CN111955746A - 牡蛎肽-鱼油复合微凝胶及其制备方法 - Google Patents
牡蛎肽-鱼油复合微凝胶及其制备方法 Download PDFInfo
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- CN111955746A CN111955746A CN202010908436.6A CN202010908436A CN111955746A CN 111955746 A CN111955746 A CN 111955746A CN 202010908436 A CN202010908436 A CN 202010908436A CN 111955746 A CN111955746 A CN 111955746A
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- fish oil
- oyster peptide
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- oyster
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Abstract
本发明提供一种牡蛎肽‑鱼油复合微凝胶及其制备方法,牡蛎肽‑鱼油复合微凝胶包括牡蛎肽水溶液、鱼油和乳化剂的油包水型乳液,并且所述油包水型乳液分散在海藻酸钠与氯化钙交联形成的三维网状凝胶结构中。本发明的微凝胶能够对牡蛎肽起到缓释及活性保护作用,而且掩盖了鱼油和牡蛎肽的腥味,防止鱼油的氧化变质,使鱼油和牡蛎肽得以结合,提高了鱼油、牡蛎肽的利用率以及利用价值。
Description
技术领域
本发明涉及水产提取物的技术领域,尤其涉及一种牡蛎肽-鱼油复合微凝胶及其制备方法。
背景技术
牡蛎肽是以牡蛎肉为原料,经酶解、精制而得的小分子低聚肽,具有多种生物功能活性。尽管牡蛎肽具有多种功效,但是在胃肠道消化过程中,由于胃内酸性条件及消化蛋白酶的作用,牡蛎肽可能会发生进一步降解,甚至失去功效活性。
鱼油是由深海鱼经一系列复杂工艺提取而得,富含磷脂、ε-3多不饱和脂肪酸、多种维生素以及微量元素。
由于来源于海洋,牡蛎肽及鱼油均具有一定程度的腥味,加之鱼油中富含EPA、DHA等多不饱和脂肪酸,对氧、光及热极为敏感,易发生氧化,丧失功能活性。现有技术中通过脱氧包装方法、添加抗氧化剂、迷迭香除异味以及酸洗等方法来防止鱼油腐败变质、脱除异味,但是上述方法都存在一定的弊端,比如添加剂会对食品本身造成一定的影响,而且添加剂的过量摄入会影响人体健康。
由于上述问题,限制了牡蛎肽和鱼油在健康食品工业中的应用,也限制了牡蛎肽和鱼油的药用价值。
发明内容
鉴于上述问题,本发明的一个实施方式提供一种牡蛎肽-鱼油复合微凝胶,包括牡蛎肽水溶液、鱼油和乳化剂的油包水型乳液,并且所述油包水型乳液分散在海藻酸钠与氯化钙交联形成的三维网状凝胶结构中。
在上述的牡蛎肽-鱼油复合微凝胶中,所述乳化剂包括司盘80。
在上述的牡蛎肽-鱼油复合微凝胶中,所述鱼油和乳化剂的总体积与所述牡蛎肽水溶液的体积之比为4.5:5.5至8:2,优选5:5至6:4,更优选5:5。
在上述的牡蛎肽-鱼油复合微凝胶中,所述牡蛎肽水溶液中牡蛎肽的质量百分比浓度为3~7%,优选4~6%。
在上述的牡蛎肽-鱼油复合微凝胶中,所述乳化剂相对于所述乳化剂和所述鱼油之和的质量百分比为1~3%,优选1.8~2.2%。
在上述的牡蛎肽-鱼油复合微凝胶中,牡蛎肽的分子量小于5000道尔顿,优选小于3000道尔顿,更优选小于1000道尔顿。
本发明的另一实施方式提供一种牡蛎肽-鱼油复合微凝胶的制备方法,包括:
利用牡蛎肽水溶液、鱼油和乳化剂形成油包水乳液;
将所述油包水乳液与海藻酸钠胶体溶液混合形成水包油包水乳液;
将所述水包油包水乳液滴加至氯化钙水溶液中,使得氯化钙与海藻酸钠交联后形成所述牡蛎肽-鱼油复合微凝胶。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,利用注射器将所述水包油包水乳液滴加至氯化钙水溶液中。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,所述乳化剂优选司盘80。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,所述鱼油和乳化剂的总体积与所述牡蛎肽水溶液的体积之比4.5:5.5至8:2,优选5:5至6:4,更优选5:5。