CN104304838A - 一种耐受机械搅拌的高载油营养脂质微囊粉的制备方法 - Google Patents
一种耐受机械搅拌的高载油营养脂质微囊粉的制备方法 Download PDFInfo
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Abstract
本发明提供了一种耐受机械搅拌的高载油营养脂质微囊粉的制备方法,将蛋白类壁材加入水中,在40~70℃下搅拌溶解,调pH值至7.0~12.0,在40~70℃条件下反应0.5~4h,反应液中加入糖类壁材和稳定剂搅拌溶解,得水相溶液;营养脂质类芯材中加入抗氧化剂和乳化剂,在40~70℃下搅拌溶解,得油相溶液;两相混合,乳化均质,喷雾干燥得到微囊粉。本发明的微囊粉总脂肪含量高达60~85%,表面油低于5%、能够耐受机械力,而且此微囊粉具有良好的自乳化能力,可溶解为均一、稳定、无颗粒漂浮和沉淀的细腻乳液,可用于食品领域,可添加到面包、饼干、营养棒和奶制品等食品中,也可作为固体冲剂饮用。
Description
技术领域
本发明涉及一种微囊化技术领域,特别是涉及微囊化的芯材为营养类脂质,载油量达到60~85%,且能够耐受机械搅拌的微囊粉的制备方法。
背景技术
营养脂质包括中性脂肪和类脂,前者主要作用是提供能量,后者具有多重生理功能。脂质的基本组成为脂肪酸,有必需脂肪酸和非必需脂肪酸之分。必需脂肪酸主要有3种,即亚油酸、亚麻酸和花生四烯酸。营养脂质中n-3和n-6系列多不饱和脂肪酸作为人类必需脂肪酸,在人体生理中发挥着非常关键的作用,主要表现在:心血管病、癌症等疾病的防止,促进生理细胞的生长和免疫调节等方面。
营养脂质类物质在使用过程中存在不稳定的问题,油脂氧化是油脂及油基食品败坏的主要原因之一。油脂在食品加工和贮藏期间,因空气中的氧气、光照、微生物、酶等的作用,产生令人不愉快的气味,苦涩味和一些有毒性的化合物,这些过程统称为酸败。油脂氧化的初级产物是氢过氧化物,其形成途径有自动氧化、光敏氧化和酶促氧化三种。
此外,营养脂质类物质作为脂溶性产品在食品领域应用也受到极大的限制。例如它与植物油脂可以混溶,将其添加到油脂中很容易,但应用于水基型食品却存在添加困难、难以混合均匀、含量不稳定、容易酸败,而且它自身口味差、有油脂气味。因此,营养脂质类物质在食品中的应用面临综上所述的诸多问题。
近年来,微囊技术成为一种活性成分的新型稳态化技术,它是一种利用天然或化学合成的高分子材料,将固体、液体,甚至是气体物质包裹起来,形成具有半透性或密封囊膜的微型胶囊。微囊化技术主要解决营养脂质在应用中存在的两方面问题:一是有效保护功能成分,避免外界环境对功能成分的破坏;二是改变物质形态,将脂溶性的功能成分变成水溶性固体粉末,为营养脂质在食品方向的应用开辟了新天地。
传统工艺制备营养脂质微囊粉存在一定的技术缺欠,国内多篇专利报道(CN1287114A、CN101999475、CN101856125 A、CN101856124 A、CN102742674 A)将营养脂质进行微囊化包埋,但是载油量只有30~40%。本专利采用的制备方法载油量在60%以上,即补充等量的营养脂质所食用的产品剂量将减半,减少了产品壁材用量,从而降低了产品成本。也有专利报道(专利号CN1380056A)高含量油溶性维生素微囊化制备方法,载油量达到70%,但是它是采用油包水包油复乳包覆,工艺过程复杂,而且外油相使用液体石蜡等油溶剂或有机溶剂,导致产品食用安全性下降。还有专利报道(CN102716087 A),壁材采用辛烯基琥珀酸淀粉钠,将脂溶性维生素作为油相,均质后,加入交联剂进行交联,载油量大概在60%,产品流动性好,但是缺点是微囊粉非水溶。