CN114191381B - 一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶及其制备和应用 - Google Patents
一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶及其制备和应用 Download PDFInfo
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Abstract
本发明公开了一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶及其制备和应用。所述双凝胶包含质量比为2~5:5~8的油凝胶与复配水凝胶;所述油凝胶中油凝胶剂的浓度为3%~25%(w/w);所述复配水凝胶中热可逆型水凝胶剂A的浓度为1%~2%(w/w),热不可逆型水凝胶剂B的浓度为0.3%~1.5%(w/w)。本发明通过将油凝胶以及特定组成的复配水凝胶经热乳化、冷却凝胶法制得具备油凝胶‑水凝胶结构的特殊双凝胶体系,该双凝胶体系结构稳定性高,不易分层,且该双凝胶具备特殊的温敏型流变学特性,可在口腔温度下产生质构响应,具有口腔内感官以及消化道内消化行为可控的特性,为塑性脂肪替代品提供新型配方。
Description
技术领域
本发明属于凝胶制备技术领域,具体地,涉及一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶及其制备和应用。
背景技术
研究表明,高血压、高血脂、肥胖等诸多疾病都与高脂高热量饮食密切相关。因此,为了满足消费者对健康的日益重视,降低产品的热量和油脂含量尤为重要,基于此,脂肪替代品应运而生,到目前为止,已有多种替代品如蛋白质类,碳水化合物类,脂肪基类以及多种原料混合作为脂肪替代产品。然而,这些产品的结构容易受环境的变化而失去塑性脂肪的特性及口感,可塑性不高。
乳液凝胶同时包含乳液的结构特征和凝胶的特性,涵盖了两者的优良特性,是一种理想的脂肪替代物,对于品质优异的凝胶类脂肪替代物,需要其在口腔温度下产生不同的质构响应特征,以达到人们对食品口感的需求,有效替代传统塑性脂肪。专利CN202110687399.5提供了一种制备相变可调的乳液凝胶型脂肪替代物的方法及应用,将油溶性的多糖引入体系以降低油溶性小分子凝胶剂的使用量,制备出乳液凝胶型脂肪替代物。但该乳液凝胶型脂肪替代物并不具备口腔感官质构可调控和消化道程控的特征。
发明内容
本发明针对现有技术存在的不足,旨在提供一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶。本发明通过将油凝胶以及特定组成的复配水凝胶经热乳化、冷却凝胶法制得具备油凝胶-水凝胶结构的特殊双凝胶体系,该双凝胶体系的结构稳定性高、在口腔温度下流变学性质发生转变,且在消化道中的消化速率可控。
本发明的另一目的是提供所述双凝胶的制备方法。
本发明的另一目的是提供所述双凝胶在制备或作为代脂产品中的应用。
本发明的上述目的是通过以下技术方案实现的:
本发明首先提供了一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶,所述双凝胶包含:
(1)油凝胶;
(2)复配水凝胶;
所述油凝胶与复配水凝胶的质量比为2~5:5~8;
所述油凝胶中油凝胶剂的浓度为3%~25%(w/w);
所述复配水凝胶包含热可逆型水凝胶和热不可逆型水凝胶;所述复配水凝胶中热可逆型水凝胶剂A的浓度为1%~2%(w/w),热不可逆型水凝胶剂B的浓度为0.3%~1.5%(w/w)。
本发明上述双凝胶体系由特定的水凝胶与油凝胶复配而成,这种由水凝胶、油凝胶复配形成的结构与传统塑性脂肪如猪油的液体油与固体脂均匀融合的结构非常相似。具有油凝胶分散于水凝胶的乳液型凝胶结构以及油凝胶-水凝胶这种独特的双凝胶结构,结构稳定性高,且该双连续凝胶结构可有效延缓油脂的消化作用。该凝胶型制品可在零饱和脂肪酸、低油脂含量、零表面活性剂条件下模拟塑性脂肪质构特征。
