CN112754016A - 一种高稳定性藻油dha微胶囊及其制备方法 - Google Patents
一种高稳定性藻油dha微胶囊及其制备方法 Download PDFInfo
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Abstract
本发明属于一种藻油制剂及其制备方法领域,具体涉及了一种高稳定性藻油DHA微胶囊的制备方法。具体的,本发明提供一种微胶囊,是通过藻油DHA乳状液喷雾干燥得到的,包括壁材和芯材。所述壁材为辛烯基琥珀酸酯化淀粉、麦芽糊精,所述的乳状液为DHA藻油的水乳液。本发明还提供该微胶囊的制备方法,先将水和壁材搅匀,后水油相混合,经过预乳化,和两步低压均质,最后喷雾干燥。最终得到的微胶囊粒径控制在30‑100μm,胶囊产品的表面油含量可控制在0.39%以下,浸出率0.48%以下,包埋率可提高至98.07%以上。
Description
技术领域
本发明属于一种藻油制剂及其制备方法领域,具体涉及了藻油DHA微胶囊的制备工艺。
背景技术
作为婴幼儿配方奶粉的重要成分之一,二十二碳六烯酸(Docose HexaenoieAcid,DHA)可促进婴儿大脑发育,提高记忆力。微藻油是DHA的主要来源之一,因结构简单易吸收而得到广泛应用。但DHA含有多个双键,极易因氧化而变质,丧失生理功效,产生对人体有害的反式脂肪酸和令人反感的腥异味,严重影响了其在食品中的应用。通过一定的方式将DHA微胶囊化,可以有效隔绝外界环境,防止其氧化变质。
微胶囊化是预防油脂氧化的主要措施。微胶囊化是将壁材与DHA油脂混合制成乳状液,利用喷雾干燥等方法,将DHA油脂液滴包裹成的毫米级微小粒子的过程。微胶囊产品质量与乳状液稳定性紧密相关。
在实际的工业化生产中,有很多微胶囊化的方法如喷雾冷却法、空气悬浮法、挤压法、界面聚合法和原味聚合法等。物理化学法则有凝聚法、相分离法等。传统微胶囊制备方法尽管能够提高油脂稳定性,掩盖油脂的腥味,但是制备得到的微胶囊经历较长时间保存后的稳定性和风味会明显下降,继而对产品品质有较大影响。
发明内容
针对现有技术中,缺少高稳定性藻油DHA微胶囊产品,这一技术空白,本发明提供一种高稳定性藻油DHA微胶囊的及其制备方法。
一种高稳定性藻油DHA微胶囊,由DHA乳状液通过喷雾干燥制备而成;DHA乳状液包括外层壁材、内层芯材和水组成;外层壁材和内层芯材总质量占乳状液质量的20-35%,外层壁材占干物质含量的75-85%,内层芯材占干物质质量的15-25%。
其中,所述的乳状液中含有氯化钙,浓度为0.05-0.1mol/L。
其中,所述的外层壁材选自辛烯基琥珀酸酯化淀粉、麦芽糊精,质量比为0.5-3:1。
其中,所述的内层芯材选自微藻发酵所得的DHA藻油。
其中,所述的微胶囊的制备方法为:
(1)水相溶液的制备:将辛烯基琥珀酸酯化淀粉、氯化钙、麦芽糊精和水按照所述的比例,加入烧杯中,50℃水浴电动搅拌10 min;
(2)水油相溶液混合:将发酵所得的DHA藻油按照所述含量,加入水相溶液中,50℃水浴中电动搅拌5 min;
(3)预乳化:将(2)中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2-3分钟,获得预乳化液;
(4)均质阶段:将(3)中所得的预乳化液倒入高压均质机中,均质压力20-40 MPa,经过多步均质后,获得终乳化液;
(5)对终乳化液进行喷雾干燥。
其中,所述的喷雾干燥工艺条件为:进风温度180-200℃,出风温度70-90℃,风机频率60-70。
其中,均质次数为1-2次。
