CN115500511B - 多活性组分共包埋稳态化递送体系的加工方法与应用 - Google Patents

多活性组分共包埋稳态化递送体系的加工方法与应用 Download PDF

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CN115500511B
CN115500511B CN202211138303.0A CN202211138303A CN115500511B CN 115500511 B CN115500511 B CN 115500511B CN 202211138303 A CN202211138303 A CN 202211138303A CN 115500511 B CN115500511 B CN 115500511B
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amylopectin
cyclized
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缪铭
史雅凝
黎若兰
张涛
李赟高
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Jiangnan University
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Abstract

本发明属于新型健康食品加工技术领域，具体涉及多活性组分共包埋稳态化递送体系的加工方法与应用。本发明以亲水性活性组分与疏水性活性组分作为原料，通过环化支链淀粉互作组装和溶剂共沉淀调控技术制备多活性组分共包埋稳态化递送体系，从而提高亲水性活性组分与疏水性活性组分的负载率，疏水性活性组分的溶解度。本发明方法具有操作简单方便、过程安全可控等特点，所得产品不仅适用于个性化精准营养食品的创制开发，还能应用于功能食品、医药、化妆品等多个领域。

Description

多活性组分共包埋稳态化递送体系的加工方法与应用
技术领域
本发明属于新型健康食品加工技术领域，具体涉及多活性组分共包埋稳态化递送体系的加工方法与应用。
背景技术
近年来，随着大众对高品质生活的向往以及预期寿命的延长，人们对健康食品的要求日益提高。亲水性活性组分和疏水性活性组分在改善人类健康方面发挥重要作用，是健康食品的核心成分。目前，罗氏制药、帝斯曼、巴斯夫等国外主要健康食品生产供应商都开发了疏水性活性组分的脂质体、乳液、微胶囊、凝胶载体产品并形成了规模化的生产销售。而国内食品企业则多数局限于单一活性组分作为初级配料使用。因此，为了进一步拓展活性组分资源的开发利用，本发明旨在开发多活性组分共包埋稳态化递送体系的加工方法。
自然界中大多数活性组分可以从植物或者动物体内提取后，直接加入食品中。然而疏水性活性组分在水中的溶解度低，易受外界环境(温度、光照、氧气)、食品的加工贮存条件、消化道环境(pH值、酶、其他物质)的影响，进而降低其在食品和营养保健品中的生物利用度。因此，最大限度保留亲水性活性组分和疏水性活性组分的活性，改善疏水性活性组分的水溶性，提高活性组分的稳定性和生物利用率，实现活性组分的稳态化可控释放，是亟待克服的技术难题。
发明内容
技术问题：
提供一种操作简单方便、过程安全可控的亲水性活性组分和疏水性活性组分共包埋稳态化递送体系的加工方法，以解决亲水性活性组分与疏水性活性组分共包埋稳态化递送难题。
技术方案：
本发明的第一目的在于提供一种多活性组分共包埋稳态化递送体系的加工方法，依次包括如下步骤：
(1)将环化支链淀粉溶解于pH6.0-7.0的缓冲盐溶液体系得到环化支链淀粉质量浓度5％-40％的均一溶液，继续添加环化支链淀粉质量0.5-10倍的亲水性活性组分混匀，得到环化支链淀粉和亲水性活性组分的混合溶液；
(2)将疏水性活性组分溶解于纯乙醇，得到疏水性活性组分质量浓度为2-10％的溶液；然后将其添加到步骤(1)所得环化支链淀粉和亲水性活性组分的混合溶液中，搅拌混匀并调控混合体系中乙醇质量浓度达到35％以上；
(3)将步骤(2)所得体系置于功率200-500W、0-10℃超声场处理3-20min后，离心、沉淀干燥即得到目标产物——亲水性活性组分与疏水性活性组分共包埋稳态化递送体系。
作为本发明的一种实施方式，在步骤(1)中，将环化支链淀粉溶解于pH6.0-7.0的缓冲盐溶液体系得到环化支链淀粉质量浓度5％-25％的均一溶液。
作为本发明的一种实施方式，在步骤(1)中，环化支链淀粉与亲水性活性组分的质量比为1:(1～6)。
作为本发明的一种实施方式，在步骤(2)中，将疏水性活性组分溶解于纯乙醇，得到疏水性活性组分质量浓度为3-10％的溶液。
作为本发明的一种实施方式，在步骤(2)中，搅拌混匀并调控混合体系中乙醇质量浓度达到40～55％。
作为本发明的一种实施方式，在步骤(3)中，超声功率为200-450W。
作为本发明的一种实施方式，在步骤(3)中，超声处理时间为3-8min。
