CN110693848B - 无抗氧化剂的维生素a微囊制剂及其制备方法 - Google Patents
无抗氧化剂的维生素a微囊制剂及其制备方法 Download PDFInfo
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Abstract
无抗氧化剂的维生素A微囊制剂及其制备方法,所述的制备方法包括原料准备、制备水相、油相、乳液制备及喷雾干燥等步骤,所述的原料物按照质量份含有:维生素A 50‑70份,辛烯基琥珀酸淀粉钠5‑25份,***胶5‑20份,维生素E琥珀酸聚乙二醇酯1‑5份,酸度调节剂0.1‑2份,葡萄糖氧化酶0.1‑1份,抗结剂0‑1.5份。本发明采用微囊化工艺对维生素A进行包埋,通过喷雾干燥,得到无抗氧化剂、高载油、高包埋率、高生物利用度和高稳定性的维生素A微囊粉。
Description
技术领域
本发明属于微囊技术领域,尤其涉及一种无抗氧化剂高生物利用度高稳定性的维生素A微囊制剂制备方法。
背景技术
维生素A是第一个被发现,也是一种极其重要、极易缺乏的,为人体维持正常代谢和机能所必需的脂溶性维生素。维生素A并不是单一的化合物,而是一系列包括视黄醇、视黄醛、视黄酸、视黄醇乙酸酯和视黄醇棕榈酸酯等在内的视黄醇的衍生物。
维生素A属于脂溶性维生素,可以不同程度地溶于大部分有机溶剂,但不溶于水。维生素A及其衍生物很容易被氧化和异构化,特别是在暴露于光线(尤其是紫外线)、氧气、性质活泼的金属以及高温环境时,可加快这种氧化破坏。但一般烹调过程不至于对食物中的维生素A造成太多破坏。在理想条件下,如低温冷冻等,血清、组织或结晶态的类视黄醇可保持长期稳定。在无氧条件下,视黄醛对碱比较稳定,但在酸中不稳定,可发生脱氢或双键的重新排列。油脂在酸败过程中,其所含的维生素A和胡萝卜素会受到严重的破坏。
因而很多企业、科研院所等都对维生素A的稳态化制剂进行研究开发,希望让维生素A更加稳定。
CN201010101199.9公开了一种连续化稳定维生素A微胶囊的制备方法,在氮气保护下,将维生素A晶体与抗氧剂按比例连续加到结晶熔化器中,配成含抗氧剂的维生素A熔油;然后用泵将上述熔油送入带有液体分布器的超重力旋转填充床乳化器中,同时将含有可凝胶化改性淀粉的水溶液经脱氧处理后用泵送入上述超重力旋转填充床乳化器,在出口得到维生素A乳化液;将该乳化液连续雾化喷入冷却的淀粉床中进行造粒,然后在氮气作干燥介质的流化床中进行流态化干燥、凝胶化处理,即得到稳定维生素A微胶囊。本发明的优点是可连续生产,并且由于采用可凝胶化改性淀粉和造粒、凝胶化处理,其包埋效果好,因而产品的贮存稳定性好。
CN201110142580.4公开一种用于饮料的维生素A微胶囊营养强化剂的制备方法,该专利主要采用酪朊酸钠作为主壁材对VA棕榈酸酯进行包埋,采用小分子麦芽糊精和白砂糖进行填充,主要重点强调了生产过程无氧、填补保护气体和产品的稳定性。
CN201710637373.3公开了一种脂溶性营养素微胶囊及其制备方法,该脂溶性营养素微胶囊的制备方法包括乳化和制粒过程,其中,乳化是在空化乳化器中进行,通过该制备方法可以使脂溶性营养素微胶囊的营养素活性物质损失少,并且稳定性高。
