CN112869155A - 一种叶黄素酯水分散制剂及其制备方法和应用 - Google Patents
一种叶黄素酯水分散制剂及其制备方法和应用 Download PDFInfo
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- CN112869155A CN112869155A CN202110060387.XA CN202110060387A CN112869155A CN 112869155 A CN112869155 A CN 112869155A CN 202110060387 A CN202110060387 A CN 202110060387A CN 112869155 A CN112869155 A CN 112869155A
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- lutein ester
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- water dispersible
- lutein
- oil phase
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- 238000002360 preparation method Methods 0.000 title claims abstract description 53
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Abstract
本发明涉及一种叶黄素酯水分散制剂及其制备方法和应用。该制剂由叶黄素酯晶体1‑8％，油相载体10‑25％，油相抗氧化剂0.5‑5％，复合水相载体65‑75％，水相抗氧化剂1‑3％为原料，通过加热溶解、混合搅拌、剪切乳化、纳米研磨、喷雾干燥等工艺制备获得。该制剂具有着色效果稳定，吸收好的优点，同时工艺简便，成本低。
Description
技术领域
本发明属食品着色剂、营养补充剂领域，具体涉及一种叶黄素酯水分散制剂及其制备，以及其在液体饮料中的应用。
背景技术
叶黄素酯，化学名称叶黄素二棕榈酸酯(CAS注册号：547-17-1)，是一种含氧类胡萝卜素酯，广泛存在于万寿菊花、南瓜、甘蓝、苜蓿等植物体内。叶黄素酯中的叶黄素能大量吸收近于紫外光的蓝光，保护眼睛不受光线损害，延缓眼睛的老化及防止病变，尤其能有效预防AMD(老年性视网膜黄斑退化)。另外叶黄素还具有抗氧化、抗癌、抗诱变、延缓动脉硬化等生理功能，是一种天然营养健康的功能性色素。中国卫生部2007年第8号公告批准叶黄素酯为营养强化剂、着色剂和2008年第12号公告批准叶黄素酯为新食品原料。研究证实，叶黄素酯分解得到的叶黄素生物利用度，比未酯化的叶黄素高60％以上。并且，叶黄素酯对一些不利的物理、化学因素，具有更好的稳定性。但由于叶黄素酯的油溶性及难溶于水的性质，限制了其在食品等领域的应用。若将叶黄素酯的油溶性改性为水溶性，不仅可以直接应用于水基质食品、饮料中，扩大了其应用范围，还有利于人体的吸收，提高叶黄素酯的生物利用率。
现有的水溶性叶黄素酯制剂溶解后液体透明度不高，并且不稳定，久置易产生变色或沉淀。叶黄素酯常用于添加到饮料中，透明包装是饮料的常见包装，而现有水溶性叶黄素酯制剂添加后存在透明度低且不稳定的问题，顾客购买时会错以为饮料变质，对饮料的销售带来不良影响，限制了水溶性叶黄素酯添加剂在饮料领域的应用。
CN 201310194981公开了一种水溶性叶黄素酯制备方法，将叶黄素酯与乳化剂、抗氧化剂充分混匀得到混合物，将所述混合物真空干燥；其中，所述乳化剂为分子蒸馏单甘脂、聚甘油脂肪酸酯、三聚甘油单硬脂酸酯、聚甘油蓖麻醇酯、双乙酰酒石酸单双甘油酯、聚乙二醇300、聚乙二醇400、聚乙二醇600中的1-3种。但该发明粉末干燥方式为真空干燥，与喷雾干燥相比设备投资费用高，生产效率低，不易大规模生产；且配方中未加入阿拉伯胶等增稠剂作为高分子包埋材料，产品稳定性较差。
