CN109674751B - 一种高包埋率花色苷乳液的制备方法 - Google Patents
一种高包埋率花色苷乳液的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高包埋率花色苷乳液的制备方法。该方法先用辛烯基琥珀酸酐对平均粒径为1~5μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.028~0.100的改性小粒径淀粉颗粒;将花色苷提取物和亲脂性乳化剂分别溶解在水和油并混合,经高速剪切得W/O乳液;然后将改性小粒径淀粉颗粒按质量分数1~8%(w/w)均匀分散于蒸馏水中,与W/O乳液混合高速剪切得负载花色苷乳液。本发明方法制备的花色苷乳液包埋率高,工艺简单,油脂含量少,可应用于食品饮料、化妆品水乳等领域。
Description
技术领域
本发明涉及一种花色苷的制剂技术,具体涉及一种负载活性成分花色苷的乳液及其制备方法,特别涉及一种以花色苷为活性成分的微米级淀粉基W/O/W乳液的制备方法,属于食品、药品和化妆品制备技术领域。
背景技术
花色苷(Anthocyanins),是一类水溶性天然食用色素,属黄酮类化合物,具有C6-C3-C6碳骨架结构,由花青素(Anthocyanidin)在自然状态下与各种糖结合形成,广泛存在于植物中,使植物呈现蓝、红、黄或紫色,通常来源于葡萄皮、蓝莓、越橘、红叶卷心菜、紫甘薯、黑枸杞等。花色苷除了是一种广泛存在于植物中的水溶性天然色素,也是一种重要的生物活性物质。近年来,大量的体外和体内实验证明花色苷具有抗氧化性,清除自由基功能,抗肿瘤、抗癌症、抗炎、抗菌,抑制脂质过氧化和血小板凝集,保护肝脏,预防糖尿病,预防肥胖,保护视力等。Prior等(Journal ofAgricultural&FoodChemistry,2010,58(7):3970-3976)发现纯化的花色苷能降低小鼠血清中的瘦素水平,在预防肥胖上起一定作用。Miyake等(Laboratory Investigation,2011,92(1):102-109)研究表明富含花色苷的越橘提取物对视网膜炎症期间的视觉功能具有保护作用。由于花色苷具有保健功效,近年来对其开发与有关产品应用成为研究热点。
虽然花色苷能赋予食物丰富的色彩,但花色苷本身含有大量极不稳定的酚羟基,其稳定性受自身结构影响很大。同时,花色苷的稳定性还与加工和贮藏过程中的一些理化因子,如pH、温度、光、氧、酶、抗坏血酸、糖及其降解产物、二氧化硫、氨基酸、酚酸、金属离子、加工方法等有关,因此限制了花色苷在食品工业中的应用。
目前,国内外常用的稳定花色苷的方法主要为微胶囊化法,常用的壁材有碳水化合物类、植物水溶性胶类和蛋白类。常用的碳水化合物类微胶囊壁材有淀粉、壳聚糖、糊精、小分子糖类等。除淀粉外,其他碳水化合物类壁材都需要与蛋白、胶体等复配使用,因为单一使用某种壁材效果较差。亲水性胶体壁材包括海藻胶提取物类如海藻酸盐、微生物发酵及代谢产物类如黄原胶、植物分泌物类如阿拉伯胶等。蛋白质类微胶囊壁材有大豆蛋白、明胶、乳清蛋白等。喷雾干燥法制备花色苷微胶囊虽然包埋效果不低,但存在不足:1)大多采用喷雾干燥法,微胶囊颗粒大小难以控制,温敏材料容易发生降解;2)制备的形式为固体形式居多,主要应用到固态和半固态产品开发,较少应用到液态食品和高端食品,如口服液等保健食品,应用范围受限。
乳液是两个互不相溶的液相的混合物,其中一相作为液滴分散在另一个相中,主要有两种形式:油滴分散在连续相水中称为水包油(O/W)乳液,水滴分散在连续相油中称为油包水(W/O)乳液。将由固体颗粒作为乳化剂稳定的乳液称为Pickering乳液。
发明内容
本发明的目的在于提供一种高效、工艺简单、包埋率高且较为稳定的包埋花色苷的乳液体系,是对花色苷的包埋提供新的方法,也是对现有双重乳液体系的应用的拓展。
本发明具体技术方案如下:
一种高包埋率花色苷乳液的制备方法,其特征在于包埋如下步骤:
(1)改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1~5μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.028~0.100的改性小粒径淀粉颗粒;
(2)将亲脂性乳化剂溶解在液态油脂中,作为油相,按浓度为0.5~6%(w/v)进行溶解,将商品化的花色苷提取物溶解到蒸馏水,作为内水相中,将内水相和油相混合,高速剪切得到油包水乳液(W-O乳液),剪切转速为15000~26000rpm,剪切时间为2~5min;