本发明上述双凝胶体系中的水凝胶可取代猪油中的液体油,富含不饱和脂肪酸的油凝胶则取代猪油中的饱和脂肪酸;此外,随着复配水凝胶中热可逆凝胶、热不可逆凝胶比例的变化,双凝胶体系在口腔温度下产生不同的硬度、融化特征,表现不同的质构响应特征,可达到人们对食品口感的需求。比起传统塑性脂肪替代品,质构原料可调控的双凝胶既能满足人们健康饮食的需求,也能为人们带来更加丰富独特的口感,在口腔中能同时感觉到水相和油相,其在感官质构方面具有独特优势,因此可在口腔温度下产生不同的质构响应特征,可达到人们对食品口感的需求,有效替代传统塑性脂肪。
优选地,所述油凝胶与复配水凝胶的质量比为1:9或2:8或3:7或4:6或5:5。
最优选地,所述油凝胶与复配水凝胶的质量比为5:5。
优选地,所述热可逆型水凝胶剂A包括明胶、琼脂中的一种或几种;所述热不可逆型水凝胶剂B包括魔芋胶、甜菜果胶、柑橘果胶、瓜尔豆胶、刺云实胶中的一种或几种。
本发明上述双凝胶体系同时具有水凝胶及油凝胶特性,可用于同时、稳定地包埋油溶性和/或水溶性活性组分,双凝胶体系的结构性质处于凝胶与乳液之间,同时兼具二者的稳定性及双递送效果。
因此本发明上述双凝胶体系可作为双递送基质,负载油溶性活性组分和/或水溶性组分,起到提高活性物稳定性、增强生物利用度及健康效应的作用,在功能食品、药妆领域均具有独特的优势及广阔的应用发展空间。
优选地,所述油凝胶中还包含油溶性活性组分,包括但不局限于姜黄素、槲皮素、番茄红素中的一种或多种。
优选地,所述复配水凝胶中还包含水溶性活性组分,包括但不局限于迷迭香酸、茶多酚、水溶性维生素、花青素中的一种或多种。
本发明还提供了上述双凝胶的制备方法,包括如下步骤:
S1.油凝胶的制备:将油溶性活性组分、油凝胶剂分散在油脂中加热及搅拌至充分溶解,冷却得到油凝胶;
S2.复配水凝胶的制备:水溶性活性组分、热可逆型水凝胶剂A加入水中加热及搅拌至充分溶解,后加入热不可逆型水凝胶剂B,加热及剪切得到复配水凝胶;
S3.双凝胶的制备:将油凝胶和水凝胶加热及剪切,后冷却得到双凝胶。
优选地,步骤S1所述油凝胶剂包括乙基纤维素、卵磷脂、硬脂酸、蜂蜡中的任一种。
优选地,所述油脂包括甘油三酯、甘油二酯中的任一种。包括但不限于大豆油、葵花籽油、花生油、橄榄二酯食用油、亚麻籽二酯食用油中的一种或几种。
优选地,上述制备方法中,所述加热为在50~80℃下加热;所述冷却为在-20~25℃下冷却。
优选地,上述制备方法中,所述搅拌为在150~500rpm速率下磁力搅拌;所述剪切的速率为1000~10000rpm。
本发明的双凝胶具有模拟塑性脂肪质构特征的凝胶型制品,结构稳定性高,在口腔温度下其流变学性质发生改变,产生不同的质构响应特征,且此配方下的双凝胶能实现消化道的程控性释放效果,因此可进一步根据胃肠消化过程,设计在口腔中停留时间较长的食品,促进满足感;开发控制胃稳定性的食品增强饱腹感;创新消化慢的食品避免血糖或血脂水平升高。根据不同人群的需求,通过调控不同参数来实现理想的口腔感官效果及所需的消化道释放效果,满足人们健康饮食需求的同时也能为人们带来更加丰富独特的口感。
因此,上述温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶在本发明的保护范围内。
上述双凝胶在制备或作为代脂产品或在制备口腔感官质构、消化道消化行为可控产品中的应用亦在本发明的保护范围内。
本发明该双凝胶的结构性质处于凝胶与乳液之间,同时兼具二者的稳定性及双递送效果,能稳定地同时递送亲水性和疏水性功能活性成分或药物,具备较好的铺展性和水洗性,能改善活性成分的渗透性,增强角质层的水合作用和控制药物释放速率的能力。
因此,本发明还请求保护上述双凝胶在制备或作为药物或活性物递送载体中的应用。
与现有技术相比,本发明的有益效果是:
(1)本发明的双凝胶可在零饱和脂肪酸、低油脂含量、零表面活性剂条件下模拟塑性脂肪质构特征,且可在口腔温度下产生不同的硬度、融化特征,表现不同的质构响应特征,不仅可有效替代传统塑性脂肪,质构原料可调控的双凝胶更能满足人们对食品口感的个性化需求。
(2)本发明的双凝胶同时具有水凝胶及油凝胶特性,可用于同时、稳定地包埋油溶性及水溶性活性组分,通过调整油凝胶、水凝胶比例,以及复配水凝胶中热可逆凝胶、热不可逆凝胶的比例,可实现其在消化道中脂肪消化率、活性物释放速率的精准调控。
附图说明
图1为实例1制备的双凝胶制品宏观图;
图2为实例1制备的双凝胶制品的微观图;