CN 201310117340公开了一种叶黄素酯纳米颗粒及其制备方法:加热条件下包裹材料(环糊精/羟甲基纤维素钠/聚维酮/聚乙二醇/甘露糖/半乳糖/胆酸)溶于有机溶剂中，叶黄素酯加热溶解在同种溶剂中(丙酮/甲醇/乙醇/乙酸乙酯)中，在将叶黄素酯乳化，挥干溶剂成型的方法制备叶黄素酯纳米制剂。但该工艺在制剂化过程中使用有毒有机溶剂，大大限制其在食品领域中的应用。
CN 201310194981公开了一种水溶性叶黄素酯制备方法，将油溶性叶黄素酯与乳化剂、抗氧化剂充分混匀得到混合物，将所述混合物真空干燥，最终得到水溶性叶黄素酯。但是该水溶性叶黄素酯为制备硬糖的添加成分，因此不能解决在叶黄素酯制剂液体饮料中的稳定性问题。
CN 201810352049.1公开了一种叶黄素/叶黄素酯微粒及其制备方法，通过将含有叶黄素和/或叶黄素酯、壁材以及助乳化剂的原料混合物在低温条件下制备成粒径不超过1微米的纳米乳液，再喷涂至蔗糖-淀粉颗粒上制备。所述的壁材是纤维素衍生物。
CN 202010304096.6公开了一种叶黄素酯水溶颗粒及其制备方法，将叶黄素酯、乳化剂、抗氧化剂、载体分别粉碎、过筛；混合加热到55-80℃，100-150℃温度加入热熔挤出机中挤出，冷却、粉碎、过筛后获得叶黄素酯水溶颗粒。颗粒在水溶液中稳定性高，久置不易产生浑浊沉淀变色。但该发明中制备过程中多次设计高温工艺，可能会对产品含量产生影响；且仅考察制剂在水中稳定性，并未真正考察其在终端产品中的应用。
目前已公开的文献中记载的叶黄素酯制剂多以追求水溶性为目的，但在制备过程中有的会涉及到有机溶剂，有的工艺相对复杂，并且均未对叶黄素酯制剂在终端饮料产品中的应用稳定性加以考察和关注。
发明内容
本发明所要解决的技术问题是提供一种应用于饮料中透明度高、无沉淀且色调稳定的叶黄素酯水溶性制剂及其制备方法，该制剂可应用于多类液体饮料中用于着色剂，例如特殊用途饮料(品)、果汁(浆)及果汁饮料(品)、蔬菜汁及蔬菜汁饮料(品)以及茶饮料(品)类等。本发明通过对各原料的组成进行全面优化，尤其是对原料中各组分相对含量进行控制，可以确保采用所述原料制备得到的着色剂具有良好的色调。不但能够起到稳定的着色效果，而且吸收好，利于发挥叶黄素酯的保健活性；同时工艺简便，成本低。
具体而言，本发明的制剂原料包含；叶黄素酯晶体、油相载体、油相抗氧化剂、复合水相载体、水相抗氧化剂。
本发明优选所述原料包括如下重量份的成分：叶黄素酯晶体1-8％，油相载体10-25％，油相抗氧化剂0.5-5％,复合水相载体65-75％，水相抗氧化剂1-3％。
本发明所述油相载体可选用本领域常规的食品用分子蒸馏单甘酯、辛癸酸甘油酯、三聚甘油单硬脂酸酯或乙酰化单、双甘油脂肪酸酯中的一种或多种。其中，优选分子蒸馏单甘酯。
本发明所述水相载体可选用具由空间网状结构的增稠剂、麦芽糊精和蔗糖组成的载体。其中优选增稠剂占原料质量百分比25-45％，麦芽糊精和蔗糖质量比为2:1-1:1。所述增稠剂可选自但不限于辛烯基琥珀酸淀粉钠、海藻酸钠、β-环糊精、黄原胶或阿拉伯胶。
本发明在配方中加入抗氧化剂可以使所述着色剂具有抗氧化功能。所述特定比例的抗氧化剂可以与叶黄素酯协同作用，使着色剂具有良好的稳定性。所述水相载体抗氧化剂可选用本领域常用的可食用抗氧化剂，如L-抗坏血酸、D-异抗坏血酸钠、抗坏血酸钠、茶多酚中的一种或多种，所述油相载体抗氧化剂可选用GB1886.233《食品安全国家标准食品添加剂维生素E》中的任意一种或多种，优选维生素E。
本发明同时提供了叶黄素酯水分散制剂的制备方法。具体而言，所述制剂是将原料混合后，经乳化、研磨、喷雾而成。
本发明提供的所述的叶黄素酯水分散制剂的制备方法，包括如下步骤：
1)按质量占比将叶黄素酯、油相载体，油相抗氧化剂混合，加热至65-80℃，得到油相；
2)按质量占比将复合水相载体、水相抗氧化剂混合，65-80℃加热搅拌溶解，得到水相；
3)5000-9000rpm条件下剪切乳化，将油相缓慢加入水相中获得制剂初乳液。
4)初乳液经过纳米研磨后，进行喷雾干燥，获得所述叶黄素酯水分散制剂。