(3)将步骤(1)所得的改性小粒径淀粉颗粒按1~8%的质量分数均匀分散于蒸馏水中,高速剪切使其分散,剪切转速18000~26000rpm,时间10~60s,形成淀粉颗粒悬浮液,作为外水相;将步骤(2)得到的W-O乳液加入到外水相,高速剪切,剪切转速为10000~18000rpm,剪切时间为1~4min,制备得花色苷乳液。
本发明进一步技术方案在于,步骤(2)中,所述的亲脂性乳化剂为单硬脂酸甘油酯、聚甘油蓖麻醇酯、Span 80、卵磷脂中的一种或几种。
所述的液态油脂为玉米油、葵花籽油、大豆油、棕榈油中的一种或者几种。
所述的花色苷提取物溶解到蒸馏水的浓度为1~5%(w/v)。
所述的商品化的花色苷提取物的来源可以是蓝莓、欧洲越橘、葡萄籽或黑树莓中的一种或者几种。
所述的油包水乳液内水相和油相的体积比为1:9、2:8、3:7、4:6或5:5。
本发明进一步技术方案在于,所述W-O初乳与外水相的体积比为7:3、6:4、5:5、4:6或3:7。
一种保护花色苷的方法,其特征在于,利用如上任意一项所述的制备方法对花色苷进行包埋。
一种提高花色苷包埋率的方法,其特征在于,利用权利要求1-3任意一项所述的制备方法对花色苷进行包埋。
一种高包埋率的花色苷包埋物,其特征在于,利用如上任意一项所述的制备方法所制备的产物。
利用如上任意一项所述的制备方法所制备的产物在制备食品或者化妆品或者药品中的用途。
一种高包埋率花色苷乳液的制备方法,其特征在于,具体步骤如下:
a.改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
b.称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
c.称取0.28g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
d.取3mL步骤b得到的内水相,与步骤c得到的油相混合,高速剪切20000r/min,3min,获得W-O初乳;
e.称取步骤a得到的改性小粒径淀粉颗粒0.4g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
f.取步骤d所得W-O初乳,与步骤e所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的W-O-W双重乳液;
所得的W-O-W双重乳液对花色苷的包埋率为97.1%,平均粒径为42.163μm。
一种高包埋率花色苷乳液的制备方法,其特征在于,具体步骤如下:
a.改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
b.称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
c.称取0.14g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
d.将步骤b得到的内水相与步骤c得到的油相按一定的体积比混合,高速剪切20000r/min,3min,获得W-O初乳;
e.称取步骤a得到的改性小粒径淀粉颗粒0.6g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
f.取步骤d所得W-O初乳,与步骤e所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的W-O-W双重乳液;
所得的W-O-W双重乳液对花色苷的包埋率为97.2%,平均粒径为30.721μm。
本发明与现有技术相比,具有以下优点:
1)工艺简单:采用两步法,都只经过高速剪切2~3min,就获得稳定的包埋花色苷的W/O/W双重乳液,简便易行。
2)制备的双重乳液与传统的水包油乳液相比,降低了油脂的用量,与目前提倡的低脂食品趋势符合;与传统的W/O乳液相比,把水溶性的花色苷溶解在内水相中,外层再吸附一层淀粉颗粒形成Pickering乳液,既很好地保护花色苷,降低光照、氧气等条件下花色苷的降解,又使最外层为水,在食品工业、化妆品领域有更广泛的应用。
3)包埋率高:本方法的花色苷包埋率可达95%以上,与传统的喷雾干燥和其他方式包埋方式的包埋率85%相比,有所提高。
附图说明
为了进一步说明本发明,下面结合附图进一步进行说明:
图1为实施例1中制备的花色苷乳液微观结构和表观图