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,所述牡蛎肽水溶液中牡蛎肽的质量百分比浓度为3~7%,优选4~6%。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,将鱼油和所述乳化剂预先混合形成油相混合物,所述油相混合物中所述乳化剂的质量百分比为1~3%,优选1.8~2.2%。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,所述油包水乳液与海藻酸钠胶体溶液的体积比为1:0.8~1:5,优选1:1~1:3。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,优选所述氯化钙水溶液的质量百分比浓度为0.5~6%,更优选1~4%。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,优选所述海藻酸钠胶体溶液的质量百分比浓度为0.2~2%,优选0.5~1.5%,更优选0.8~1%。
在上述的牡蛎肽-鱼油复合微凝胶的制备方法中,牡蛎肽的分子量小于5000道尔顿,优选小于3000道尔顿,更优选小于1000道尔顿。
本发明的又一实施方式提供一种食品,所述食品包括上述的牡蛎肽-鱼油复合微凝胶。
本发明的再一实施方式提供一种药品,所述药品包括上述的牡蛎肽-鱼油复合微凝胶。
本发明的牡蛎肽-鱼油复合微凝胶包括牡蛎肽水溶液、鱼油和乳化剂的油包水型乳液,并且所述油包水型乳液分散在海藻酸钠与氯化钙交联形成的三维网状凝胶结构中,因此,能够对牡蛎肽起到缓释及活性保护作用,而且掩盖了鱼油和牡蛎肽的腥味,防止鱼油的氧化变质,使鱼油和牡蛎肽得以结合,提高了鱼油、牡蛎肽的利用率以及利用价值。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本发明的某些实施例,因此不应被看作是对本发明范围的限定。
图1示出了本发明实施例的牡蛎肽-鱼油复合微凝胶脱水处理后的SEM图像。
图2示出了实施例8、9、10和4中形成的微凝胶颗粒外观示意图。
图3示出了实施例4的微凝胶颗粒以及对照鱼油在烘箱中保存后的过氧化物值测试结果示意图。
图4示出了实施例4的微凝胶颗粒以及对照鱼油在烘箱中保存后的TBARS值测试结果示意图。
具体实施方式
如本文所用之术语:
“由……制备”与“包含”同义。本文中所用的术语“包含”、“包括”、“具有”、“含有”或其任何其它变形,意在覆盖非排它性的包括。例如,包含所列要素的组合物、步骤、方法、制品或装置不必仅限于那些要素,而是可以包括未明确列出的其它要素或此种组合物、步骤、方法、制品或装置所固有的要素。
连接词“由……组成”排除任何未指出的要素、步骤或组分。如果用于权利要求中,此短语将使权利要求为封闭式,使其不包含除那些描述的材料以外的材料,但与其相关的常规杂质除外。当短语“由……组成”出现在权利要求主体的子句中而不是紧接在主题之后时,其仅限定在该子句中描述的要素;其它要素并不被排除在作为整体的所述权利要求之外。
当量、浓度、或者其它值或参数以范围、优选范围、或一系列上限优选值和下限优选值限定的范围表示时,这应当被理解为具体公开了由任何范围上限或优选值与任何范围下限或优选值的任一配对所形成的所有范围,而不论该范围是否单独公开了。例如,当公开了范围1~5时,所描述的范围应被解释为包括范围1、1.5、2、2.5、3、3.5、4、4.5和5等。当数值范围在本文中被描述时,除非另外说明,否则该范围意图包括其端值和在该范围内的所有整数和分数。
在这些实施例中,除非另有指明,所述的份和百分比均按质量计。
质量份表示多个组分的质量比例关系的基本计量单位,1份可表示任意的单位质量,如可以表示为1g,也可表示2.689g等。假如我们说A组分的质量份为a份,B组分的质量份为b份,则表示A组分的质量和B组分的质量之比a:b。或者,表示A组分的质量为aK,B组分的质量为bK(K为任意数,表示倍数因子)。不可误解的是,与质量份数不同的是,所有组分的质量份之和并不受限于100份之限制。
“和/或”用于表示所说明的情况的一者或两者均可能发生,例如,A和/或B包括(A和B)和(A或B)。