图3为实例1制备的多组双凝胶制品流变图,A为不同油凝胶(O):水凝胶(W)比例的双凝胶制品的粘弹性温度扫描流变特性图;B为不同油凝胶(O):水凝胶(W)比例的双凝胶制品在室温下的应力扫描流变特性图;C为不同油凝胶(O):水凝胶(W)比例的双凝胶制品的粘度温度扫描流变特性图;D为不同油凝胶(O):水凝胶(W)比例的双凝胶制品的结构回复性扫描流变特性图;
图4为实例2制备的双凝胶制品的微观图(其中,图中的KGM代表魔芋胶,G代表明胶);
图5为实例2制备的多组双凝胶制品流变图,A为不同热可逆/热不可逆水凝胶比例的双凝胶制品的粘弹性温度扫描流变特性图,B为不同热可逆/热不可逆水凝胶比例的双凝胶制品在室温下的应力扫描流变特性图;C为热可逆/热不可逆水凝胶的双凝胶制品的粘度温度扫描流变特性图;D为不同热可逆/热不可逆水凝胶比例的双凝胶制品的结构回复性扫描流变特性图(其中,图中的KGM代表魔芋胶,G代表明胶);
图6为实例7包埋花青素的双凝胶制品及其微观结构图(右上);
图7为实例8包埋姜黄素的双凝胶制品及其微观结构图(右上);
图8为实例9包埋花青素及姜黄素的双凝胶制品及其微观结构图(右上)
图9为对比例1制备的样品宏观图;
图10为对比例2制备的双凝胶制品流变图,A为油凝胶:水凝胶(O5:W5)的双凝胶制品在室温下与实施例1的应力扫描流变特性对比图;B为油凝胶:水凝胶(O5:W5)的双凝胶制品与实施例1的粘度温度扫描流变特性对比图;C为油凝胶:水凝胶(O5:W5)的双凝胶制品与实施例1的结构回复性扫描流变特性对比图;
图11为对比例3制备的样品宏观图;
图12为对比例4制备的样品宏观图;
图13为对比例5制备的样品宏观图;
图14为实验例1油脂消化实验的游离脂肪酸释放曲线图。
具体实施方式
下面结合说明书附图和具体实施方式对本发明作进一步的说明,但实施例并不对本发明做任何形式的限定。除非另有说明,本发明实施例采用的原料试剂为常规购买的原料试剂。
实施例1不同油凝胶和复配水凝胶比例双凝胶的制备
本实施例提供了4种不同油凝胶和复配水凝胶比例的双凝胶。
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照2:8、3:7、4:6、5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双凝胶A(油凝胶和复配水凝胶2:8)、B(油凝胶和复配水凝胶3:7)、C(油凝胶和复配水凝胶4:6)、D(油凝胶和复配水凝胶5:5)。将制备的双凝胶A~D在4℃保存24℃小时。
2、样品测试
(1)制备得到的双凝胶A~D如图1所示,从图1可以看到,油水比2:8~5:5双凝胶体系的结构不会由于分层而被破坏,稳定性好。
图2为油凝胶和水凝胶按照2:8、3:7、4:6、5:5比例得到的双凝胶制品(左下)及其微观结构图,从图2可以看到,具有不同的油水比形成的双凝胶表现出不同的微观形态,在油凝胶组分相对较低(2:8、3:7、4:6)的体系中观察到清晰的油滴,表明形成O/W型双凝胶,而在油水比5:5的体系中则形成双连续凝胶。
(2)流变测试
1)方法
将制备得到的双凝胶A~D进行流变性测试,分别将双凝胶A~D样品铺在流变仪平板上,等待2分钟达到热平衡,然后进行流变实验。首先在应变振荡幅度扫描模式下确定双凝胶的线性粘弹性区域(LVR),然后在应力值为0.01%-1000%的范围内进行频率扫描,记录双凝胶体系的弹性模量G’和粘性模量G”数据;其次进行温度扫描,温度扫描试验分为动态粘弹性温度扫描和动态粘度温度扫描两个部分,温度扫描从4℃开始,以5℃/min的升温速率加热至60℃结束,选用直径为40mm的铝制平板夹具,间隙设定为1000μm,应变范围设定为1%(在线性粘弹区域内),角频率为6.283rad/s。最后进行结构回复性扫描,每个样品做3次平行实验,测量后从电脑中导出结果,进行绘图。
2)结果