有专利报道(CN101869294A)产品在冷水中能迅速分散为均匀的乳状,稳定性良好,但是其工艺过程中乳液固含量只有30%,固含量是乳液在规定条件下烘干后剩余部分占总量的质量百分数,固含量较低,意味着制备等量的粉末所蒸发的水量增大,所消耗的热能源增加而造成能源的浪费。本发明的乳液固含量在50%以上,在降低热能源消耗的基础上同时提高产业化生产效率。有专利报道(CN101269310A)微囊产品为冷水可分散,复水稳定性好,载油量更高,表面油更低,但是没有明确载油量和表面油的具体数值。另有专利报道(CN1556115A)由于加入十二辛烯基丁二酸酐使得淀粉分子结构上交联了具有长链亲油的烷基和具有亲水的羧基,并且把淀粉分子之间架桥连接,形成一紧密的网状结构,从而使被包埋后的微囊具有很好的抗机械破坏能力。但是此反应时间较长,需要22~31h,而且专利中未提及衡量抗机械破坏能力的数据及实施例支持。本发明的反应时间只需要0.5~2h即可完成,耐受机械搅拌的能力以表面油作为衡量指标。
发明内容
鉴于上述所述的制备营养脂质类微囊粉中存在的问题,提供一种载油量高、抗机械搅拌能力强的新的营养脂质类微囊粉的制备方法。该方法制备得到的营养脂质类微囊粉的载油量高达60~85%,产品初始表面油在5%以下,2h抗剪切试验后,产品表面油在10%以下,而且粉末能够自由流动,说明此产品具有良好的抗机械搅拌的能力,适合于预混料的干混工艺。
本发明的目的是通过下述技术方案来实现的:
一种耐受机械搅拌的营养脂质微囊粉的制备方法,该制备方法包括分别制备得到水相溶液和油相溶液,以及将二者混合、乳化均质、喷雾干燥的步骤,其特征在于:
水相溶液的制备方法为:将蛋白类壁材加入水中,在40~70℃下搅拌溶解,加入pH调节剂调pH值至7.0~12.0,优选pH7.5~9.5,最优选pH8.0~9.0,在40~70℃条件下反应0.5~4h,优选0.5~2h,反应液中加入糖类壁材和稳定剂搅拌溶解,得水相溶液,其中蛋白类壁材占终产品质量的1%~40%,优选2%~20%;糖类壁材占终产品质量的5%~40%,优选10%~30%;
油相溶液的制备方法为:营养脂质类芯材中加入抗氧化剂和乳化剂,在40~70℃下搅拌溶解,得油相溶液,其中营养脂质类芯材占终产品质量的60~85%,优选60%~78%。
在上述技术方案中,所述的pH调节剂优选为氢氧化钠、碳酸氢钙、碳酸氢钠、柠檬酸钠、氢氧化钙、氯化钙中的一种或几种,更优选氢氧化钙。实际使用时,所述pH调节剂配制成0.1~5.0%水溶液后用来调节溶液pH值。
在上述所有技术方案中,所述的蛋白类壁材选自植物蛋白、乳清蛋白、酪蛋白、酪蛋白酸盐中的一种或几种,更优选酪蛋白、酪蛋白酸钠、酪蛋白酸钙中的一种或几种,最优选酪蛋白酸钠。
在上述所有技术方案中,所述的糖类壁材为低聚麦芽糖、麦芽糊精、聚葡萄糖、海藻糖、葡萄糖浆、果葡糖浆、固体葡萄糖浆中的一种或多种。
在上述所有技术方案中,所述的乳化剂选自蔗糖酯、单双甘油酯、单甘脂、卵磷脂、硬脂酰乳酸钠、司盘-60、司盘-80中的一种或几种。
在上述所有技术方案中,所述的营养脂质类芯材选自亚麻籽油、月见草油、琉璃苣油、共轭亚油酸甘油酯、共轭亚油酸甲酯、中链甘油三酸酯、鱼油、藻油、维生素A、维生素D、维生素E中的一种或几种。
本发明对所述的稳定剂没有特别限定,本领域通常使用的稳定剂都可以使用,可以优选使用磷酸,焦磷酸二氢二钠、焦磷酸钠、磷酸二氢钙、磷酸二氢钾、磷酸氢二铵、磷酸氢二钾、磷酸氢钙、磷酸三钙、磷酸三钾、磷酸三钠、六偏磷酸钠、三聚磷酸钠、磷酸二氢钠、磷酸氢二钠,更优选使用磷酸氢二钾、磷酸氢钙、磷酸三钙、三聚磷酸钠、磷酸二氢钠、磷酸氢二钠。