本发明外层壁材采用辛烯基琥珀酸酯化淀粉和麦芽糊精。辛烯基琥珀酸酯化淀粉在淀粉分子中引入了疏水性基团,使其具有了两亲性,成为非离子表面活性剂,能够在O/W界面形成较厚的吸附层,从而阻止油滴在乳液中重新聚结。更多的,辛烯基琥珀酸酯化淀粉和麦芽糊精能吸附钙离子,使油相液滴表面带电,更难易凝聚。
本领域公知,乳状液的分层和沉降速率与乳状液的黏度成反比,与两相间的密度差成正比。外层壁材的采用会造成体系黏度增加,乳状液分层/沉降速率下降,减少了油滴的聚结,从而使乳状液的稳定性得到提升,但是整体乳状液稠度增加,不利于后续的喷雾干燥。本发明微胶囊为大粒径,控制在30-100μm,油滴密度与水相仿,沉降速率极低,乳状液稳定。
本发明有益效果
本发明的DHA藻油微胶囊制备方法,可用于高稳定性的DHA藻油微胶囊的生产。微胶囊产品的表面油含量可控制在0.39%以下,浸出率0.48%以下,包埋率可提高至98.07%以上。
本发明的DHA藻油微胶囊制备方法,工艺简单,操作方便,适用于连续化工业生产。
具体实施方式
实施例1
水相溶液的制备:称取辛烯基琥珀酸酯化淀粉20g,麦芽糊精30g,水500ml,氯化钙5g,加入烧杯中混匀,50℃水浴电动搅拌10 min。
水油相溶液混合:称取发酵所得的DHA藻油10g,加入水相溶液中,50℃水浴中电动搅拌5 min
预乳化:将上一步中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2分钟,获得预乳化液。
均质阶段:本发明采用多步均质法获取终乳化液。将上一步中所得的预乳化液倒入高压均质机中,设置均质压力20 MPa,经过两步步均质后,获得终乳化液。
微胶囊制作:将DHA藻油乳化液进行喷雾干燥获得微胶囊粉末产品,设置喷雾干燥工艺条件为:进风温度180℃,出风温度80℃,风机频率65。
获得的DHA藻油微胶囊为浅黄澄清粉末,有淡藻味,DHA藻油包埋率98.07%,电镜观察粒径约为40μm,7天(168h)存储后,DHA油脂的氧化值为1.78mmol/kg。
实施例2
水相溶液的制备:称取辛烯基琥珀酸酯化淀粉20g,麦芽糊精30g,水500ml,氯化钙5g,加入烧杯中混匀,50℃水浴电动搅拌10 min。
水油相溶液混合:称取发酵所得的DHA藻油10g,加入水相溶液中,50℃水浴中电动搅拌5 min
预乳化:将上一步中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2分钟,获得预乳化液。
均质阶段:本发明采用多步均质法获取终乳化液。将上一步中所得的预乳化液倒入高压均质机中,设置均质压力30MPa,经过一步均质后,获得终乳化液。
微胶囊制作:将DHA藻油乳化液进行喷雾干燥获得微胶囊粉末产品,设置喷雾干燥工艺条件为:进风温度180℃,出风温度80℃,风机频率65。
获得的DHA藻油微胶囊为浅黄澄清粉末,有淡藻味,DHA藻油包埋率96.47%,电镜观察粒径约为50μm,7天(168h)存储后,DHA油脂的氧化值为1.86mmol/kg。
实施例3
水相溶液的制备:称取辛烯基琥珀酸酯化淀粉20g,麦芽糊精30g,水500ml,氯化钙5g,加入烧杯中混匀,50℃水浴电动搅拌10 min。
水油相溶液混合:称取发酵所得的DHA藻油10g,加入水相溶液中,50℃水浴中电动搅拌5 min
预乳化:将上一步中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2分钟,获得预乳化液。
均质阶段:本发明采用多步均质法获取终乳化液。将上一步中所得的预乳化液倒入高压均质机中,设置均质压力40MPa,经过两步均质后,获得终乳化液。
微胶囊制作:将DHA藻油乳化液进行喷雾干燥获得微胶囊粉末产品,设置喷雾干燥工艺条件为:进风温度180℃,出风温度80℃,风机频率65。