图3为本实施例按照不同油凝胶:复配水凝胶比例制备的双凝胶制品的流变测试图,其中,A图为4~60℃下粘弹性温度扫描流变特性图,表明所制备的双凝胶制品的弹性模量随温度的升高而下降,在37℃有明显的下降趋势,能很好地模拟塑性脂肪在口腔中融化的流变特性;B图为在室温下的应力扫描流变特性图,不同油水比制备的双凝胶的G均大于G”,即样品的弹性模量大于粘性模量,有更明显的固相特性,抗形变能力越强,结构越稳定;C图为在4~60℃下的粘度温度扫描流变特性图,可以看到,制备的双凝胶制品的粘度随温度的升高变化而下降,在27℃~37℃有明显的下降趋势,表明其可在口腔温度下产生不同的硬度、融化特征,表现不同的质构响应特征,可达到人们对食品口感的需求,可有效替代传统塑性脂肪,质构原料可调控的双凝胶既能满足人们健康饮食的需求,也能为人们带来更加丰富独特的口感;D图为结构回复性扫描流变特性图,可以看到,随着油水比例的增大(即油凝胶相的增加),双连续凝胶结构恢复率逐渐增大,由于体系的抗形变能力主要由物体的弹性所贡献,再结合相关流变数据可知,油凝胶组分含量越高,其G’>G”,弹性性能越好,所以抗形变能力越强,因此具有更高的恢复率,即双凝胶结构更稳定。综上,可以调控油水相比例来实现理想的口腔感官效果,满足人们健康饮食需求的同时也能为人们带来更加丰富独特的口感。
(3)质构测试
1)方法
设置TPA模式设置具体参数为:探头型号为P/36R,触发力为5g,测前速递2mm/s,测定速度为1mm/s,测后速递2mm/s,压缩程度60%,两次压缩时间间隔为5s。分别测试双连续凝胶A~D的硬度、粘性、弹性、内聚性、胶粘性、耐咀性、回复性。
2)结果
表1
表1为双凝胶A~D的质构测试结果,从表1可以看到,随着油水比的增加(即油相增加),粘度上升,趋势明显。而硬度和耐咀性则先上升后下降,在油水比5:5时的数据恰恰说明油水比5:5时制备的是双连续型凝胶,结合之前的微观结构图片,油相不再是连续相,它的结构改变才会出现油相的比例增大了,但是质构特性中的硬度反而降低。同时可以根据不同人群的不同需求,通过设计不同油水比例来调控双凝胶制品的软硬程度、粘弹性、内聚性以及耐咀嚼性等。
实施例2不同热可逆/热不可逆水凝胶比例制备的双凝胶
本实施例提供了4种不同热可逆/热不可逆水凝胶比例制备的双连续凝胶。
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双连续凝胶E~H在4℃保存24℃小时。
其中双连续凝胶E的复配水凝胶中,明胶浓度(1.875%,w/w),魔芋胶浓度(0.375%,w/w);
双连续凝胶F的复配水凝胶中,明胶浓度(1.607%,w/w),魔芋胶浓度(0.643%,w/w);
双连续凝胶G的复配水凝胶中,明胶浓度(1.25%,w/w),魔芋胶浓度(1%,w/w);
双连续凝胶H的复配水凝胶中,明胶浓度(1.023%,w/w),魔芋胶浓度(1.227%,w/w)。
2、样品测试
微观结构,流变测试同实施例1,结果表明:如图4为不同热可逆/热不可逆水凝胶比例按照1:5、2:5、4:5、6:5比例制备得到的双凝胶制品(左下)及其微观结构图,从图4可以看到,具有不同热可逆/热不可逆水凝胶比例形成的双凝胶表现出类似的微观形态,这也表明形成双连续凝胶的关键因素是一定比例的油水比(即5:5)。
图5为本实施例制备的双凝胶制品的流变测试图,其中,A图为4~60℃下粘弹性温度扫描流变特性图,表明所制备的双凝胶制品的弹性模量G’均大于粘性模量G”,有很好的固相属性,满足人们对口感的追求,且随温度的升高而下降,在37℃有明显的下降趋势,能很好地模拟塑性脂肪在口腔中融化的流变特性;B图为在室温下的应力扫描流变特性图;C图为在4~60℃下的粘度温度扫描流变特性图,可以看到,制备的双凝胶制品的粘度随温度的升高变化而下降,在30℃~40℃有明显的下降趋势,表明其可在口腔温度下产生不同的硬度、融化特征,表现不同的质构响应特征;D图为结构回复性扫描流变特性图,可以看到,随着水凝胶复配比例的增大(即魔芋胶浓度的增加),双连续凝胶结构恢复率逐渐降低,说明双凝胶结构的回复性主要由明胶贡献,由此可通过调控水凝胶的不同比例来调控稳定性,实现理想的口腔感官效果,满足人们健康饮食需求的同时也能为人们带来更加丰富独特的口感。
实施例3一种双凝胶
(1)油凝胶的制备:将蜂蜡(5%,w/w)分散在葵花籽油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将琼脂(1.5%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向琼脂水溶液中添加瓜尔豆胶(0.3%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照2:8、的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双连续凝胶。
