CN111447925B - 一种番茄红素微囊粉及其制备方法 - Google Patents
一种番茄红素微囊粉及其制备方法 Download PDFInfo
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Abstract
一种番茄红素微囊粉的制备方法,将番茄红素与水相充分混合,得到番茄红素乳化液,再将所述乳化液研磨至粒径小于1μm,喷雾干燥,即可。所述水相中包括:分子量为5000~10000Da的明胶酶解液、双糖、多糖以及抗氧化剂。所述双糖为蔗糖、麦芽糖、乳糖种的一种或几种;所述多糖为普鲁兰多糖、壳聚糖中的一种或几种。
Description
技术领域
本发明涉及一种色素的微囊技术,尤其是一种番茄红素微囊粉的制备方法。
背景技术
番茄红素(lycopene)是类胡萝卜素的一种,是目前自然界的植物中被发现的最强抗氧化剂之一,具有重要的生理功能。近年来流行病学研究表明,与其它类胡萝卜素相比,番茄红素在治疗和预防多种慢性疾病(如肿瘤、癌症、心血管疾病、动脉硬化等),以及提高机体免疫力方面表现出更显著的疗效。因此,番茄红素的研究引起了越来越多人的关注。
番茄红素是一种化学结构式中含有11个共扼双键和2个非共扼双键的非环状平面多不饱和脂肪烃,在具有较强的抗氧化性的同时,其性质也非常不稳定,易受光、热、氧的作用而被氧化降解,这在很大程度上限制了其应用范围。微胶囊技术以有效减少活性物质对外界环境因素(如光、氧、水)的反应,可以提高番茄红素的稳定性,从而增加其在功能性产品方面的应用。有关番茄红素微胶囊技术在功能营养品方面应用的研究有很多,例如专利文件 CN106038511A提出了一种纳米番茄红素微囊化冷水分散型粉剂的制备方法,其采用溶剂使番茄红素与复配的非离子表面活性剂等充分溶解均质后得到纳米级番茄红素微囊粉;该方法制备的番茄红素微囊粉剂色泽较差,并且制备过程中使用乙醚、石油醚、乙酸乙酯、丙酮、氯仿、苯等有毒溶剂易对人体造成伤害。专利文件 CN104431690A提供了一种番茄红素微囊颗粒及其制备工艺,其使用植物油分散番茄红素晶体制备油相,产品仍然呈番茄红素的暗红色,色相较差。
发明内容
本发明的目的是克服现有技术的缺陷,提供一种色相好、性质稳定的番茄红素微囊粉的制备方法。
具体而言,本发明提供的方法是将番茄红素与水相充分混合,得到番茄红素乳化液;再将所述乳化液研磨至粒径小于1μm,喷雾干燥,即可。
本发明对水相中的具体组分进行优化,以确保番茄红素包裹于所述组分组成的壁材中,从而具有良好的综合性能。具体而言,本发明所述水相中包括明胶酶解液、双糖、多糖以及抗氧化剂。
明胶是一种常用的微胶囊包埋壁材,但市售产品分子量一般在 15000~250000Da,分子量较大,空间网状结构较密集,一般经包埋后所得产品色调发暗,色差亮度值一般小于20,品相较差。本发明提供的方法对明胶进行酶解后,可降低明胶的分子量,确保以其为壁材包埋番茄红素后所得产品具有良好的色泽。具体而言,本发明优选所述明胶酶解液中明胶的分子量为5000~10000Da。
作为本发明的一种优选方案,所述明胶酶解液可采用包括如下步骤的方法制备而成:将明胶加入到水中,在55~65℃、pH值为 7.5~8.5的条件下加入蛋白酶酶解;酶解后煮沸、冷却至55~65℃保温,即得明胶酶解液。所述蛋白酶可选用巯基蛋白酶,最好为木瓜蛋白酶。
在实际制备中,优选明胶与水的质量比为1~2:3~4,所述蛋白酶的质量为明胶质量的2.0%~3.0%。
本发明在对明胶酶解液进行优化的基础上,优选所述双糖为蔗糖、麦芽糖和/或乳糖,所述多糖为普鲁兰多糖和/或壳聚糖。当采用上述优选的糖组分时,可确保其与所述酶解后的明胶发挥协同作用,形成更加致密的网状结构,将番茄红素包埋,从而使番茄红素微囊粉具有良好的色泽以及稳定性。
本发明所述抗氧化剂的作用是防止番茄红素氧化失活,采用本领域常用的食品级天然抗氧化剂即可,如采用抗坏血酸、维生素E 中的一种或两种的混合物。