图2为实施例2中制备的花色苷乳液微观结构和表观图
图3为实施例3中制备的花色苷乳液微观结构和表观图
图4为花色苷包埋率的测定计算公式
具体实施方式
为更好地理解本发明,下面结合实施例对本发明做进一步说明,但本发明的实施方式不限于此。本发明实施例中有关测定方法说明如下:
1、花色苷包埋率的测定:
取2ml乳液于4ml蒸馏水中,摇晃均匀,使乳液分散,外水相更好分散在水中。离心,4000rpm,10min,用注射器取下层清液,过PES水系滤膜得到滤液,用pH示差法测得滤液中的花色苷含量。用下式计算出双重乳液对花色苷的包埋率:
D:稀释倍数(稀释液体积/双重乳液体积)。
2、乳液性质测定:
1)粒度分布:乳液粒度分布采用马尔文2000粒度仪进行测定:分别设定油和水的折光系数,光吸收指数设定为0.001,每个样品重复测定3次;液滴平均粒径用平均粒径d[0.5]表示。
2)形貌观察:利用OlympusBH-2型光学显微镜进行观测,放大倍数为500倍。
3)激光共聚焦观察:将大豆油用0.01%的尼罗红染液进行染色,将改性的小颗粒淀粉用0.01%的尼罗蓝染液进行染色,进行乳液的制备,在488nm和633nm的激发波长下观察乳滴的形态和分布。
实施例1
一种高包埋率的花色苷乳液的制备方法,具体步骤如下:
1、改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0286的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.28g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得油包水(W-O)乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.4g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的乳液。
所得的乳液如图1所示,由图中的表观现象看,此条件下未能形成均一的乳液体系,出现明显的分层,上层为W-O乳液,下层为淀粉颗粒;从显微图片看,没有均匀分布的乳滴,说明未能形成稳定的W-O-W双重乳液。这是由于改性之后的小粒径淀粉颗粒表面的酯化取代度不够,仍有较多羟基,亲水强而疏水性弱,导致其乳化能力差,不能在水油界面稳定,因此形成不了均一的W-O-W乳液。
实施例2
一种高包埋率的花色苷乳液的制备方法,具体步骤如下:
1、改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.07g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得W-O乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.4g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷乳液。
所得的乳液对花色苷的包埋率为74.4%,平均粒径为36.504μm,其显微图片和表观图片如图2所示。从表观图片看出,形成的乳液不是很均匀,部分乳液中间存在断层,有花色苷溶液裸露;从显微图片看出形成乳滴较大,但分布均匀。
实施例3
一种高包埋率花色苷乳液的制备方法,具体步骤如下:
1、改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.28g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得W-O乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.4g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的乳液。
所得的乳液对花色苷的包埋率为97.1%,平均粒径为42.163μm,其显微图片和表观图片如图3所示。由表观图片看出,形成了均一的乳液,从显微图片看到均匀分布的乳滴。说明随着取代度的增加,小粒径淀粉颗粒表面的疏水基团增加了,即乳化性能提高了,使水油界面的淀粉覆盖率增加,通过调整油水体积分数,使乳液体系絮凝程度增加,从而形成均一的体系。对比实施例3和实施例2,随着PGPR添加量的增加,对花色苷的包埋率逐渐增加。从表观现象看,随着PGPR含量的增加,乳液形成体系更为均一,与包埋率的数据一致;从显微图片看,随着PGPR含量的增加,乳滴的出现不透光现象,乳滴粒径有减小的趋势。