作为本发明的一种实施方式，所述环化支链淀粉的分子量为(3～100)×104g/mol，表面侧链平均链长DP>20，内部环状结构平均尺寸DP16～100且含α-1,6糖苷键5～10％。
作为本发明的一种实施方式，所述环化支链淀粉的分子量为(6～30)×104g/mol，表面侧链平均链长DP 25～50，环状结构平均尺寸DP20～40且含α-1,6糖苷键5～7％。
作为本发明的一种实施方式，所述环化支链淀粉采用如下步骤制得：将粮谷作物籽粒胚乳分级处理得到支链淀粉，添加来源于嗜热脂肪芽孢杆菌Q酶反应2-12小时后得到环化支链淀粉，其中Q酶转苷酶活力>150U。
作为本发明的一种实施方式，所述粮谷作物包括稻米、玉米和小麦中的至少一种。
作为本发明的一种实施方式，所述亲水性活性组分包括花色苷、蛋白短肽、水溶性维生素、栀子黄色素、抗性糊精、聚葡萄糖和矿物质中的至少一种。
作为本发明的一种实施方式，所述疏水性活性组分包括槲皮素、姜黄素、植物甾醇、β-胡萝卜素、白藜芦醇、叶黄素、番茄红素、辣椒素、亚麻籽油、鱼油和DHA藻油中的至少一种。
本发明的第二目的在于提供前述的方法制得的亲水性活性组分与疏水性活性组分共包埋稳态化递送体系。
本发明的第三目的在于提供前述的亲水性活性组分与疏水性活性组分共包埋稳态化递送体系在制备功能食品、药品或化妆品中的应用。
有益效果：
(1)本发明提供了一种操作简单方便、过程安全可控的亲水性活性组分和疏水性活性组分共包埋稳态化递送体系的加工方法，克服了亲水性活性组分与疏水性活性组分共包埋稳态化递送的技术难题。
(2)本发明利用环化支链淀粉的表面柔性侧链和内部环状结构特性，基于环化支链淀粉互作聚集组装包埋和溶剂共沉淀调控的技术原理，开发了一种多活性组分共包埋稳态化递送体系的加工方法。基于本发明的方法制得的多活性组分共包埋稳态化递送体系固态粒子尺寸为20-75μm；其中亲水性活性组分负载率不低于85％，疏水性活性组分负载率不低于39％，疏水性活性组分相较于游离疏水性活性组分的溶解度提高了74倍以上，对疏水性活性组分具有良好的活性保护和靶向递送效果，可以用于设计制备控释功能食品、药品或化妆品。
(3)本发明方法具有操作简单方便、过程安全可控、可实现连续化和低成本绿色生产等特点，且充分利用淀粉资源设计多活性组分共包埋稳态化递送体系，能够提升食品营养品质，实现个性化和营养精准食品的制造。所得产品不仅适用于个性化精准营养食品的创制开发，还能应用于功能食品、医药、化妆品等多个领域。
附图说明
图1实施例1制备的葡萄花色苷与槲皮素共包埋稳态化递送体系的电镜照片。
具体实施方式
下面结合实施例与对比例进一步阐明本发明的内容，但本发明所保护的内容不仅仅局限于下面的实施例。
颗粒粒径测定：采用激光粒度分析仪测定，以波长658nm固定激光为光源，散射光角度为90°，操作温度为25℃。
疏水性活性组分负载率测定方法：准确称取20mg包合物(多活性组分共包埋稳态化递送体系)溶于1mL去离子水中，室温避光平衡12h，4℃离心(3000rpm，5min)去除不溶物。取0.2mL前述离心上清液，加入4倍体积的无水乙醇后，旋涡振荡15min，离心(10000rpm，5min)分离萃取。计算得到疏水性活性组分含量(W1)、溶解性淀粉质量(M1)，负载率计算公式如下：
疏水性活性组分负载率(％)＝W1/M1×100。
亲水性活性组分负载率测定方法：准确称取20mg包合物(多活性组分共包埋稳态化递送体系)溶于1mL去离子水中，室温避光平衡12h，4℃离心(3000rpm，5min)去除不溶物。取0.2mL前述离心上清液，直接测定计算亲水性活性组分含量(W2)、溶解性淀粉质量(M2)，负载率计算公式如下：
亲水性活性组分负载率(％)＝W2/M2×100。
溶解度测定方法：准确称取20mg包合物(多活性组分共包埋稳态化递送体系)溶于1mL去离子水中，室温避光平衡12h，4℃离心(3000rpm，5min)去除不溶物。取0.2mL前述离心上清液，加入4倍体积的无水乙醇后，旋涡振荡15min，离心(10000rpm，5min)分离萃取多种活性组分和淀粉。取上清通过紫外分光光谱仪测定吸光值，代入标准曲线方程计算可得到溶解度。
涉及的生物材料的直接来源、关键参数和/或制备方法：
环化支链淀粉：将来源于稻米、玉米、小麦等粮谷作物籽粒胚乳分级得到支链淀粉，添加来源于嗜热脂肪芽孢杆菌Q酶反应2-12小时后得到环化支链淀粉，其中Q酶转苷酶活力>150U。
花色苷：来源于葡萄、血橙、紫叶甘蓝、茄子、樱桃等水溶性黄酮类色素。
槲皮素：来源于荞麦、沙棘、山楂、洋葱、卷心菜、芥菜、青椒、菊苣、葡萄柚等黄酮醇类化合物。
蛋白短肽：来源大豆蛋白、乳清蛋白、胶原蛋白、稻米蛋白、玉米蛋白等水解短肽产物。
维生素：包括维生素B1、B2、B6、B12、维生素C、泛酸、叶酸、胆碱等水溶性维生素。
植物甾醇：包括来源于植物油类、坚果、豆类中的谷固醇、菜油固醇、豆固醇、菜籽固醇和相应的烷醇等甾体化合物。
以下实施例中的商业化亲水性活性组分和疏水性活性组分均是由杜邦公司购买。