为了进一步提高上述协同效果,确保番茄红素微囊粉具有良好的色泽以及稳定性,本发明对各组分用量进行优选。作为本发明的一种优选方案,所述水相中包括:以1~2份明胶、3~4份水为原料经酶解得到的分子量为5000~10000Da的明胶酶解液,双糖2~3份,多糖0.3~0.5份,抗氧化剂0.1~0.2份。
所述水相在制备过程中,可在55~65℃进行充分搅拌(如:以转速30~50r/min搅拌30~60min),以确保其中各组分充分混合,得到均一的水相。
本发明优选将所述番茄红素与水相以特定比例混合,以水相中的明胶计,所述番茄红素与明胶的质量比优选为1:1~2。上述方案可以使得番茄红素被充分、均匀包埋的同时,确保所得微囊粉中番茄红素与微囊壁具有合适的尺寸比例,从而具有良好的色泽与稳定性。
本发明所述将番茄红素与水相充分混合,优选为在55~65℃以 7000~9000r/min剪切搅拌,可以得到混合程度优异的番茄红素乳化液。其中,为了确保所得产品的品质,所述采用的番茄红素原料优选为番茄红素晶体。
为了使所得产品具有良好的性能以及使用效果,本发明进一步优选所述研磨为研磨至粒径200~600nm。所述研磨可采用纳米研磨机进行,研磨至所需要的粒径即可。例如:在转速为1600~1800r/min 研磨1.0~2.0h。
本发明所述喷雾干燥采用本领域常规的喷雾干燥方式进行。作为本发明的一种优选方案,可采用以下参数:进风温度为165~180℃,出风温度为90~105℃,风量为300~500mL/h。
作为本发明的一种优选方案,所述番茄红素微囊粉的制备方法包括以下具体步骤:
(1)将1~2份明胶加入到3~4份水中,加入蛋白酶酶解后煮沸、冷却,得到55~65℃、分子量为5000~10000Da的明胶酶解液;
(2)将双糖2~3份、多糖0.3~0.5份以及抗氧化剂0.1~0.2份加入到所述明胶酶解液中,充分搅拌溶解,得水相;
(3)在所述水相中加入1份番茄红素,在55~65℃以 7000~9000r/min剪切搅拌,得到番茄红素乳化液;
(4)将所述番茄红素乳化液经研磨至粒度为200~600nm,得到番茄红素微乳液;
(5)将所述番茄红素微乳液喷雾干燥,即得番茄红素微囊粉。
本发明同时保护采用上述方法制备而成的番茄红素微囊粉。本发明提供的番茄红素微囊粉色度值可达到:L*38.5~40.5;a*29.0~ 30.0;b*19.0~20.0。经长期放置后,番茄红素的含量以及色度值均保持稳定。
本发明提供的方法以酶解后的明胶作为壁材,结合纳米研磨机的研磨作用,采用喷雾干燥的方式得到番茄红素微囊粉,解决了产品色泽发暗、对光、热、自由基的稳定性差的问题;所得番茄红素微囊粉的色调为樱桃红色,相较番茄红素晶体和普通番茄红素粉末的暗红色色调明亮鲜艳,能够增进消费者的食欲,而且其对光、热、自由基的稳定性高,室温下放置1年颜色无明显变化,含量保留率可达到97%以上。本发明该工艺简单,绿色环保,生产成本低,适合大规模制备番茄红素微囊粉。
具体实施方式
下面结合实施例,对本发明的具体实施方式作进一步详细描述。以下实例用于说明本发明,但不用来限制本发明的范围。
实施例1
本实施例提供了一种番茄红素微囊粉的制备方法,具体为:
(1)将150g明胶加入到225g纯净水中,木瓜蛋白酶的添加量为3.75g,调节溶液pH值为7.5,水浴温度为55℃,酶解3h,然后煮沸15min,冷却至55℃,得到明胶酶解液,所述明胶酶解液中明胶分子量为7000Da;
(2)在所述明胶酶解液中加入225g蔗糖、22.5g普鲁兰多糖、 10g抗坏血酸和5g维生素E,65℃下以转速40r/min搅拌45min,制得水相;
(3)在所述水相中边搅拌边加入75g含量为90wt%的番茄红素晶体,剪切得番茄红素乳化液,剪切转速为9000r/min、时间为10min、剪切时乳液温度为65℃;
(4)将所述番茄红素乳化液经纳米研磨机进行研磨,研磨机转速为1700r/min,研磨时间为1.5h,得到粒度为400nm的番茄红素微乳液;