实施例4一种双凝胶
(1)油凝胶的制备:将蜂蜡(5%,w/w)分散在玉米油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(2%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向琼脂水溶液中添加甜菜果胶(0.5%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照3:7的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双连续凝胶。
实施例5一种双凝胶
(1)油凝胶的制备:将蜂蜡(5%,w/w)分散在花生油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将琼脂(1.5%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向琼脂水溶液中添加柑橘果胶(1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照4:6的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却,得到双连续凝胶。
实施例6一种双凝胶
(1)油凝胶的制备:将蜂蜡(5%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向琼脂水溶液中添加瓜尔豆胶(1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双连续凝胶。
实施例7一种包埋花青素的双凝胶制品的制备
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.75%,w/w)分散在含有花青素(0.3%,w/w)的蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(0.75%,w/w)并保持温度在75℃使其充分浸润溶解,并且在3000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照3:7的比例75℃、6000rpm高速剪切混合2min,然后将混合物立即转移到-20℃冰箱冷却6分钟,促进两相凝胶和双凝胶的形成,制备的双凝胶在4℃保存24℃小时。
图6为包埋花青素的双凝胶制品及其微观结构图(右上),从图中可以看到呈现双连续凝胶结构。
实施例8一种包埋姜黄素的双凝胶制品的制备
(1)油凝胶的制备:将卵磷脂(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,加入油溶性活性组分姜黄素(0.05%,w/w)并溶解在上述配方中,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(1.25%,w/w)并保持温度在75℃使其充分浸润溶解,并且在9000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照4:6的比例75℃、5000rpm高速剪切混合2min,然后将混合物立即转移到-20℃冰箱冷却6分钟,促进两相凝胶和双凝胶的形成,制备的双凝胶在4℃保存24℃小时。
图7为包埋姜黄素的双凝胶制品及其微观结构图(右上),从图中可以看到呈现双连续凝胶结构。
实施例9一种同时包埋花青素及姜黄素的共递送双凝胶制品的制备
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,加入油溶性活性组分姜黄素(0.05%,w/w)并溶解在上述配方中,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.5%,w/w)分散在含有花青素(0.5%,w/w)的蒸馏水中,并在150rpm、60℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(1%,w/w)并保持温度在60℃使其充分浸润溶解,并且在6000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照5:5的比例75℃、5000rpm高速剪切混合2min,然后将混合物立即转移到-20℃冰箱冷却6分钟,促进两相凝胶和双凝胶的形成,制备的双凝胶在4℃保存24小时。
