CN112535293A - 一种光热稳定的维生素微囊粉及其制备方法 - Google Patents
一种光热稳定的维生素微囊粉及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种光热稳定的维生素微囊粉及其制备方法;所述光热稳定的维生素微囊粉原辅料包括:维生素、油脂、变性淀粉、淀粉糖、稳定剂组合物、pH调节剂、缓冲剂、淀粉糖酶、抗结剂;其制备方法为:先将维生素溶于油脂中,加入稳定剂组合中的虾青素;将变性淀粉溶于水中,加入上述溶液得到初乳液;将淀粉糖溶于水中,加入淀粉糖酶,控制DE值70‑85%,灭活后将酶解液加入上述溶液,进行一次乳化;将稳定剂组合中的结冷胶和魔芋胶溶于水中,加入上述溶液,进行二次乳化;将所述乳液喷雾干燥,得到维生素微囊粉。采用本发明提供的方法得到的维生素微囊粉具有光热条件稳定、包埋率高等特点。
Description
技术领域
本发明属于微囊技术领域,尤其涉及一种光热稳定的维生素微囊粉及其制备方法。
背景技术
维生素,顾名思义是人和动物维持正常的生理功能必须摄入的一类微量营养物质。一般维生素无法自身产生,必须由食物中摄取。尽管人和动物对维生素的摄入量较低,但缺乏维生素会导致严重的健康问题,摄入适量的维生素对身体健康是必要的。近年来,随着膳食补充剂市场的火热,以及人们对健康越来越重视,维生素的需求也逐年增加。
维生素包括很多种类,常见的有维生素A、维生素D、维生素E以及B族维生素等,不同的维生素对肌体发挥着不同的重要作用。比如维生素A具有维持正常视觉功能,维持骨骼正常生长发育等功能,缺乏会导致多种眼睛疾病,生长迟缓,免疫力下降等。维生素D具有提高机体对钙、磷的吸收,促进生长和骨骼钙化,防止氨基酸通过肾脏损失等作用。维生素K具有防止新生婴儿出血疾病、预防内出血及痔疮、减少生理期大量出血、促进血液正常凝固的作用。
尽管不同的维生素具有不同的作用,但不可避免的有个共性问题即易受到环境的破坏。这是制约维生素应用的一大因素,这些因素包括水分、温度、氧气、光照等。尤其是温度、光照等问题,一直是解决维生素应用的热点问题。有研究表明温度是影响维生素稳定性的首要问题,在高温条件下,维生素A、维生素B1、维生素C和叶酸等有明显降解。大量实验证实:食物在烹调过程中,叶酸会损失50%-90%,加热到100℃15分钟,食物叶酸的量会减少50%。可见光和紫外线是维生素的另一“杀手”,大部分维生素都会受到光照的影响。有研究表明,日光照射6小时,奶粉中维生素K1的保留率不足30%。
微胶囊技术是将固体、液体或气体包埋在微小而密封的胶囊中,能在特定条件下释放的技术。其特点是可以减少外界因素对活性物质的反应,改变活性物质的物理状态,改善活性物质口感和提高利用度等。随着微胶囊技术的发展,其广泛应用在食品、药品、农药化学品、香料、饲料添加剂等领域。
尽管微胶囊技术对活性物质有一定的保护作用,但对维生素的保护研究相对较少。现有技术记载了一些关于提高维生素稳定性的研究成果:CN201910343072.9公开了一种维生素微胶囊的制备方法:将蛋白质溶解于缓冲溶液中,加入所述维生素,壁材芯材比按照1-6:1比例,溶解后调节pH至蛋白的等电点,搅拌产生沉淀,经离心后冷冻干燥,制得微胶囊。US10568843公开了一种制备微胶囊粉末或微粒的方法:将壁材物质部分溶解在手中后,加入含有多个双键的脂溶性营养物质,得到均质后的纳米粒径乳液,将剩余壁材加入到乳液中,剪切,溶解,喷雾造粒得到微胶囊。CN202010066362.6公开了一种维生素D2油脂微胶囊的制备方法:壁材溶于水中,形成水相溶液;脂溶性抗氧化剂溶解到植物油中后与维生素D2油混合,水溶性抗氧化剂溶解到水中后加入到混合后的维生素D2油中形成油相;水相与油相混合,除氧,巴氏杀菌,喷雾干燥得到维生素D2微胶囊。CN201511030503.4公开了一种维生素、胡萝卜素粉剂的制备方法:首先得到维生素、胡萝卜素微胶囊产品;凝胶剂与抗氧化剂溶解在植物油中,形成超分子溶液;在流态化空气中,将超分子溶液喷涂到微胶囊表面,形成粉剂。以上专利都公开了维生素微胶囊或粉剂的制备方法,这些方法中有些涉及的设备昂贵,一般难以实现,同时对因环境因素导致维生素的损失涉及较少,尤其是对因温度、光照引起的维生素的损失保护更是有限。