(5)将所述番茄红素微乳液进行喷雾干燥,喷雾干燥的进风温度为175℃、出风温度为100℃、流量为500mL/h,得到番茄红素微囊粉。
实施例2
本实施例提供了一种番茄红素微囊粉的制备方法,具体为:
(1)将200g明胶加入到437.5g纯净水中,木瓜蛋白酶的添加量为6g,调节溶液pH值为8.0,水浴温度为60℃,酶解5h,然后煮沸15min,冷却至60℃,得酶解后明胶水溶液,所述明胶酶解液中明胶分子量为8000Da;
(2)在所述明胶酶解液中加入250g麦芽糖、62.5g普鲁兰多糖、 2.5g抗坏血酸和10g维生素E,60℃下以转速30r/min搅拌50min,制得水相;
(3)在所述水相中边搅拌边加入125g含量为90wt%的番茄红素晶体,剪切得番茄红素乳化液,剪切转速为8000r/min、时间为 15min,剪切时乳液温度为60℃;
(4)将所述番茄红素乳化液经纳米研磨机进行研磨,研磨机的转速为1800r/min,研磨时间为1.0h,得到粒度为500nm的番茄红素微乳液;
(5)将所述番茄红素微乳液进行喷雾干燥,喷雾干燥的进风温度为180℃、出风温度为105℃、流量为400mL/h,得到番茄红素微囊粉。
实施例3
本实施例提供了一种番茄红素微囊粉的制备方法,具体为:
(1)将165g明胶加入到440g纯净水中,木瓜蛋白酶的添加量为3.3g,调节溶液pH值为8.5,水浴温度为65℃,酶解4h,然后煮沸15min,冷却至65℃,得酶解后明胶水溶液,所述明胶酶解液中明胶分子量为5000Da;
(2)在所述明胶酶解液中加入275g乳糖、44g壳聚糖、22g抗坏血酸,65℃下以转速50r/min搅拌30min,制得水相;
(3)在所述水相中边搅拌边加入110g含量为90%的番茄红素晶体,剪切得番茄红素乳化液,剪切转速为7000r/min、时间为20min,剪切时乳液温度为65℃;
(4)将所述番茄红素乳化液经纳米研磨机进行研磨,研磨机的转速为1800r/min、研磨时间为2.0h,得到粒度为200nm的番茄红素微乳液;
(5)将所述番茄红素微乳液进行喷雾干燥,喷雾干燥的进风温度为170℃、出风温度为95℃、流量为300mL/h,得到番茄红素微囊粉。
实施例4
本实施例提供了一种番茄红素微囊粉的制备方法,具体为:
(1)将100g明胶加入到320g纯净水中,木瓜蛋白酶的添加量为2.5g,调节溶液pH值为8.2,水浴温度为60℃,酶解3.5h,然后煮沸15min,冷却至55℃,得到明胶酶解液,所述明胶酶解液中明胶分子量为10000Da;
(2)在所述明胶酶解液中加入125g蔗糖和125g麦芽糖、20g 普鲁兰多糖和15g壳聚糖、15g维生素E,55℃下以转速45r/min搅拌60min,制得水相;
(3)在所述水相中边搅拌边加入100g含量为92wt%的番茄红素晶体,剪切得番茄红素乳化液,剪切转速为7500r/min、时间为 30min,剪切时乳液温度为55℃;
(4)将所述番茄红素乳化液经纳米研磨机进行研磨,研磨机的转速为1600r/min、研磨时间为1.0h,得到粒度为600nm的番茄红素微乳液;
(5)将所述番茄红素微乳液进行喷雾干燥,喷雾干燥的进风温度为165℃、出风温度为90℃、流量为450mL/h,得到番茄红素微囊粉。
对比例1
(1)具体为将150g明胶加入到225g纯净水中,煮沸15min,冷却至55℃,得到溶液,所述明胶溶液中明胶分子量为45000Da;
(2)在所述明胶溶液中加入225g蔗糖、22.5g普鲁兰多糖、10g 抗坏血酸和5g维生素E,65℃下以转速40r/min搅拌45min,制得水相;
(3)在所述水相中边搅拌边加入75g含量为90wt%的番茄红素晶体,剪切得番茄红素乳化液,剪切转速为9000r/min、时间为10min、剪切时乳液温度为65℃;
(4)将所述番茄红素乳化液经纳米研磨机进行研磨,研磨机转速为1700r/min,研磨时间为1.5h,得到粒度为1.2μm的番茄红素微乳液;