获得的DHA藻油微胶囊为浅黄澄清粉末,有淡藻味,DHA藻油包埋率84.20%,电镜观察粒径约为20μm,7天(168h)存储后,DHA油脂的氧化值为3.16mmol/kg。
对比例1
水相溶液的制备:称取辛烯基琥珀酸酯化淀粉40g,麦芽糊精60g,水500ml,氯化钙10g,加入烧杯中混匀,50℃水浴电动搅拌10 min。
水油相溶液混合:称取发酵所得的DHA藻油10g,加入水相溶液中,50℃水浴中电动搅拌5 min
预乳化:将上一步中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2分钟,获得预乳化液。
均质阶段:本发明采用多步均质法获取终乳化液。将上一步中所得的预乳化液倒入高压均质机中,设置均质压力35MPa,经过两步步均质后,获得终乳化液。
微胶囊制作:将DHA藻油乳化液进行喷雾干燥获得微胶囊粉末产品,设置喷雾干燥工艺条件为:进风温度180℃,出风温度80℃,风机频率65。
获得的DHA藻油微胶囊为浅黄澄清粉末,有淡藻味,DHA藻油包埋率91.00%,电镜观察粒径约为20μm,7天(168h)存储后,出现沉降,DHA油脂的氧化值为2.13mmol/kg,乳状液稠度过大,后续不易喷雾干燥,21天后,沉降完全。
对比例2
水相溶液的制备:称取辛烯基琥珀酸酯化淀粉20g,麦芽糊精30g,水500ml,加入烧杯中混匀,50℃水浴电动搅拌10 min。
水油相溶液混合:称取发酵所得的DHA藻油10g,加入水相溶液中,50℃水浴中电动搅拌5 min
预乳化:将上一步中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2分钟,获得预乳化液。
均质阶段:本发明采用多步均质法获取终乳化液。将上一步中所得的预乳化液倒入高压均质机中,设置均质压力20 MPa,经过两步步均质后,获得终乳化液。
7天后略微沉降,49天后,沉降完全。
Claims (7)
1.一种高稳定性藻油DHA微胶囊,其特征在于,由DHA乳状液通过喷雾干燥制备而成;DHA乳状液包括外层壁材、内层芯材和水组成;外层壁材和内层芯材总质量占乳状液质量的20-35%,外层壁材占干物质含量的75-85%,内层芯材占干物质质量的15-25%。
2.根据权利要求1所述的微胶囊,其特征在于,所述的乳状液中含有氯化钙,浓度为0.05-0.1mol/L。
3.根据权利要求1所述的微胶囊,其特征在于,所述的外层壁材选自辛烯基琥珀酸酯化淀粉、麦芽糊精,质量比为0.5-3:1。
4.根据权利要求1所述的微胶囊,其特征在于,所述的内层芯材选自微藻发酵所得的DHA藻油。
5.根据权利要求1所述的微胶囊,其特征在于,所述的微胶囊的制备方法为:
(1)水相溶液的制备:将辛烯基琥珀酸酯化淀粉、氯化钙、麦芽糊精和水按照所述的比例,加入烧杯中,50℃水浴电动搅拌10 min;
(2)水油相溶液混合:将发酵所得的DHA藻油按照所述含量,加入水相溶液中,50℃水浴中电动搅拌5 min;
(3)预乳化:将(2)中所得的水油混合液加入到胶体磨中,转速设置每分钟6000转,处理2-3分钟,获得预乳化液;
(4)均质阶段:将(3)中所得的预乳化液倒入高压均质机中,均质压力20-40 MPa,经过多步均质后,获得终乳化液;
(5)对终乳化液进行喷雾干燥。
6.根据权利要求5所述的微胶囊,其特征在于,所述的喷雾干燥工艺条件为:进风温度180-200℃,出风温度70-90℃,风机频率60-70。
7.根据权利要求5所述的微胶囊,其特征在于,所述的均质次数为1-2次。
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