实施例1
将环化稻米支链淀粉(分子量为6.7×104g/mol，表面侧链平均链长DP27，内部环状结构平均尺寸DP 21和α-1,6糖苷键6.1％)溶解于pH7.0的缓冲盐溶液体系得到环化稻米支链淀粉的质量浓度10％的均一溶液，继续添加环化稻米支链淀粉质量2倍的葡萄花色苷混匀，得到环化稻米支链淀粉和葡萄花色苷的混合溶液；
将槲皮素溶解于纯乙醇得到槲皮素的质量浓度为5％的溶液，然后将其添加到前述环化稻米支链淀粉和葡萄花色苷的混合溶液中，搅拌混匀并调控混合体系乙醇浓度达到45％；置于功率250W、4℃超声场处理5min后，离心、沉淀干燥即得到目标产物——葡萄花色苷与槲皮素共包埋稳态化递送体系。
经过测定，葡萄花色苷与槲皮素共包埋稳态化递送体系中葡萄花色苷负载率85％，槲皮素负载率39％，其中葡萄花色苷与槲皮素共包埋稳态化递送体系中槲皮素的溶解度相较于天然疏水性槲皮素提高了74倍，制备得到的固态粒子(葡萄花色苷与槲皮素共包埋稳态化递送体系)平均尺寸为56μm。
实施例2
将环化玉米支链淀粉(分子量为2.8×105g/mol，表面侧链平均链长DP45，内部环状结构平均尺寸DP 34和α-1,6糖苷键7.0％)溶解于pH6.0的缓冲盐溶液体系得到环化玉米支链淀粉的质量浓度25％的均一溶液，继续添加环化玉米支链淀粉质量1倍的稻米蛋白短肽混匀，得到环化玉米支链淀粉和稻米蛋白短肽混合溶液；
将姜黄素溶解于纯乙醇得到姜黄素的质量浓度为3％的溶液，然后将其添加到前述环化玉米支链淀粉和稻米蛋白短肽混合溶液中，搅拌混匀并调控混合体系乙醇浓度达到40％；置于功率450W、0℃超声场处理3min后离心、沉淀干燥即得到目标产物——稻米蛋白短肽与姜黄素共包埋稳态化递送体系。
经过测定，稻米蛋白短肽与姜黄素共包埋稳态化递送体系中稻米蛋白短肽负载率91％，姜黄素负载率46％，其中稻米蛋白短肽与姜黄素共包埋稳态化递送体系中姜黄素的溶解度相较于天然疏水性姜黄素的溶解度提高了114倍，制备得到固态粒子(稻米蛋白短肽与姜黄素共包埋稳态化递送体系)平均尺寸为73μm。
实施例3
将环化小麦支链淀粉(分子量为1.2×105g/mol，表面侧链平均链长DP36，内部环状结构平均尺寸DP 28和α-1,6糖苷键5.9％)溶解于pH6.5的缓冲盐溶液体系得到环化小麦支链淀粉的质量浓度5％的均一溶液，继续添加环化小麦支链淀粉质量6倍的维生素C混匀，得到环化小麦支链淀粉和维生素C混合溶液；
将菜油固醇溶解于纯乙醇得到菜油固醇的质量浓度为10％的溶液，然后将其添加到前述环化小麦支链淀粉和维生素C混合溶液中，搅拌混匀并调控混合体系乙醇浓度达到55％；置于功率200W、10℃超声场处理8min后离心、沉淀干燥即得到目标产物——维生素C与菜油固醇共包埋稳态化递送体系。
经过测定，维生素C与菜油固醇共包埋稳态化递送体系中维生素C负载率95％，菜油固醇负载率61％，其中维生素C与菜油固醇共包埋稳态化递送体系中菜油固醇的溶解度相较于天然疏水性菜油固醇提高了174倍，制备得到的固态粒子(维生素C与菜油固醇共包埋稳态化递送体系)平均尺寸为69μm。
对比例1
参照实施例1，区别仅在于，将环化稻米支链淀粉替换为普通稻米淀粉，其他条件不变，得到目标产物——葡萄花色苷与槲皮素共包埋稳态化递送体系-1。
经过测定，对比例1制备的花色苷与槲皮素共包埋稳态化递送体系-1中葡萄花色苷负载率仅为13％，槲皮素负载率仅为6％，其中葡萄花色苷与槲皮素共包埋稳态化递送体系-1中槲皮素的溶解度的溶解度相较于天然疏水性槲皮素仅提高了2倍，制备得到固态粒子(葡萄花色苷与槲皮素共包埋稳态化递送体系-1)平均尺寸为127μm。
对比例2
参照实施例1，区别仅在于，将调控混合体系乙醇浓度达到45％调整为5％，其他条件不变，得到目标产物——葡萄花色苷与槲皮素共包埋稳态化递送体系-2。
经过测定，对比例2制备的葡萄花色苷与槲皮素共包埋稳态化递送体系-2中葡萄花色苷负载率仅为9％，槲皮素负载率仅为15％，其中葡萄花色苷与槲皮素共包埋稳态化递送体系-2中槲皮素的溶解度相较于天然疏水性槲皮素提高了18倍，制备得到固态粒子(葡萄花色苷与槲皮素共包埋稳态化递送体系-2)平均尺寸为97μm。
对比例3
参照实施例1，区别仅在于，省略置于功率250W和4℃超声场处理5min，其他条件不变，得到目标产物——葡萄花色苷与槲皮素共包埋稳态化递送体系-3。
经过测定，对比例3制备的葡萄花色苷与槲皮素共包埋稳态化递送体系-3中葡萄花色苷负载率仅为42％，槲皮素负载率仅为27％，其中葡萄花色苷与槲皮素共包埋稳态化递送体系-3中槲皮素的溶解度相较于天然疏水性槲皮素提高了36倍，制备得到固态粒子(葡萄花色苷与槲皮素共包埋稳态化递送体系-3)平均尺寸为75μm。
本文所描述的具体实施案例仅作为对本发明精神和部分实验做举例说明。本发明所述领域的技术人员可以对所描述的具体实施案例做出各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。