(5)将所述番茄红素微乳液进行喷雾干燥,喷雾干燥的进风温度为175℃、出风温度为100℃、流量为500mL/h,得到番茄红素微囊粉。
实验例1:色度对比
从市场上随机采购三种番茄红素微囊粉,与实施例1~4提供的番茄红素一起检测色度,检测结果见表1。
表1:番茄红素微囊粉色度检测值
L* | a* | b* | |
实施例1 | 38.5 | 30.0 | 19.5 |
实施例2 | 40.2 | 29.0 | 20.0 |
实施例3 | 39.0 | 29.6 | 19.3 |
实施例4 | 39.4 | 29.3 | 19.7 |
对比例1 | 57.2 | 13.09 | 1.32 |
市售产品1 | 23.72 | 8.44 | 4.64 |
市售产品2 | 27.99 | 9.52 | 4.39 |
市售产品3 | 32.13 | 7.89 | 5.07 |
由表1结果可知,本发明提供的方法能有效地提升所得产品的暗红色色调,使之更加明亮鲜艳。
实验例2:稳定性实验
将实施例1~4提供的番茄红素微囊粉在温度25℃、湿度60%、避光条件下,放置1年,对其中番茄红素的含量以及色度值进行检测,结果如表2所示。
表2:番茄红素含量及色度值变化
由表2结果可知,本发明提供的番茄红素微囊粉稳定性良好,放置1年后番茄红素含量以及色度值均未出现明显变化。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种番茄红素微囊粉的制备方法,其特征在于,将番茄红素与水相充分混合,得到番茄红素乳化液;再将所述乳化液研磨至粒径小于1μm,喷雾干燥,即可;
所述水相中包括:以1~2份明胶和3~4份水为原料经酶解得到的分子量为5000~10000Da的明胶酶解液、双糖2~3份、多糖0.3~0.5份以及抗氧化剂0.1~0.2份;
所述双糖为蔗糖、麦芽糖、乳糖中的一种或几种;
所述多糖为普鲁兰多糖和/或壳聚糖;
所述抗氧化剂为抗坏血酸和/或维生素E;
所述番茄红素与水相中所含明胶的质量比为1∶1~2。
2.根据权利要求1所述的制备方法,其特征在于,所述明胶酶解液采用包括如下步骤的方法制备而成:将明胶加入到水中,在55~65℃、pH值为7.5~8.5的条件下加入蛋白酶酶解;酶解后煮沸、冷却至55~65℃保温,即得。
3.根据权利要求2所述的制备方法,其特征在于,所述蛋白酶为木瓜蛋白酶,和/或,所述蛋白酶的用量为明胶质量的2.0%~3.0%。
4.根据权利要求1所述的制备方法,其特征在于,所述充分混合方法为:在55~65℃以7000~9000r/min剪切搅拌。
5.根据权利要求1所述的制备方法,其特征在于,所述研磨为研磨至粒径200~600nm。
6.根据权利要求5所述的制备方法,其特征在于,所述研磨采用纳米研磨机在转速1600~1800r/min条件下研磨1.0~2.0h。
7.根据权利要求1所述的制备方法,其特征在于,所述喷雾干燥条件包括:进风温度为165~180℃,出风温度为90~105℃,风量为300~500mL/h。
8.根据权利要求1所述的制备方法,其特征在于,包括以下具体步骤:
(1)将1~2份明胶加入到3~4份水中,加入蛋白酶酶解后煮沸、冷却,得到55~65℃、分子量为5000~10000Da的明胶酶解液;
(2)将双糖2~3份、多糖0.3~0.5份以及抗氧化剂0.1~0.2份加入到所述明胶酶解液中,充分搅拌溶解,得水相;
(3)在所述水相中加入1份番茄红素,在55~65℃以7000~9000r/min剪切搅拌,得到番茄红素乳化液;
(4)将所述番茄红素乳化液经研磨至粒度为200~600nm,得到番茄红素微乳液;
(5)将所述番茄红素微乳液喷雾干燥,即得番茄红素微囊粉。
9.权利要求1~8任意一项所述制备方法制备而成的番茄红素微囊粉。
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