图8为包埋花青素及姜黄素的双凝胶制品及其微观结构图(右上),从图中可以看到呈现双连续凝胶结构。
对比例1
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2水凝胶的制备:将明胶(2.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和水凝胶分别按照2:8、3:7、4:6、5:5的比例在75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双凝胶,制备的双凝胶在4℃保存24小时。
2、样品测试
对比例1制备得到的样品如图9所示,从图9可以看到,使用单一水凝胶按照油水比2:8~5:5制备的样品体系结构易分层,其不能形成双凝胶,且结构稳定性不好。
对比例2
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2水凝胶的制备:将魔芋胶(2.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,冷却形成复配水凝胶。
(4)双凝胶的制备:油凝胶和水凝胶分别按照5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双凝胶,制备的双凝胶在4℃保存24小时。
3、样品测试
流变测试同上,结果表明,图10为对比例2制备的双凝胶制品流变图,A为油凝胶:水凝胶(5:5)的双凝胶制品在室温下与实施例1的应力扫描流变特性对比图,由图可知,对比例2的屈服应力(G’=G”)小于实施例1的屈服应力,表明其抗形变能力比较弱,结构稳定性不好;B为油凝胶:水凝胶(5:5)的双凝胶制品与实施例1的粘度温度扫描流变特性对比图,由图可知,制备的双凝胶制品的粘度随温度的升高变化而下降,但在口腔温度37℃左右没有有明显的下降趋势,表明其不可在口腔温度下产生不同的硬度、融化特征,不能表现不同的质构响应特征;C为油凝胶:水凝胶(5:5)的双凝胶制品与实施例1的结构回复性扫描流变特性对比图,从图中可以看到,其结构回复性不及实施例1的回复率高。综上,其不可以调控油水相比例来实现理想的口腔感官效果,不能满足人们健康饮食需求的同时也不能为人们带来更加丰富独特的口感。
对比例3
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将海藻酸钠(1.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后滴加1%氯化钙使其凝胶,最后向海藻酸钠凝胶中添加黄原胶(1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双凝胶,制备的双凝胶在4℃保存24小时。
2、样品测试
对比例3制备得到的样品如图11所示,从图11可以看到,使用海藻酸钠作为水相凝胶剂制备成的水凝胶会出现局部成胶的现象(图11的a),并且它与黄原胶复配不能形成双凝胶。
对比例4
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(0.5%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(0.1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照5:5的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到双凝胶,制备的双凝胶在4℃保存24小时。
2、样品测试
对比例4制备得到的样品如图12所示,可以看到,此浓度下的水凝胶和油凝胶不能形成双凝胶体系。
对比例5
本对比例提供了4种不同油凝胶和复配水凝胶配比的凝胶。