发明内容
本发明公开了一种光热稳定的维生素微囊粉及其制备方法,通过采用酶解淀粉糖、多步处理、特定的稳定剂组合的方式对维生素物质进行包埋,喷雾干燥,最终得到光热稳定的维生素微囊粉。
本发明的第一方面在于保护一种光热稳定的维生素微囊粉,其原辅料按重量份含有下述组分:
对于上文所述的技术方案,优选的原辅料重量组成为:
对于上文所述的技术方案,优选的,所述稳定剂组合物为结冷胶、魔芋胶和虾青素的组合;其中结冷胶、魔芋胶与虾青素的重量比为0.5-3:1-5:1-3;
对于上文所述的技术方案,优选的,所述的维生素选自维生素A醋酸酯、维生素A棕榈酸酯、维生素D3、维生素K1中的至少一种;
对于上文所述的技术方案,优选的,所述的油脂选自大豆油、玉米油、葵花籽油、中链甘油三酯(MCT)中的至少一种;优选MCT;
对于上文所述的技术方案,优选的,所述淀粉糖选自抗性糊精、麦芽糊精、低聚麦芽糖、固体玉米糖浆中的至少一种;优选固体玉米糖浆;
对于上文所述的技术方案,优选的,所述淀粉糖酶选自α-淀粉酶、β-淀粉酶、葡糖糖糖化酶、异淀粉酶、多糖酶、普鲁兰酶中的至少一种;优选葡萄糖糖化酶。
对于上文所述的技术方案,优选的,所述pH调节剂为磷酸、柠檬酸、盐酸、醋酸中一种或几种;优选磷酸。
对于上文所述的技术方案,优选的,所述缓冲剂选自磷酸二氢钾、磷酸二氢钠、磷酸氢二钾、磷酸氢二钠、柠檬酸钾、柠檬酸钠中的至少一种;优选磷酸二氢钾;
对于上文所述的技术方案,优选的,所述抗结剂选自二氧化硅、磷酸三钙、硅酸钙的至少一种。
本发明的另一方面在于保护上文所述光热稳定的维生素微囊粉的制备方法,该方法包括以下步骤:
(1)在避光通氮条件下,将维生素、稳定剂组合中的虾青素加入到油脂中,温度控制40-55℃;更优选40-42℃,使其完全溶解混匀;
(2)初乳液:将变性淀粉投入去离子水中,温度控制40-60℃;更优选40-42℃,搅拌分散均匀,加入步骤(1)获得的溶液,搅拌乳化,得到初乳液;
其中,所述初乳液中变性淀粉与去离子水的重量比为1:1-3;
(3)一次乳化:将淀粉糖投入去离子水中,温度控制45-70℃,更优选55-60℃,用pH调节剂调节溶液pH为4.4-5.5,向其中加入淀粉糖酶,酶解,控制DE值70-85%,然后使酶灭活,降低溶液温度至40-60℃,更优选40-42℃,加入缓冲剂,搅拌溶解,将酶解液加入到步骤(2)中,搅拌后至少2次均质;一般情况下,所述搅拌的时间为20-40min;
其中,所述酶解液中淀粉糖与去离子水的重量比为1:1-2.5;
(4)二次乳化:将结冷胶和魔芋胶投入去离子水中,温度控制45-70℃,更优选65-70℃,使其完全溶解,降低温度至40-60℃,更优选40-42℃,将其加入到步骤(3)中,搅拌乳化后20-40MPa均质一次;其中,所述乳化的搅拌时间为10-20min,20-30MPa;所述结冷胶与去离子水的重量比为1-10:200;
(5)喷雾干燥:将步骤(4)所制备的乳液进行喷雾干燥;
(6)向干燥后的粉末中加入抗结剂,然后筛分、包装。
对于上文所述的技术方案,优选的,步骤(3)所述的至少2次均质为,至少在20-40MPa均质一次,在45-70MPa高压均质一次;所述的2次均质优选的条件为20-30MPa均质一次,在50-60MPa高压均质一次;
对于上文所述的技术方案,优选的,步骤(5)所述的喷雾干燥条件为控制进风温度110-140℃,出风温度80-100℃。
对于上文所述的技术方案,优选的,步骤(3)所述的使酶灭活采用沸水浴10-30min。
通过上述方法制得的维生素微囊粉也是本发明的目的之一。
本发明采用酶解淀粉糖、多步处理、特定的稳定剂组合对维生素进行包埋,通过喷雾干燥,得到光热稳定的、高含量的维生素微囊粉。
本发明解决了维生素制剂不稳定尤其是在光热环境下易降解的问题,产品可广泛用于烘焙、固体饮料、胶囊、压片等。
有益效果:
本发明通过微囊化手段,将脂溶性维生素制备成水溶性较好的固体制剂。本发明采用独特的制备工艺以及特定的稳定剂组合,有效的隔绝外部的氧气、光等对活性成分的破坏,解决了目前维生素制剂在光热环境下不稳定的难题,极大的提高了维生素制剂的稳定性及应用范围;同时本发明涉及的工艺简单,适于扩大生产。通过本发明的方法制备出的维生素微囊粉在光照稳定性试验评价中,保留率超过90%,明显高于原料保留率。通过本发明的方法制备出的维生素微囊粉,产品粒度均一,流动性好,水溶性出色,同时稳定性好,包埋率超过98%。
具体实施方式
下述非限制性实施例用于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
在避光通氮条件下,称取150gMCT于500ml烧杯中,温度保持42℃,加入1.0g虾青素和120g维生素D3,搅拌至完全溶解。此为A相溶液。
称取300g去离子水于1000ml烧杯中,温度保持42℃,加入250g变性淀粉,搅拌分散均匀,加入A相溶液,搅拌乳化,得到初乳液。
称取500g去离子水于1000ml烧杯中,温度控制60℃,向其中加入460g麦芽糊精,搅拌分散均匀,用2.0g磷酸将乳液pH调整至4.7,向其中加入5g葡萄糖糖化酶,酶解,得到溶液DE值为78%,然后沸水浴20min,使酶灭活,将酶解液降温至42℃,加入2.2g磷酸二氢钾,搅拌溶解。将其加入到初乳液中,进行一次乳化,25MPa均质一次,56MPa高压均质一次。此为B相乳液。
称取200g蒸馏水与500ml烧杯中,水温保持66℃,向其中加入1g结冷胶和1g魔芋胶,搅拌溶解后,降低温度至42℃,将其加入到B相乳液中进行二次乳化,然后25MPa均质一次。此为C相乳液。
将所制备C相乳液进行喷雾干燥:进风温度125℃,出风温度86℃,最后向粉中加入10g二氧化硅并筛分,得到维生素D3微囊粉。记作样品1。
实施例2
在避光通氮条件下,称取750g葵花籽油于2000ml烧杯中,温度保持40℃,加入8.0g虾青素和500g维生素K1,搅拌至完全溶解,此为A相溶液。
称取2000g去离子水于5000ml烧杯中,温度保持40℃,加入1400g变性淀粉,搅拌分散均匀,加入A相溶液,搅拌乳化,得到初乳液。
称取2500g去离子水于2000ml烧杯中,水温保持58℃,向其中加入2260g低聚麦芽糖,搅拌分散均匀,用5.0g盐酸将乳液pH调整至4.5,向其中加入40g异淀粉酶,酶解,得到溶液DE值为70%,然后沸水浴20min,使酶灭活,将酶解液降温至40℃,加入5.5g磷酸氢二钠,搅拌溶解。将其加入到初乳液中,进行一次乳化,28MPa均质一次,60MPa高压均质一次。此为B相乳液。
称取600g去离子水于1000ml烧杯中,水温保持68℃,向其中加入5.5g结冷胶和7.5g魔芋胶,搅拌溶解后,降低温度至40℃,将其加入到B相乳液中进行二次乳化,然后27MPa均质一次。此为C相乳液。
将所制备的C相乳液进行喷雾干燥:进风温度121℃,出风温度82℃,最后向粉中加入45g二氧化硅并筛分,得到维生素K1微囊粉。记作样品2。
实施例3
在避光氮气保护条件下,称取260g大豆油于500ml烧杯中,温度保持41℃,加入2.4g虾青素和300g维生素A棕榈酸酯,搅拌至完全溶解,此为A相。
称取600g去离子水于2000ml烧杯中,水温保持40℃,加入440g变性淀粉,搅拌分散均匀,加入A相溶液,搅拌乳化,得到初乳液。
称取1000g去离子水于1500ml烧杯中,水温保持56℃,向其中加入940g抗性糊精,搅拌分散均匀,用2.0g柠檬酸将乳液pH调整至5.1,加入16g普鲁兰酶,酶解,得到溶液DE值为79%,然后沸水浴20min,使酶灭活,将酶解液降温至41℃,加入8.2g柠檬酸钾,搅拌溶解。将其加入到初乳液中,进行一次乳化,22MPa均质一次,58MPa高压均质一次。此为B相乳液。
称取450g去离子水与100ml烧杯中,水温保持69℃,向其中加入2.4g结冷胶和4.0g魔芋胶,搅拌溶解后,降低温度至41℃,将其加入到B相乳液中进行二次乳化,然后24MPa均质一次。此为C相乳液。