本发明对所述的抗氧化剂没有特别限定,本领域通常使用的稳定剂都可以使用,可以优选使用维生素E、抗坏血酸棕榈酸酯、抗坏血酸、抗坏血酸钠、茶多酚、磷脂、迷迭香提取物,更优选使用维生素E、磷脂、抗坏血酸棕榈酸酯。
本发明中,根据上述技术方案制备得到的水相溶液和油相溶液混合、乳化均质、喷雾干燥后得到本发明的营养脂质微囊粉。具体步骤为:将壁材加入水中,在40~70℃下搅拌溶解,加入pH调节剂调pH值至7.0~12.0,在40~70℃条件下反应0.5~4h,反应液中加入糖类和稳定剂搅拌溶解,得水相溶液。将油相溶液缓慢加入水相溶液中,在40~70℃下机械搅拌乳化,形成初乳液,初乳液在压力30~60Mpa下高压均质,得油滴粒径D50<1000nm的均质乳液;均质乳液160~185℃下喷雾干燥。其中,水相溶液和油相溶液的加入量没有特别限定,本领域技术人员可以根据常规技术采用水相溶液和油相溶液的使用量并实现本发明,本发明优选采用油相质量占终产品质量的60%~85%。
本发明为解决营养脂质因分解、氧化、挥发等过程造成的成分损失,采用微囊化技术,筛选壁材,将营养脂质进行包埋,载油量达到60-85%。当微囊粉载油量高达60~85%的时候,在运输和预混料过程中,产品极易因为外界机械强度造成微囊破损漏油,引起表面油升高,进而产品发生粘连结团,大大降低产品品质而影响产品的应用。本发明通过在微囊粉制备工艺过程中加入pH调节剂,调节蛋白溶液pH值,使得溶液中酸度调节剂与蛋白发生反应生成一种具有刚性强度的材料作为微囊粉的壁材,主要解决了微囊粉在载油量高达60~85%情况下,微囊容易破损的难题。即本发明的方法制备出的微囊粉,在载油量60~85%条件下,具有一定耐受机械搅拌的能力,产品初始表面油在5%以下,2h抗剪切试验后,产品表面油在10%以下,而且粉末能够自由流动,说明此产品具有一定抗机械搅拌的能力,适合于预混料的干混工艺。
本发明的另一目的是提供上述技术方案所述的方法制备得到的营养脂质微囊粉。所述的营养脂质微囊粉表面油低于5%,为自由流动粉末,该粉末能够耐受机械搅拌,抗剪切试验,搅拌2h,表面油保持在10%以下,将微囊粉在40℃温水中分散,轻微搅拌,微囊粉可自行溶解为均一、稳定、无颗粒漂浮和沉淀的细腻乳液。本发明的方法制备得到的营养脂质微囊粉产品可用于食品领域,可添加到面包、饼干、营养棒和奶制品等食品中,也可作为固体冲剂饮用。
本发明的有益效果:
1.本发明的营养脂质微囊粉的制备方法,选用蛋白作为壁材,并在其水溶液中加入特定的pH调节剂,调pH值至7.0~12.0,在50~70℃条件下反应0.5~4h,使得溶液中pH调节剂与蛋白发生反应生成一种具有刚性强度的材料作为微囊粉的壁材,主要解决了微囊粉在载油量高达60~85%情况下,微囊容易破损的难题。
2.本发明的营养脂质微囊粉的制备方法,载油量高达60~85%,保证使用相同剂量的产品,有效含量高,壁材用量相对少,产品成本降低,产品具有价格优势。
3.本发明的营养脂质微囊粉的制备方法,在载油量高达60~85%的情况下,表面油在5%以下,说明包埋效果良好,保证了产品的稳定性,同时延长产品货架期。
4.本发明的方法制备得到的营养脂质微囊粉,在2h抗剪切试验后,产品表面油在10%以下,说明此微囊粉具有良好的耐受机械搅拌的能力,避免高载油产品在运输过程中因碰撞产生的漏油现象,而且在产品应用过程中,与其它粉末预混料不易发生粘连,混料更顺利。
5.本发明的方法制备得到的营养脂质微囊粉,40℃温水可分散,无需搅拌,微囊粉可自行溶解为均一、稳定、无颗粒漂浮和沉淀的细腻乳液。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。下述实施例中,如无特殊说明,所使用的实验方法均为常规方法,所用材料、试剂等均可从生物或化学公司购买。