1、制备方法
(1)油凝胶的制备:将硬脂酸(3%,w/w)分散在大豆油中,使其在150rpm磁力搅拌,75℃下加热直至溶解,将热溶液冷却至室温形成油凝胶。
(2)复配水凝胶的制备:将明胶(1.25%,w/w)分散在蒸馏水中,并在150rpm、75℃中加热直至完全溶解,然后向明胶水溶液中添加魔芋胶(1%,w/w)并保持温度在75℃使其充分浸润溶解,并且在8000rpm下剪切1min后冷却形成复配水凝胶。
(3)双凝胶的制备:油凝胶和复配水凝胶分别按照6:4、7:3;8:2、9:1的比例75℃、9000rpm高速剪切混合3min,然后将混合物立即转移到-20℃冰箱冷却6分钟,得到4种凝胶体系,在4℃保存24℃小时。
2、样品测试
对比例5制备得到的4个样品如图13所示,从图13可清楚看到,制备的样品虽然能成凝胶,但是在成胶之前油水相就已经分层,结构不稳定。此对比例说明形成双凝胶的前提是需要适当比例的油水相。
实验例1油脂消化实验
1、实验方法
模拟小肠消化
研究油水比为5:5的双连续凝胶与油水比2:8、3:7、4:6水包油型双凝胶经口服摄入后在模拟小肠液中脂质的消化特性。将1g胰酶溶解于5mL脂解缓冲液(50mM马来酸、150mM氯化钠、5mM无水氯化钙、20mM牛脱氧胆酸钠、5mM大豆卵磷脂),磁力搅拌(500rpm、15min),然后在4℃下冷藏制得胰酶储液。将25mL脂解缓冲液搅拌热水浴10min,加入模拟胃液消化完毕的样品,用0.25M NaOH调节pH至7.2,混合液温度达到37℃后,加入2.8mL冰冷的胰酶储液开始消化。在脂解过程中,通过手动添加0.25M NaOH使pH维持在7.20±0.02。记录2h脂肪分解实验中NaOH随时间的消耗量,用于计算脂肪分解产生的游离脂肪酸的浓度。
2、实验结果
如图14所示,由于油水比2:8、3:7、4:6制备的是的水包油型双凝胶,而油水比5:5是双连续凝胶,图14的结果表明,相对于水包油型双凝胶而言,油水比5:5的双连续凝胶具有明显的延缓油脂消化效果。
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。
Claims (9)
1.一种温敏型模拟塑性脂肪、口腔质构及消化行为可控的双凝胶,其特征在于,所述双凝胶由质量比为2~5:5~8的油凝胶与复配水凝胶组成;
所述油凝胶中油凝胶剂的浓度为3%~25%(w/w);
所述复配水凝胶包含热可逆型水凝胶和热不可逆型水凝胶;所述复配水凝胶中热可逆型水凝胶剂A的浓度为1%~2%(w/w),热不可逆型水凝胶剂B的浓度为0.3%~1.5%(w/w);所述热可逆型水凝胶剂A选自明胶、琼脂中的一种或几种;所述热不可逆型水凝胶剂B选自魔芋胶、甜菜果胶、柑橘果胶、瓜尔豆胶中的一种或几种;所述油凝胶剂选自卵磷脂、硬脂酸、蜂蜡中的任一种。
2.根据权利要求1所述双凝胶,其特征在于,所述油凝胶中负载油溶性活性组分。
3.根据权利要求1所述双凝胶,其特征在于,所述复配水凝胶中负载水溶性活性组分。
4.权利要求1~3任一所述双凝胶的制备方法,其特征在于,包括如下步骤:
S1.油凝胶的制备:将油溶性活性组分、油凝胶剂分散在油脂中加热及搅拌至充分溶解,冷却得到油凝胶;
S2.复配水凝胶的制备:水溶性活性组分、热可逆型水凝胶剂A加入水中加热及搅拌至充分溶解,后加入热不可逆型水凝胶剂B,加热及剪切得到复配水凝胶;
S3.双凝胶的制备:将油凝胶和水凝胶加热及剪切,后冷却得到双凝胶。
5.根据权利要求4所述方法,其特征在于,步骤S1所述油脂选自甘油三酯、甘油二酯中的任一种。
6.根据权利要求4所述方法,其特征在于,所述加热为在50~80℃下加热;所述冷却为在-20~25℃下冷却;所述搅拌为在150~500rpm速率下磁力搅拌;所述剪切的速率为1000~10000rpm。
7.权利要求4~6任一所述方法制备得到的双凝胶。
8.权利要求1~3任一所述双凝胶或权利要求4~6任一所述方法制备得到的双凝胶在制备代脂产品或制备消化道消化行为可控产品中的应用。
9.权利要求1~3任一所述双凝胶或权利要求4~6任一所述方法制备得到的双凝胶在制备药物或活性物递送载体中的应用。
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