将所制备的C相乳液进行喷雾干燥:进风温度130℃,出风温度84℃,最后向粉中加入16g二氧化硅并筛分,得到维生素A棕榈酸酯微囊粉。记作样品3。
实施例4
对样品1、样品2、样品3进行光照稳定性实验评价,结果如表1:
表1
同时对样品1、样品2、样品3所用原料进行光照稳定性实验评价,结果如表2:
表2
从结果可以看出,用本发明公开的工艺得到的维生素微囊粉产品包埋率高、冲调性好,并且经过光照稳定性实验评价,产品保留率高。与未处理的原料相比,大大提高了产品稳定性。这些性状指标都表明该产品具有很好的稳定性,可广泛用于固体饮料、压片、胶囊、烘焙等终端产品。
其中光照稳定性试验评价方法为:分别称取相同质量且大小为75mm×30mm样品块,共10块,置于QUV紫外耐候试验机中,设定温度80℃,模拟日光照射,24小时后随机选取各组三块样品,检测含量,取平均值,对比实验前后保留率变化,我们认为保留率≥90%为合格。
实施例5
将样品1、样品2、样品3放入40℃、75%湿度的加速烘箱的上、下箱中,对三组样品同时进行光照和非光照的三个月产品稳定性实验评价,结果如表3-1~表3-4:
表3-1.加速稳定性实验
表3-2.加速稳定性实验
表3-3.加速稳定性实验
表3-4.加速稳定性实验
从加速稳定性实验可以看出,经过三个月加速后,三组样品在光照和非光照条件下的外观、冲调性均没有发生变化,含量保留率略有下降,但一般认为加速三个月含量保留率≥90%产品合格。产品经过加速三个月后,光照稳定性试验合格。由发明所述的工艺制备的维生素微囊粉稳定性优异。
实施例6
以实施例1的工艺为基础,用葡萄糖糖化酶将麦芽糊精水解成不同的DE值,验证不同DE值对产品性能的影响,结果如表4:
表4
乳液DE值 | 包埋率 | 冲调性 | 光照实验保留率 |
10 | 71.5 | 稍有漂油,有小颗粒 | 64.1% |
30 | 77.9 | 稍有漂油,有小颗粒 | 69.8% |
50 | 84.3 | 稍有漂油,乳液均一 | 73.1% |
70 | 98.7 | 无漂油,乳液均一 | 98.7% |
80 | 99.2 | 无漂油,乳液均一 | 99.2% |
85 | 99.5 | 无漂油,乳液均一 | 98.6% |
90 | 95.1 | 明显漂油,乳液均一 | 82.4% |
95 | 89.3 | 明显漂油,乳液均一 | 75.6% |
从结果可以看出,淀粉糖酶对淀粉糖的水解程度对产品冲调性和光照实验稳定性有很大影响。当DE值较低时,产品溶解性较差。当DE值较高时,产品的包埋性较差。只有当淀粉糖的DE值在70-85%时,产品包埋性能和稳定性都表现优异。
实施例7
以实施例1的工艺为基础,验证多步处理对产品性能的影响:
包埋工艺:
工艺1:A相溶液中不加入油脂,维生素D3直接热熔融形成溶液,未经过二次乳化。其余步骤按实施例1工艺进行,经过初乳液制备、一次乳化、喷雾干燥;
工艺2:未经过二次乳化。其余步骤按实施例1工艺进行,经过初乳液制备、一次乳化,喷雾干燥;
工艺3:A相溶液中不加入油脂,维生素D3直接热熔融形成溶液。其余步骤按实施例1工艺进行,经过初乳液制备、一次乳化、二次乳化、喷雾干燥;
工艺4:按实施例1工艺进行,经过初乳液制备、一次乳化、二次乳化、喷雾干燥;
结果如表5:
表5
包埋处理 | 包埋率 | 冲调性 | 光照稳定性试验保留率 |
处理1 | 90.4% | 乳液均一 | 68.3% |
处理2 | 93.4% | 乳液均一 | 78.2% |
处理3 | 90.7% | 乳液均一 | 77.9% |
处理4 | 99.7% | 乳液均一 | 98.1% |
从结果看,乳液制备和处理工艺对产品的影响很大。经过本发明所述的乳液制备及处理工艺,产品的包埋率及光照稳定性都表现优异。
实施例8
以实施例1的工艺为基础,验证稳定剂组合中,虾青素换成其他抗氧化剂对产品稳定性的影响,结果如表6:
表6
从结果看,当稳定剂组合中的虾青素换成其他抗氧化剂时,产品的光照稳定试验结果较。只有当稳定剂组合中使用结冷胶和魔芋胶与虾青素组合,产品稳定性表现优异。
实施例9