下述实施例制备得到的高载油营养脂质微囊粉的相应质量参数以及分析方法如下:
1.抗剪切能力评价方法:
称取微囊粉70g置于250mL旋转蒸发瓶中,搅拌2h,转速为150r/min,分别在搅拌0h、1h、2h后测定表面油并记录数据,依据记录数据对比0h,1h和2h后表面油的变化情况,判断高载油微囊粉的抗剪切能力。
表面油含量分析方法:按SC/T 3505-2006《鱼油微胶囊》附录A规定执行。
微囊粉抗剪切能力评价标准:根据2h剪切后产品表面油含量(简称2h表面油含量)来判断,如:
良好:2h表面油≤6%;
好:6%<2h表面油≤10%;
差:2h表面油>10%。
2.复水稳定性评价方法:
量取150mL 40℃温水,倒入250mL烧杯中,将烧杯置于25℃水浴锅中,搅拌桨转速250r/min,称量3g微囊粉投入烧杯中,持续搅拌5min,评价乳液状态。
微囊粉复水稳定性评价标准:
实施例1
将6kg酪蛋白酸钙溶解于60℃、245kg水中,待完全溶解后加入0.02kg氢氧化钠调节溶液pH值,最终pH=7.0,在60℃搅拌反应4h,然后在反应液中加入34kg麦芽糊精和1kg三聚磷酸钠,搅拌溶解,制得水相,水相温度为60℃;
共轭亚油酸甘油脂中加入2kg单甘脂、0.6kg混合生育酚和0.38kg葵花磷脂,温度升高到75℃,搅拌溶解制得油相,油相降温至60℃;
将60℃的油相缓慢加入水相混合,在150rpm、60℃下机械搅拌1h,再以压力50Mpa高压均质两遍,得油滴粒径D50为460nm的均质乳液;均质乳液在喷雾干燥机中干燥,喷雾干燥条件为进风温度160℃,出风温度80℃,喷雾干燥得到共轭亚油酸甘油酯油脂微囊粉,其粒度为40目100%通过。该微囊粉相应质量参数如表1。
表1.
表1的结果可知,共轭亚油酸甘油酯微囊粉载油量达到78.5%,2h抗剪切能力测试,表面油由1.6%只上升至2.4%,表明微囊粉抗剪切性能良好。
实施例2
将50kg酪蛋白溶解于70℃、500kg水中,待完全溶解后加入10kg氯化钙调节溶液pH值,最终pH=12,在70℃反应1h后,反应液中加入2.5kg磷酸氢二钾、5kg蔗糖酯和80kg海藻糖,搅拌溶解1h,制得水相,水相温度为70℃;
350kg高油酸葵花油(油酸含量为78%)中加入1kg混合生育酚和1.5kg大豆磷脂,60℃下搅拌30min制得油相;
将油相缓慢加入水相混合,在63rpm、70℃下搅拌1h乳化,再以均质压力50Mpa下高压均质两遍,得油滴粒径为D50为310nm的均质乳液;均质乳液在喷雾干燥机中干燥,,喷雾干燥条件为进风温度170℃,出风温度78℃,即得到高油酸葵花油微囊粉,其粒度为40目95%通过。该微囊粉相应质量参数如表2。
表2.
表2的结果可知,高油酸葵油微囊粉载油量达到71.1%,2h抗剪切能力测试,表面油由2.1%只上升至5.5%,表明微囊粉抗剪切性能良好。
实施例3
将26.1kg大豆分离蛋白溶解于50℃、370kg水中,加入0.9kg三聚磷酸钠,待完全溶解后加入3.0kg氢氧化钙调节溶液pH值,溶液最终pH=9.0,在50℃反应0.5h,加入69kg低聚麦芽糖,搅拌溶解0.5h,制得水相,水相温度为50℃.;
210kg大豆油中加入0.3kg混合生育酚和0.2kg葵花磷脂,升温至50℃,搅拌溶解,制得油相,保温50℃待用;
将油相缓慢加入水相中混合,在97rpm、50℃下搅拌1h,在以均质压力50Mpa下高压均质两遍,均质乳液在喷雾干燥机中干燥,喷雾干燥条件为进风温度180℃,出风温度75℃,即得到大豆油微囊粉,其粒度为40目95%通过。该微囊粉相应质量参数如表3。
表3.