更进一步，所述的叶黄素酯水分散制剂的制备方法中步骤4)所述纳米研磨工艺为：首先采用0.4-0.6mm粒径氧化锆球将料液粒径研磨至＜0.3μm后，再用0.2-0.3mm粒径氧化锆球继续研磨料液，使得料液平均粒径＜0.1μm。
上述料液粒径均的测定均通过Nano ZS型号纳米粒度及Zeta电位分析仪进行测量。
本发明的有益效果：
本发明通过水相载体与油相载体的选择，以及串联研磨工艺，获得的叶黄素酯水分散制剂水溶性好，可应用于多种类型的液体饮料中的着色。着色后的饮料透明度高，货架期放置90天无沉淀，色调变化△b*小于5(色调采用分光测色计进行测定)。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1
叶黄素酯晶体25g，分子蒸馏单甘酯112.5g，辛烯基琥珀酸淀粉钠150g,麦芽糊精115g,蔗糖60g，L-抗坏血酸12.5g，维生素E 25g。
(1)将上述重量的辛烯基琥珀酸淀粉钠、麦芽糊精、蔗糖和L-抗坏血酸溶解于70℃的纯水中，制得水相；
(2)70℃条件下将叶黄素酯熔融于添加了维生素E的分子蒸馏单甘酯中；
(3)7000r/min高剪切乳化条件下将油相加入到水相中，添加完毕后继续乳化10min，得到初乳液；
(4)将初乳液用首先采用0.4-0.6mm粒径氧化锆球将料液粒径研磨至0.25μm后，更换0.2-0.4mm粒径氧化锆球继续研磨料液，料液粒径0.08μm；
(5)将研磨后乳液进行喷雾干燥，即得。
将本实施例所得叶黄素酯制剂分散于饮料中，当叶黄素酯的浓度为7.5ppm时，饮料色调值为L*91.22，a*4.69，b*49.11。
实施例2
叶黄素酯晶体300g，分子蒸馏单甘酯1350g、阿拉伯胶1800g,麦芽糊精1380g蔗糖720g，D-异抗坏血酸钠150g，混合生育酚125g。具体为：
(1)将阿拉伯胶、麦芽糊精、蔗糖混合物和L-抗坏血酸溶解于70℃的纯水中，制得水相；
(2)70℃条件下将叶黄素酯熔融于添加了混合生育酚的辛癸酸甘油酯中；
(3)7000r/min高剪切乳化条件下将油相加入到水相中，添加完毕后继续乳化10min，得到初乳液；
(4)将初乳液用首先采用0.4-0.6mm粒径氧化锆球将料液粒径研磨至0.25μm后，更换0.2-0.4mm粒径氧化锆球继续研磨料液，料液粒径0.08μm；
(5)将处理后乳液进行喷雾干燥，即得。
将本实施例所得叶黄素酯制剂分散于饮料中，当叶黄素酯的浓度为24ppm时，饮料色调值为L*90.06，a*3.25，b*47.66。
实施例3
叶黄素酯晶体1kg,分子蒸馏单甘酯4.5kg,阿拉伯胶1.8kg,麦芽糊精4.6kg,蔗糖＝2.4kg，L-抗坏血酸500g，维生素E1kg。
具体为：
(1)将阿拉伯胶、麦芽糊精、蔗糖、L-抗坏血酸溶解于70℃的纯水中，制得水相；
(2)70℃条件下将叶黄素酯熔融于添加了L-抗坏血酸的三聚甘油单硬脂酸酯中；
(3)8000r/min高剪切乳化条件下将油相加入到水相中，添加完毕后继续乳化10min，得到初乳液；
(4)将初乳液用首先采用0.4-0.6mm粒径氧化锆球将料液粒径研磨至0.25μm后，更换0.2-0.4mm粒径氧化锆球继续研磨料液，料液粒径0.08μm。；
(5)将研磨后乳液进行喷雾干燥，即得
将本实施例所得叶黄素酯制剂分散于饮料中，当叶黄素酯的浓度为24ppm时，饮料色调值为L*92.87，a*3.19，b*47.37。
对比例1
叶黄素酯加热至45℃，然后向其中加入5％总量的分子蒸馏单甘脂、三聚甘油单硬脂酸酯和聚乙二醇600，以及0.3％维生素E，将混合物置于搅拌机中以300转/分转速搅拌2h，混合物充分混匀。将混匀的混合物用高速剪切均质机以3000转/分的速度，均质25分钟，得到叶黄素酯乳液，将所述乳液在55℃下真空干燥后粉碎，过100目筛，得到对比例水溶性叶黄素粉末。
对比例2
叶黄素酯加热至50℃，然后向其中加入叶黄素酯量2％的聚甘油脂肪酸酯，以及叶黄素酯量0.5％的特丁基对苯二酚，将混合物置于搅拌机中以200转/分转速搅拌2h，混合物充分混匀。将混匀的混合物用高速剪切均质机以3500转/分的速度，均质35分钟，得到叶黄素酯乳液，将所述乳液在55℃下真空干燥后粉碎，过100目筛，得到对比例水溶性叶黄素粉末。