CN201811312455.1公开了辛烯基琥珀酸淀粉酯、脂溶性营养素微胶囊及制备方法和应用,辛烯基琥珀酸淀粉酯的制备方法包括:将糊化淀粉和辛烯基琥珀酸酐在空化乳化过程中发生酯化反应,得到所述辛烯基琥珀酸淀粉酯。该制备方法通过空化乳化过程促进和强化了酯化反应,使得糊化状态下的淀粉与辛烯基琥珀酸酐因分子碰撞加剧而在淀粉的结晶区和无定形区均发生显著的取代,进而提高了制得的辛烯基琥珀酸淀粉酯的酯化率,因此大大提高了乳化性能。且该方法快速高效,酯化后无需进行水解步骤,避免了水解导致分子链被不同程度破坏、直链淀粉的链长和含量显著降低进而导致辛烯基琥珀酸淀粉酯成膜的致密度降低、易吸潮、易脆及易导热的问题,提高了其应用性能。
CN109452467 A公开了一种维生素A微胶囊及其制备方法和应用,该发明中,使用抗坏血酸棕榈酸酯和鼠尾草酸在胆碱和/或胆碱衍生物预处理后作为抗氧化剂,各组分之间对维生素A在饲料或饲料预混料中的稳定性起到了预料不到的协同作用。还发现,维生素A在pH值介于6.0~7.5之间时可保持最佳稳定性,因此本发明在所述维生素A微胶囊的制备过程中,将维生素A乳液的pH值控制在介于6.0~7.5之间能够为维生素A提供最佳的存储环境。
还有很多现有研究结果也公开了维生素A的微囊化制备方法,但这些现有技术都是靠抗氧化剂等提高维生素A的稳定性。并且,虽然微囊化之后的维生素A稳定性有改善,但并没有现有技术公开其生物利用度的相关数据。包埋稳定虽是我们追求的目标,但过度包埋是否会影响维生素A在体内的代谢也是我们更关注的问题。
发明内容
本发明的目的在于提供稳定包埋、且具有优异释放代谢特征的维生素微囊制剂,并期望通过组分优化调整的手段替代抗氧化剂的使用来实现制剂的稳定化处理。为此,本发明首先提供一种无抗氧化剂的维生素A微囊制剂的制备方法,包括如下步骤:
(1)准备原料物,所述原料物按照质量份含有下述组分:
(2)60-80℃下将变性淀粉和***胶依次分散于水中,搅拌至完全溶解,降温至30-40℃备用;
(3)取酸度调节剂加入到步骤(2)所得的体系中,控制pH在6-8,搅拌均匀,再加入葡萄糖氧化酶,得到水相;
(4)将维生素E琥珀酸聚乙二醇酯加入到维生素A中,在60-80℃下加热融化,搅拌混合均匀,降温至30-40℃,得到油相;
(5)将油相缓慢加入到水相中,30-40℃搅拌至混合均匀;
(6)步骤(5)所得混合物剪切乳化0.5-1h,然后于40-70MPa高压均质2次得乳液;
(7)将步骤(6)所制备的乳液喷雾干燥:进风温度80-210℃,出风温度70-120℃;产物过筛后与抗结剂均匀混合。
本发明采用微囊化工艺对维生素A进行包埋,通过特定的物料组合及制剂工艺获得无抗氧化剂、高载油、高包埋率、高生物利用度和高稳定性的维生素A微囊粉产品。可广泛应用于饲料、膳食补充剂、日化、医药等领域。
具体实施方式
本发明提供一种不依赖抗氧化剂实现高稳定性的高生物利用度高维生素A微囊制剂。原料的选择与组合、以及与其所适应的操作方案是本发明实现其技术效果的核心技术手段。所述微囊制剂产品的制备方法中,原料物按照质量份含有维生素A 50-70份、变性淀粉5-25份、***胶5-20份、维生素E琥珀酸聚乙二醇酯1-5份、葡萄糖氧化酶0.1-1份、酸度调节剂0.1-2份以及抗结剂0-1.5份。
原料物中所述的维生素A通常为晶体,选自选自维生素A醋酸酯、维生素A棕榈酸酯或其混合物。