表3的结果可知,大豆油微囊粉载油量达到70.2%,2h抗剪切能力测试,表面油由1.8%只上升至7.8%,表明微囊粉抗剪切性能良好。
实施例4
将30kg酪蛋白酸钠溶解于40℃、370kg水中,然后加入1.2kg三聚磷酸钠,待完全溶解后加入4.8kg氢氧化钠调节溶液pH值,溶液最终PH值为9.5,在40℃反应0.5h后,加入78kg聚葡萄糖,搅拌溶解0.5h,制得水相,水相温度为40℃;
将480kg亚麻籽油中加入4.2kg单双甘油酯、1.2kg混合生育酚和0.6kg葵花磷脂,升温至75℃,待乳化剂完全溶解,制得油相,油相降温至40℃待用;
将油相和水相混合,在63rpm、40℃下搅拌乳化1h,再以均质压力50Mpa下高压均质两遍,得油滴粒径D50为460nm的乳液;均质乳液在喷雾干燥机中干燥,喷雾干燥条件为进风温度175℃,出风温度83℃,即得到亚麻籽油微囊粉粉,其粒度为40目100%通过。该微囊粉相应质量参数如表4。
表4.
表3的结果可知,亚麻籽油微囊粉载油量达到80.9%,2h抗剪切能力测试,表面油由3.3%只上升至6.8%,表明微囊粉抗剪切性能良好。
以上实施例仅用于阐述本发明,而本发明的保护范围并非仅仅局限于以上实施例,凡是依据本发明的技术实质对以上实施例所作的任何细微修改,等同变化与修饰,均属于本发明技术方案的保护范围内。
Claims (7)
1.一种耐受机械搅拌的高载油营养脂质微囊粉的制备方法,该制备方法包括分别制备得到水相溶液和油相溶液,以及将二者混合、乳化均质、喷雾干燥的步骤,其特征在于:
水相溶液的制备方法为:将蛋白类壁材加入水中,在40~70℃下搅拌溶解,加入pH调节剂调pH值至7.0~12.0,在40~70℃条件下反应0.5~4h,反应液中加入糖类壁材和稳定剂搅拌溶解,得水相溶液,其中蛋白类壁材占终产品质量的1%~40%,糖类壁材占终产品质量的5%~40%;
油相溶液的制备方法为:营养脂质类芯材中加入抗氧化剂和乳化剂,在40~70℃下搅拌溶解,得油相溶液,其中营养脂质类芯材占终产品质量的60%~85%。
2.根据权利要求1所述的制备方法,其特征在于,所述的pH调节剂为氢氧化钠、碳酸氢钙、碳酸氢钠、柠檬酸钠、氢氧化钙、氯化钙中的一种或几种。
3.根据权利要求1所述的制备方法,其特征在于,所述的蛋白类壁材选自植物蛋白、乳清蛋白、酪蛋白、酪蛋白酸盐中的一种或几种。
4.根据权利要求1所述的制备方法,其特征在于,所述的糖类壁材为低聚麦芽糖、麦芽糊精、聚葡萄糖、海藻糖、葡萄糖浆、果葡糖浆、固体葡萄糖浆中的一种或多种。
5.根据权利要求1所述的制备方法,其特征在于,所述的乳化剂选自蔗糖酯、单双甘油酯、单甘脂、卵磷脂、硬脂酰乳酸钠、司盘-60、司盘-80中的一种或几种。
6.根据权利要求1所述的制备方法,其特征在于,所述的营养脂质类芯材选自葵花油、亚麻籽油、月见草油、琉璃苣油、共轭亚油酸甘油酯、共轭亚油酸甲酯、中链甘油三酸酯、鱼油、藻油、维生素E、维生素A、维生素D中的一种或几种。
7.根据权利要求1~6的任一项所述的方法制备得到的高载油营养脂质微囊粉。
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