实施例4
一种高包埋率花色苷乳液的制备方法,具体步骤如下:
1、改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1.6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.14g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得W-O乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.6g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的乳液。
所得的乳液对花色苷的包埋率为97.2%,平均粒径为30.721μm。
本发明以辛烯基琥珀酸酐改性小粒径淀粉颗粒制备W-O-W双重乳液,并以此为载体包埋花色苷,包埋率高达95%以上,乳滴粒径在40μm左右。W-O-W双重乳液的制备工艺简单,耗时短,所需设备少,包埋率高;同时,制备的W-O-W双重乳液与传统的W-O乳液或O-W乳液相比,既使花色苷溶解在内水相,又增加一层淀粉颗粒吸附在外层油水界面,阻隔光线和氧气,增强保护效果;同时,脂肪用量减小,符合低脂食品的发展趋势,可作为开发减肥产品的基础;另外,最外层为水相,食品工业乳液大多以水作为连续相,该体系能更好地应用到食品工业。本发明以淀粉基W-O-W双重乳液为载体包埋花色苷,可以将其包裹在明胶胶囊中,应用于食品领域常见的功能性饮料、涂抹酱、胶囊保健品以及化妆品领域的水乳和医药领域的口服液、胶囊等。
需要说明的是,本专利提供的多个方案包含本身的基本方案,相互独立,并不相互制约,但是其也可以在不冲突的情况下相互结合,达到多个效果共同实现。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本领域的技术人员应该了解本发明不受上述实施例的限制,上述实施例和说明书中描述的知识说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的范围内。
Claims (5)
1.一种高包埋率花色苷乳液的制备方法,其特征在于,具体步骤如下:
1、改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1 .6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.28g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得W-O乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.4g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的乳液;
所得的乳液对花色苷的包埋率为97.1%,平均粒径为42.163μm,形成了均一的乳液。
2.一种高包埋率花色苷乳液的制备方法,其特征在于具体步骤如下:
1 、 改性小粒径淀粉颗粒的制备:用辛烯基琥珀酸酐对平均粒径为1 .6μm的小粒径淀粉颗粒进行酯化改性,得到取代度为0.0421的改性小粒径淀粉颗粒;
2、称取2g的欧洲越橘花色苷提取物,加水溶解并定容到100mL,得到浓度为2%(w/v)的花色苷提取物水溶液;
3、称取0.14g聚甘油蓖麻醇酯(PGPR)于7mL大豆油中,磁力搅拌1h;
4、取3mL步骤2得到的内水相,与步骤3得到的油相混合,高速剪切20000r/min,3min,获得W-O乳液;
5、称取步骤1得到的改性小粒径淀粉颗粒0.6g,均匀分散在5mL的水中,形成淀粉颗粒悬浮溶液;
6、取步骤4所得W-O乳液,与步骤5所得的悬浮溶液混合,按体积比为5:5混合,高速剪切15000r/min,2min,得到包埋花色苷的乳液;
所得的乳液对花色苷的包埋率为97.2%,平均粒径为30.721μm。
3.一种保护花色苷的方法,其特征在于,利用权利要求1-2任意一项所述的制备方法对花色苷进行包埋。
4.一种提高花色苷包埋率的方法,其特征在于,利用权利要求1-2任意一项所述的制备方法对花色苷进行包埋。
5.一种高包埋率的花色苷包埋物,其特征在于,利用权利要求1-2任意一项所述的制备方法所制备的产物。
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