原料物中所述的变性淀粉选自辛烯基琥珀酸淀粉钠、乙酰化双淀粉、羧基淀粉、磷酸化淀粉中的一种或几种混合物。优选辛烯基琥珀酸淀粉钠和磷酸化淀粉。
原料物中所述的酸度调节剂选自碳酸氢钠、氢氧化钠、碳酸钠、氢氧化钙、氢氧化钾中的一种或几种的混合物。优选自碳酸氢钠、氢氧化钙和氢氧化钠。
原料物中所述的抗结剂选自二氧化硅、硅酸钙和磷酸三钙。
容易理解,上述优选的技术特征可以组合构成本发明的优选技术方案,如实施例中所证明的,辛烯基琥珀酸淀粉钠和***胶共同与维生素E琥珀酸聚乙二醇酯作用可以得到本发明所述的高包埋率、高稳定性和高生物利用度的产品。
下面通过非限制性实施例进一步说明本发明的技术方案及效果,不应当被理解为对发明内容任意形式的限定。如无特殊说明,本说明书中的百分比均表示质量百分比。
实施例1
称取409g水于1000mL烧杯中,水温62℃,向其中加入125g辛烯基琥珀酸淀粉钠和100g***胶,搅拌至完全溶解,温度降至35℃备用。将6g碳酸氢钠加入水相中,控制pH在6.8~7.1,再加入4g葡萄糖氧化酶。将7.5g维生素E琥珀酸聚乙二醇酯和252.5g维生素A醋酸酯混合,放入75℃水浴中融化,搅拌均匀,降温至35℃得到油相。将油相缓慢倒入水相中,35℃下剪切乳化0.5h,40MPa高压均质2次,然后进行喷雾干燥,进风温度170℃,出风温度84℃。过筛,加入二氧化硅,得到维生素A醋酸酯微囊粉,记作样品1。
实施例2
称取1000g水于2000mL烧杯中,水温65℃,向其中加入200g辛烯基琥珀酸淀粉钠和150g***胶,搅拌至完全溶解,温度降至38℃备用。将5g氢氧化钙加入水相中,控制pH在6.9~7.5,再加入10g葡萄糖氧化酶。将20g维生素E琥珀酸聚乙二醇酯和605g维生素A醋酸酯混合,放入80℃水浴中融化,搅拌均匀,降温至38℃得到油相。将油相缓慢倒入水相中,38℃下剪切乳化0.5h,55MPa高压均质2次,然后进行喷雾干燥,进风温度180℃,出风温度90℃。过筛,加入二氧化硅,得到维生素A醋酸酯微囊粉,记作样品2。
实施例3
称取2000g水于3000mL烧杯中,水温75℃,向其中加入240g磷酸化淀粉和260g***胶,搅拌至完全溶解,温度降至40℃备用。将4g氢氧化钠加入水相中,控制pH在7.0~7.3,再加入16g葡萄糖氧化酶。将60g维生素E琥珀酸聚乙二醇酯和1400g维生素A棕榈酸酯混合,放入69℃水浴中融化,搅拌均匀,降温至40℃得到油相。将油相缓慢倒入水相中,40℃下剪切乳化1h,50MPa高压均质2次,然后进行喷雾干燥,进风温度175℃,出风温度87℃。过筛,加入二氧化硅,得到维生素A醋酸酯微囊粉,记作样品3。
实施例4
对样品1、样品2和样品3进行产品性能评价,结果如表1:
表1
名称 | 外观 | 滋气味 | 包埋率 | 堆密度 | 粒度 | 冲调性 |
样品1 | 橙黄色粉末 | 固有滋气味 | 99.2% | 0.43g/ml | ≥95%过40目筛 | 乳液均一 |
样品2 | 橙色粉末 | 固有滋气味 | 98.9% | 0.40g/ml | ≥95%过40目筛 | 乳液均一 |
样品3 | 橙色粉末 | 固有滋气味 | 99.3% | 0.38g/ml | ≥95%过40目筛 | 乳液均一 |
