-2中通过加入维生素烟酸酯的2倍量的PEG4000和1.5倍量的PVP。但是这样就无法保证可以制备50％含量以上的维生素E粉。因此，这两种方案是行不通的。为此，对配方进行改进和筛选，进行正交实验筛选，在配方中分别加入10、20、30、40、50、60kg的PEG4000、磺丁基-β-环糊精、聚乙烯吡咯烷酮K90、吐温80或其二者的组合辅料。具体制备工艺为：在溶油釜中加入537kgDL-α-生育酚乙酸酯和相应的增溶物质，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与余量的二氧化硅(总计为1000kg)在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉。
通过实验发现，加入60kg的PEG4000和聚乙烯吡咯烷酮K90在3:1的情况下，可以极大增加水溶性，可以达到43μg/mL。但是会使高湿情况下和破坏性实验中的稳定性下降，分别下降至91.1％和87.64％。因此，需要考虑如何在保持增加水溶性的情况下，改善其稳定性。
实施例3：改善维生素E粉的稳定性实验
在不断筛选和实验过程中发现，。
其制备方法如下：
在溶油釜中加入400kgDL-α-生育酚乙酸酯、45kg的PEG4000和15kg聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态。将其加入球磨机中与403kg二氧化硅在机械化学力的作用下实现有效地吸附。之后，将剩余的137kgDL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附；经过筛得到维生素E粉，并采样测试其水溶性和稳定性。
因此，通过工艺的改进，将DL-α-生育酚乙酸酯分成2批，大部分与增溶成分PEG4000和聚乙烯吡咯烷酮K90混合；最后再加入剩余的DL-α-生育酚乙酸酯进行吸附。通过该操作，可以提升维生素E粉的稳定性。且取样按维生素E粉进行检测，混批均匀后按维生素E粉成品质量标准进行检测。经检测，干燥失重≤5％；粒度为90％通过孔径为0.84mm分析筛；重金属≤10(mg/kg)；总砷(As)≤3(mg/kg)。
以上描述是本发明的一般性描述。根据情况或实际需要，可进行形式的变化和等值的替代，虽然本文采用特定的术语，但这些术语意在描述，而不是为了限制的目的。本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围之内。

Claims (4)

1.一种维生素E粉的制备方法，其特征在于在溶油釜中加入300-500质量份DL-α-生育酚乙酸酯、30-60质量份的PEG4000和10-20质量份聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与350-500质量份二氧化硅在机械化学力的作用下实现有效地吸附；之后，将100-200质量份DL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉；所述维生素E粉90％可以通过孔径为0.84mm分析筛；DL-α-生育酚乙酸酯含量≥50.0％；重金属≤10mg/kg；总砷(As)≤3mg/kg；
所述PEG4000与PVPK90的比例为3:1。
2.如权利要求1所述的制备方法，其特征在于还包括检测和包装步骤，取样检测合格后进行混批，检测合格后经过金属探测、包装、入库。
3.如权利要求1所述的制备方法，其特征在于在溶油釜中加入400质量份DL-α-生育酚乙酸酯、45质量份的PEG4000和15质量份聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与403质量份二氧化硅在机械化学力的作用下实现有效地吸附；之后，将137质量份DL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉。
4.如权利要求1所述的制备方法，其特征在于在溶油釜中加入400kgDL-α-生育酚乙酸酯、45kg的PEG4000和15kg聚乙烯吡咯烷酮K90，在氮气保护下搅拌升温预热，达到熔融状态；将其加入球磨机中与403kg二氧化硅在机械化学力的作用下实现有效地吸附；之后，将剩余的137kgDL-α-生育酚乙酸酯在氮气保护下搅拌升温预热，达到熔融状态；加入上述球磨机中继续在机械化学力的作用下实现有效地吸附，经过筛得到维生素E粉。
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