以实施例1的工艺为基础,验证稳定剂组合中,魔芋胶换成其他食品胶对产品稳定性的影响,结果如表7:
表7
从结果看,当稳定剂组合中的魔芋胶换成其他食品胶时,产品的包埋率、冲调性、光照稳定性都有不同程度的变差。只有当稳定剂组合中使用结冷胶和虾青素与魔芋胶组合,产品包埋率、冲调性、稳定性都表现优异。
实施例10
以实施例1的工艺为基础,验证稳定剂组合中,结冷胶换成其他食品胶对产品稳定性的影响,结果如表8:
表8
从结果看,当稳定剂组合中的结冷胶换成其他食品胶时,产品的包埋率、冲调性、光照稳定性都有不同程度的变差。只有当稳定剂组合中使用魔芋胶和虾青素与结冷胶组合,产品包埋率、冲调性、稳定性都表现优异。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,本领域的技术人员在本发明披露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (10)
2.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述稳定剂组合物为结冷胶、魔芋胶和虾青素的组合;其中结冷胶、魔芋胶与虾青素重量比为(0.5-3):(1-5):(1-3)。
3.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述的维生素选自维生素A醋酸酯、维生素A棕榈酸酯、维生素D3、维生素K1中的至少一种。
4.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述的油脂选自大豆油、玉米油、葵花籽油、中链甘油三酯中的至少一种。
5.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述淀粉糖选自抗性糊精、麦芽糊精、低聚麦芽糖、固体玉米糖浆中的至少一种。
6.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述淀粉糖酶选自α-淀粉酶、β-淀粉酶、葡糖糖糖化酶、异淀粉酶、多糖酶、普鲁兰酶中的至少一种。
7.根据权利要求1所述的光热稳定的维生素微囊粉,其特征在于:所述pH调节剂为磷酸、柠檬酸、盐酸、醋酸中一种或几种;所述缓冲剂选自磷酸二氢钾、磷酸二氢钠、磷酸氢二钾、磷酸氢二钠、柠檬酸钾、柠檬酸钠中的至少一种;所述抗结剂选自二氧化硅、磷酸三钙、硅酸钙的至少一种。
8.如权利要求2所述的光热稳定的维生素微囊粉的制备方法,其特征在于:所述方法包括以下步骤:
(1)在避光通氮条件下,将维生素、虾青素加入到油脂中,40-55℃使其完全溶解混匀;
(2)初乳液:将变性淀粉投入去离子水中,40-60℃搅拌分散均匀,加入步骤(1)获得的溶液,搅拌乳化,得到初乳液;
其中,所述初乳液中变性淀粉与去离子水的重量比为1:1-3;
(3)一次乳化:将淀粉糖投入去离子水中,温度控制45-70℃用pH调节剂调节溶液pH为4.4-5.5,向其中加入淀粉糖酶,酶解,控制DE值70-85%,然后使酶灭活,降低溶液温度至40-60℃,加入缓冲剂,搅拌溶解,将酶解液加入到步骤(2)中,搅拌后均质至少2次;其中,所述酶解液中淀粉糖与去离子水的重量比为1:1-2.5;
(4)二次乳化:将结冷胶和魔芋胶投入去离子水中,温度控制45-70℃,使其完全溶解,降低温度至40-60℃,将其加入到步骤(3)中,搅拌乳化后20-40MPa均质一次;其中,结冷胶与去离子水的重量比为1-10:200;
(5)喷雾干燥:将步骤(4)所制备的乳液进行喷雾干燥后加入抗结剂即得终产品。
9.根据权利要求8所述的光热稳定的维生素微囊粉的制备方法,其特征在于:步骤(3)所述的至少均质2次为:至少在20-40MPa均质一次,在45-70MPa高压均质一次。
10.根据权利要求8所述的光热稳定的维生素微囊粉的制备方法,其特征在于:步骤(5)所述的喷雾干燥条件为控制进风温度110-140℃,出风温度80-100℃。
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