从结果可以看出,用本专利公开的工艺得到的维生素A微囊粉,产品包埋率高、冲调性好、堆密度与粒度适宜,这些性状指标均表明该产品具有优异的特性,可广泛用于饲料、膳食补充剂、日化、医药等领域。
实施例5
将样品1、样品2和样品3放入40℃75%湿度的加速烘箱中进行三个月的产品稳定性评价,结果如表2:
表2
从加速稳定性实验可以看出,加速3个月后三个样品的外观、滋气味、包埋率、冲调性均没有发生变化,维生素A保留率略有降低,但一般认为加速三个月保留率≥90%产品为合格。可见本专利公开的工艺制备出的维生素A微囊粉稳定性能优异。
实施例6
对样品1-3进行了细胞水平的生物利用度评价,结果如下:
表3
名称 | 生物利用度 |
维生素A原料 | 5.63% |
样品1 | 46.73% |
样品2 | 45.60% |
样品3 | 50.11% |
从结果可以看出维生素A原料的生物利用率仅为5.63%,而通过本专利公开的配方和工艺制得的维生素A微囊粉,其生物利用度为原料的8-9倍,大大提高了生物利用度。
实施例7
参照实施例2的配方及工艺参数,仅将辛烯基琥珀酸淀粉钠和***胶更换为其他不同种类的壁材,考察不同的壁材与维生素E琥珀酸聚乙二醇酯的组合对产品的稳定性及生物利用度的影响,结果如下:
表4
从结果可以看出只有辛烯基琥珀酸淀粉钠和***胶共同与维生素E琥珀酸聚乙二醇酯作用可以得到高包埋率、高稳定性和高生物利用度的产品。而其他壁材组合没有此效果。
实施例8
参照实施例2的配方及工艺参数,仅将维生素E琥珀酸聚乙二醇酯去掉,得到的产品包埋率为98.1%,40℃加速3个月保留率93.2%,细胞水平生物利用度为14.7%。由此可见,维生素E琥珀酸聚乙二醇酯与壁材的组合,共同保证了产品的稳定性及生物利用度,缺一不可。
Claims (6)
1.无抗氧化剂的维生素A微囊制剂的制备方法,包括如下步骤:
(1)准备原料物,所述原料物按照质量份含有下述组分:
其中,所述的变性淀粉选自辛烯基琥珀酸淀粉钠和磷酸化淀粉;
(2)60-80℃下将变性淀粉和***胶依次分散于水中,搅拌至完全溶解,降温至30-40℃备用;
(3)取酸度调节剂加入到步骤(2)所得的体系中,控制pH在6-8,搅拌均匀,再加入葡萄糖氧化酶,得到水相;
(4)将维生素E琥珀酸聚乙二醇酯加入到维生素A中,在60-80℃下加热融化,搅拌混合均匀,降温至30-40℃,得到油相;
(5)将油相缓慢加入到水相中,30-40℃搅拌至混合均匀;
(6)步骤(5)所得混合物剪切乳化0.5-1h,然后于40-70MPa高压均质2次得乳液;
(7)将步骤(6)所制备的乳液喷雾干燥:进风温度80-210℃,出风温度70-120℃;产物过筛后与抗结剂均匀混合。
2.根据权利要求1所述的方法,其特征在于,所述的维生素A选自维生素A醋酸酯、维生素A棕榈酸酯或其混合物。
3.根据权利要求1所述的方法,其特征在于,所述的酸度调节剂选自碳酸氢钠、氢氧化钠、碳酸钠、氢氧化钙、氢氧化钾中的一种或几种的混合物。
4.根据权利要求3所述的方法,其特征在于,所述的酸度调节剂选自碳酸氢钠、氢氧化钙和氢氧化钠。
5.根据权利要求1所述的方法,其特征在于,所述的抗结剂选自二氧化硅、硅酸钙和磷酸三钙。
6.权利要求1的方法制备的无抗氧化剂的维生素A微囊制剂。
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