CN110859306A - 一种水凝胶珠的制备方法 - Google Patents
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Abstract
一种水凝胶珠的制备方法。本发明以海藻酸钠为壁材,利用微胶囊造粒仪,包封SPI‑EGCG复合物制备水凝胶珠颗粒。与传统的乳液相比,水凝胶珠包裹的SPI‑EGCG复合物更稳定,不易受到外界环境的影响,同时微胶囊造粒仪是一种条件温和,能够制备较小颗粒的水凝胶珠。因此,利用微胶囊造粒仪制备水凝胶珠在食品、医药领域具有广阔的发展前景。
Description
技术领域
本发明属于产品加工技术,主要涉及一种利用微胶囊造粒仪制备水凝胶珠的方法。
背景技术
胶体传递系统由于能够促进生物活性物质在食品中的结合,提高他们的化学/生化稳定性,控制它们在胃肠道环境中的释放得到了广泛的关注。典型的胶体传递体统有O/W型乳液及纳米乳液等,但是乳液或纳米乳液作为传递体统存在一定的局限性,由于乳化体系只有一层乳化剂对生物活性物质进行包裹,所以靠近液滴表面的生物活性物质都容易被亲水性组分(如酸、过渡金属或酶)降解,影响生物活性物质的稳定性,同时乳液或者纳米乳液大部分用来传递亲脂性生物活性物质,对一些大分子物质或者亲水性的生物活性物质的传递较少。水凝胶珠是一种颗粒型的微凝胶,是典型的球形粒子,其内部由交联亲水聚合物组成的多孔网络组成。水凝胶珠通常是由天然聚合物(如多糖和蛋白质)在相对温和的制备条件下形成的,它们对包封的生物活性物质的性能影响不大,因此在食品、补充剂和制药工业中,设计和制造用于装载、保护和释放生物活性物质的水凝胶珠给药系统越来越受到人们的关注。
适合在食品中使用的水凝胶珠通常由食品级生物高聚物(如蛋白质和/或多糖)通过多种方法构建。海藻酸钠是用于递送系统开发的最广泛使用的多糖之一。海藻酸盐溶液在各种二价阳离子的存在下迅速形成凝胶。这些凝胶可在0至100℃的温度下保持稳定。微胶囊造粒仪是采用挤压的原理,迫使生物聚合物通过喷嘴进入凝胶环境,在形成凝胶的过程中,生物活性成分被困在里边,围绕生物活性的水凝胶基质可以改善其物理和化学稳定性;同时微胶囊造粒仪的作用条件温和,制备的水凝胶颗粒小于1mm,也能够控制颗粒的大小,是制备水凝胶珠的良好设备。
EGCG是茶多酚中的主要成分,有相关研究表明EGCG具有抑制自由基产生、清除自由基的能力,从而具有抗衰老的作用,EGCG也可通过使突变剂灭活等其他途径发挥抗突变、抗癌变的作用,同时由于EGCG中含有多个酚羟基,故亲水性较强,也导致其在环境中不稳定,容易受到pH、温度、氧气等条件的影响。
将EGCG包裹在水凝胶中能够防止其与外界环境的接触,但由于水凝胶的孔径较大,容易接触到外界环境,因此将EGCG与蛋白进行复合,利用海藻酸钠将复合物包埋在水凝胶珠中,增加EGCG的稳定性。
发明内容
本发明所要解决的技术问题是克服上述现有技术的不足,提供一种利用微胶囊造粒仪制备水凝胶珠方法,增加EGCG在外界环境以及胃肠道中的稳定性。
本发明所要解决的技术问题是通过以下技术方案来实现的:
(1)大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌20-60min后,在室温,3000-4500g离心15-30min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在50-70℃下放置5-10h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为7-9,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,6000-9000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到6-4.5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,6000-9000g下离心30min,得到下层沉淀,之后对下层沉淀水洗1-3次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;
(2)SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌1-3h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将1-5mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为7-10后,在持续搅拌90min,得到SPI-EGCG复合物;
(3)海藻酸钠溶液的制备:10-30g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在25-60℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;
(4)水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:1-3比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为400-900Hz,电压为200-800V,压力为200-600mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
步骤(1)所述的大豆与正己烷在室温下搅拌的时间为30min,最佳离心参数为4500g,30min移除油脂,脱脂大豆粉溶于水中的pH为9,在9000g下离心30min得到溶液在水中的蛋白,沉淀蛋白的最佳pH为4.5,在9000g下离心30min得到下层沉淀,最佳的水洗参数为3次。
步骤(2)所述的SPI溶液在磷酸盐缓冲溶液中最佳搅拌时间为2h,EGCG的最佳浓度为5mg/mL,SPI与EGCG复合的最佳pH为9,在此条件下能够使SPI与EGCG进行共价复合。
步骤(3)所述的海藻酸钠溶解在磷酸盐缓冲溶液中的最佳质量为10g,搅拌的最佳温度为60℃。
步骤(4)所述的海藻酸钠与SPI-EGCG复合物混合的最佳比例为1:1,微胶囊造粒仪的最佳参数:频率700Hz,电压800V,压力为300mbar。
本发明以海藻酸钠,SPI-EGCG复合物为原料,利用微胶囊造粒仪制备水凝胶珠,增加EGCG在外界环境以及胃肠道中的稳定性。
具体实施方式
下面结合实施例对本发明具体实施例进行详细描述:
大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌20-60min后,在室温,4500g离心30min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在50-70℃下放置5-10h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为7-9,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,9000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到4.5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,9000g下离心30min,得到下层沉淀,之后对下层沉淀水洗1-3次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌2h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将1-5mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为8后,在持续搅拌90min,得到SPI-EGCG复合物;海藻酸钠溶液的制备:10g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在60℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:1比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为700Hz,电压为800V,压力为300mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
实施例1:
大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌40min后,在室温,3000g离心20min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在60℃下放置5h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为7.5,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,7000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,7000g下离心30min,得到下层沉淀,之后对下层沉淀水洗2次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌1h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将3mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为9后,在持续搅拌90min,得到SPI-EGCG复合物;海藻酸钠溶液的制备:10-30g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在45℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:3比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为400Hz,电压为300V,压力为200mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
实施例2:
大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌30min后,在室温,4000g离心20min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在50-70℃下放置5-10h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为7-9,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,8000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到6-4.5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,8000g下离心30min,得到下层沉淀,之后对下层沉淀水洗3次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌1h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将2mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为7.5后,在持续搅拌90min,得到SPI-EGCG复合物;海藻酸钠溶液的制备:15g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在60℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:2比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为500Hz,电压为500V,压力为236mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
实施例3:
大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌30min后,在室温,4500g离心30min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在50℃下放置10h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为8,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,9000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到4.5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,9000g下离心30min,得到下层沉淀,之后对下层沉淀水洗3次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌2h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将5mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为9后,在持续搅拌90min,得到SPI-EGCG复合物;海藻酸钠溶液的制备:10g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在60℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:1比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为400-900Hz,电压为200-800V,压力为200-600mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
Claims (5)
1.一种水凝胶珠的制备方法,其特征在于,包括以下步骤:
(1)大豆分离蛋白(Soybean protein isolate,SPI)的制备:脱皮大豆经筛选后利用粉碎机研磨成粉末,大豆粉与正己烷按照1:3的比例混合,在室温下搅拌20-60min后,在室温,3000-4500g离心15-30min,除去上层液体,收集下层沉淀,如此重复3次,将沉淀在50-70℃下放置5-10h,得到脱脂大豆粉,脱脂大豆粉与水按照1:6(w/v)的比例混合均匀后,调节其pH为7-9,将脱脂大豆粉中的大豆蛋白溶解在水中,在室温下持续搅拌2h,在4℃,6000-9000g下离心30min,移除沉淀得到上层液体,调节上层液体的pH到6-4.5,静置1h,沉淀上层液体中的大豆蛋白,在4℃,6000-9000g下离心30min,得到下层沉淀,之后对下层沉淀水洗1-3次,调节溶液pH为7并完全溶解,冷冻干燥后得到SPI粉末;
(2)SPI与EGCG复合物的制备:SPI溶解在0.01mol/L的磷酸盐缓冲溶液中(pH为7),在室温下持续搅拌1-3h后,置于4℃冰箱中过夜,使得SPI完全溶解,SPI最终的浓度为20mg/mL,将1-5mg/mL的EGCG加入SPI溶液中,在室温下搅拌30min,使其混合均匀后,调节混合物的pH为7-10后,在持续搅拌90min,得到SPI-EGCG复合物;
(3)海藻酸钠溶液的制备:10-30g海藻酸钠溶解在100mL的0.01mol/L的磷酸盐缓冲溶液(pH为7)中,在25-60℃下搅拌1h后,将温度降到35℃得到海藻酸钠溶液;
(4)水凝胶珠的制备:将海藻酸钠溶液与SPI-EGCG复合物按照1:1-3比例在室温下持续搅拌30min,使其完全混合,将混合溶液置于微胶囊造粒仪中,微胶囊造粒仪的频率为400-900Hz,电压为200-800V,压力为200-600mbar,溶液成串的滴在持续搅拌的10%的CaCl2溶液中,得到水凝胶珠。
2.根据权利要求1所述的一种水凝胶珠的制备方法,其特征在于,步骤(1)所述的大豆与正己烷在室温下搅拌的时间为30min,最佳离心参数为4500g,30min移除油脂,脱脂大豆粉溶于水中的pH为9,在9000g下离心30min得到溶液在水中的蛋白,沉淀蛋白的最佳pH为4.5,在9000g下离心30min得到下层沉淀,最佳的水洗参数为3次。
3.根据权利要求1所述的一种水凝胶珠的制备方法,其特征在于,步骤(2)所述的SPI溶液在磷酸盐缓冲溶液中最佳搅拌时间为2h,EGCG的最佳浓度为5mg/mL,SPI与EGCG复合的最佳pH为9,在此条件下能够使SPI与EGCG进行共价复合。
4.根据权利要求1所述的一种水凝胶珠的制备方法,其特征在于,步骤(3)所述的海藻酸钠溶解在磷酸盐缓冲溶液中的最佳质量为10g,搅拌的最佳温度为60℃。
5.根据权利要求1所述的一种水凝胶珠的制备方法,其特征在于,步骤(4)所述的海藻酸钠与SPI-EGCG复合物混合的最佳比例为1:1,微胶囊造粒仪的最佳参数:频率700Hz,电压800V,压力为300mbar。
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