对比例3
叶黄素酯加热至45℃，然后向其中加入叶黄素酯量5％的三聚甘油单硬脂酸酯、聚甘油蓖麻醇酯，以及叶黄素酯量0.3％的丁基羟基茴香醚和二丁基羟基甲苯，将混合物置于搅拌机中以300转/分转速搅拌3h，混合物充分混匀。将混匀的混合物用高速剪切均质机以3500转/分的速度，均质20分钟，得到叶黄素酯乳液，将所述乳液在55℃下真空干燥后粉碎，过100目筛，得到对比例水溶性叶黄素粉末。
实施例4叶黄素酯微囊粉分散于饮料中色调比较
称取白砂糖10g、果葡糖浆10g、凤梨浓缩汁20g、阿斯巴甜0.05g、甜菊糖0.15g、柠檬酸1g、苹果酸0.2g、柠檬酸钠0.5g、叶黄素酯制剂0.012g、山梨酸钾0.25g、加纯水至500g搅拌10min，20Mpa均质，85℃保温巴氏灭菌10min后，将饮料冷却至70℃灌装。其中叶黄素酯制剂分别采用实施例1-3以及对比例1-3所述方法制备获得。
用分光测色计分别检测饮料初始L*a*b*值,结果列于表1。
表1叶黄素酯微囊粉分散于饮料中色调值
由上述数据可知，通过本申请方法制备的叶黄素酯微囊粉溶于液体饮料中，饮料无沉淀，色调b*值为45-50；对比例对应样品中部分出现少量沉淀，色调b*值均低于41。表明本申请的叶黄素酯制剂的溶解性优于对比例，并且颜色中黄色浓度更高，具有对比例达不到的黄色色调。
实施例5叶黄素酯饮料货架期稳定性
将实施例4得到的饮料放置在光照为4000Lx,2-6℃的保鲜柜,90天后,评价饮料沉淀情况；用分光测色计检测饮料L*a*b*值,结果列于表2。
表2叶黄素酯饮料货架期稳定性变化
90d后，实施例对应样品无沉淀生成，且颜色变化不显著；对比例的a*和b*值均明显下降，原因是叶黄素酯氧化降解导致色调饱和度显著降低。表明本申请叶黄素酯在液体饮料中的稳定性优于对比例。
Claims (10)
1.一种叶黄素酯水分散制剂，其特征在于，由包括如下按质量百分比的原料制备而成：叶黄素酯晶体1-8％，油相载体10-25％，油相抗氧化剂0.5-5％，复合水相载体65-75％，水相抗氧化剂1-3％。
2.根据权利要求1所述的叶黄素酯水分散制剂，其特征在于，所述复合水相载体由空间网状结构的增稠剂、麦芽糊精和蔗糖组成，所述增稠剂占原料质量百分比30-45％，所述麦芽糊精和蔗糖质量比为2:1-1:1。
3.根据权利要求2所述的叶黄素酯水分散制剂，其特征在于所述具有增稠剂为辛烯基琥珀酸淀粉钠、海藻酸钠、β-环糊精、黄原胶或阿拉伯胶中的一种或多种。
4.根据权利要求1-3任一项所述的叶黄素酯水分散制剂，其特征在于，所述油相载体为分子蒸馏单甘酯、辛癸酸甘油酯、三聚甘油单硬脂酸酯或乙酰化单、双甘油脂肪酸酯中的一种或多种。
5.根据权利要求1-4任一项所述的叶黄素酯水分散制剂，其特征在于，所述水相抗氧化剂选自L-抗坏血酸、D-异抗坏血酸钠、抗坏血酸钠、茶多酚中的一种或多种。
6.根据权利要求1-5任一项所述的叶黄素酯水分散制剂，其特征在于，所述油相抗氧化剂是符合食品安全国家标准的任意一种或多种，优选维生素E。
7.权利要求1-6任一项所述的叶黄素酯水分散制剂的制备方法，其特征在于，包括如下步骤：
1)按质量占比将叶黄素酯、油相载体，油相抗氧化剂混合，加热至65-80℃，得到油相；
2)按质量占比将复合水相载体、水相抗氧化剂混合，65-80℃加热搅拌溶解，得到水相；
3)5000-9000rpm条件下剪切乳化，将油相缓慢加入水相中获得制剂初乳液。
4)初乳液经过纳米研磨后，进行喷雾干燥，获得所述叶黄素酯水分散制剂。
8.根据权利要求7所述的叶黄素酯水分散制剂的制备方法，其特征在于，步骤4)所述纳米研磨工艺为：首先采用0.4-0.6mm粒径氧化锆球将料液粒径研磨至＜0.3μm后，再用0.2-0.3mm粒径氧化锆球继续研磨料液，使得料液平均粒径＜0.1μm。
9.根据权利要求1-8任一项所述的叶黄素酯水分散制剂在制备液体饮料中的应用。
10.一种液体饮料，其特征在于含有权利要求1-8任一项所述叶黄素酯水分散制剂。
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