Claims (3)

1.一种多活性组分共包埋稳态化递送体系的加工方法，其特征在于，依次包括如下步骤：
（1）将环化支链淀粉溶解于pH6.0~7.0的缓冲盐溶液体系得到环化支链淀粉质量浓度5%~25%的均一溶液，继续添加亲水性活性组分混匀，得到环化支链淀粉和亲水性活性组分的混合溶液；环化支链淀粉与亲水性活性组分的质量比为1:（1~6）；
所述环化支链淀粉采用如下步骤制得：将粮谷作物籽粒胚乳分级处理得到支链淀粉，添加来源于嗜热脂肪芽孢杆菌Q酶反应2~12小时后得到环化支链淀粉，其中Q酶转苷酶活力>150 U；
所述环化支链淀粉的分子量为（6~30）×104 g/mol，表面侧链平均链长DP25~50，内部环状结构平均尺寸DP20~40且含α-1,6糖苷键5~7%；
（2）将疏水性活性组分溶解于纯乙醇，得到疏水性活性组分质量浓度为3-10%的溶液；然后将其添加到步骤（1）所得环化支链淀粉和亲水性活性组分的混合溶液中，搅拌混匀并调控混合体系中乙醇质量浓度达到40~55%；
（3）将步骤（2）所得体系置于功率200~500 W、0~10 ℃超声场处理3-20 min后，离心、沉淀干燥即得到目标产物—多活性组分共包埋稳态化递送体系。
2. 根据权利要求1所述的方法，其特征在于，在步骤（3）中，超声功率为200-450 W。
3.由权利要求1或2任一所述的方法制得的多活性组分共包埋稳态化递送体系。
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