本申请中的牡蛎肽是指以牡蛎肉为原料,经酶解、精制而得的分子量在5000Da以下的小分子低聚肽。牡蛎肽对免疫抑制小鼠免疫功能具有一定影响作用,牡蛎肽可改善CTX(环磷酰胺,免疫抑制剂)所致免疫低下、小鼠紊乱的免疫器官结构,恢复CTX造成的小鼠T淋巴细胞比例失调及细胞因子紊乱,升高骨髓有核细胞数及骨髓DNA含量,从而增强小鼠机体免疫功能。分子量3000Da以下的牡蛎ACE(血管紧张素转化酶)抑制肽对原发性高血压大鼠具有显著的降压效果,牡蛎ACE抑制肽的降压机制在体内能发挥较好作用并能持续性稳定血压。研究者从牡蛎胃蛋白水解产物中分离、纯化和鉴定新发现的抗凝血肽,分子量约1264.36Da,该肽特异性抑制活血凝血因子:凝血酶,并可有效延长活化的部分促凝血酶原激酶时间和凝血酶时间;研究者采用胃蛋白酶和木瓜蛋白酶水解牡蛎软体组织,通过分离纯化及结构鉴定,获得一种含有十三个氨基酸的抗氧化肽分子。此外,发明人经过大量研究,发现牡蛎肽具有抗氧化、改善记忆、抗疲劳等多种活性功效。
鱼油能够通过激活或抑制多种信号通路发挥显著的降血脂作用;鱼油对中间半月板(DMM)小鼠去稳定化中软骨退化的体内作用研究结果表明:鱼油能够改善小鼠软骨结构,抑制软骨细胞肥大分化,抑制关节软骨细胞凋亡异常;补充鱼油能够改善老年大鼠海马胰岛素抵抗和突触信号,此外,鱼油具有降血脂、改善关节退变、减少抑郁行为等功效。
尽管牡蛎肽及鱼油均具有多种生物功能活性,是保健食品开发重要的资源,然而,牡蛎及鱼油均来源于海洋,具有特有的腥味,加之鱼油中富含EPA和DHA,对氧、光及热极为敏感,易发生氧化,丧失生理功效,从而限制了两者在食品工业中的应用。
本发明的一个实施方式提供一种牡蛎肽-鱼油复合微凝胶,包括牡蛎肽、鱼油和乳化剂的油包水型乳液,并且所述油包水型乳液分散在海藻酸钠与氯化钙交联形成的三维网状凝胶结构中。
本发明的微凝胶颗粒能够对牡蛎肽起到缓释及活性保护作用,而且掩盖了鱼油和牡蛎肽的腥味,防止鱼油的氧化变质,使鱼油和牡蛎肽得以结合,提高鱼油和牡蛎肽的利用率以及利用价值。而且,牡蛎肽与鱼油形成的乳液体系在营养物质消化吸收、增溶、稳定性保护、防止降解及控制释放等方面具有明显的优势。因此,本发明的牡蛎肽-鱼油复合微凝胶及其制备方法能有效提高利用率、改善其风味及稳定性,弥补了两者的应用缺陷,提高其应用价值。
本申请中的牡蛎肽是小分子肽,分子量小于5000道尔顿,优选小于3000道尔顿,更优选小于1000道尔顿。由于小分子肽的吸收利用效率比游离氨基酸及大分子多肽均高,因此产品中小分子肽所占的比例越高、游离氨基酸含量越低,肽的品质越好,分子量在1000Da以下的肽可以被人体直接吸收,吸收效率近100%,而且分子量越小,溶解度也越好,因此,本申请最优选小于1000Da以下的牡蛎肽。
乳化剂优选采用司盘80(Span 80)。采用司盘80能够形成更为稳定的油包水乳液。
鱼油和乳化剂的总体积与所述牡蛎肽水溶液的体积之比为4.5:5.5至8:2,优选5:5至6:4,更优选5:5。水相比例过大时,比较难以形成均匀的乳液。在上述5:5的稳定性最佳。
牡蛎肽水溶液中牡蛎肽的质量百分比浓度为3~7%,优选4~6%。
乳化剂相对于所述乳化剂和所述鱼油之和的质量百分比为1~3%,优选1.8~2.2%,最优选2%。乳化剂的含量在优选范围时,能够获得更稳定的乳液。
本发明的牡蛎肽-鱼油复合微凝胶为颗粒状,粒径优选为1.5~2.5mm,例如1.8mm、1.9mm、2.0mm、2.3mm,更优选1.8~2.3mm。由于在制备时采用了注射器注入乳液的方式,能够形成颗粒状的牡蛎肽-鱼油复合微凝胶,方便直接使用,并且利用不同尺寸的注射器针头容易控制复合微凝胶颗粒的粒径。微凝胶在上述粒径范围时能更有效地释放牡蛎肽,粒径过大,不容易释放牡蛎肽。粒径过小对于牡蛎以及鱼油气味的遮蔽不利,并且鱼油更容易氧化。
本发明的另一实施方式提供一种食品或药品,其包括上述的牡蛎肽-鱼油复合微凝胶。牡蛎肽-鱼油复合微凝胶可通过下文的制备方法获得。
本发明的另一实施方式提供上述牡蛎肽-鱼油复合微凝胶的制备方法,包括:将牡蛎肽水溶液、鱼油和乳化剂混合形成油包水乳液;将所述油包水乳液与海藻酸钠胶体溶液混合形成水包油包水乳液;将所述水包油包水乳液滴加至氯化钙水溶液中,使得氯化钙与海藻酸钠交联后形成所述牡蛎肽-鱼油复合微凝胶。优选采用注射器将所述水包油包水乳液滴加至氯化钙水溶液中,注射器可采用例如普通的医用注射器或其他带有针头的注射器具,以其他方式加入乳液较难形成颗粒状的微凝胶。
本发明的牡蛎肽-鱼油复合微凝胶制备方法中,首先将牡蛎肽与鱼油利用乳化剂构建W/O型乳液,然后,与海藻酸钠胶体溶液形成W/O/W型双层乳液,最后与CaCl2水溶液交联形成微凝胶颗粒。海藻酸钠胶体溶液为海藻酸钠胶体水溶液。
优选将鱼油和所述乳化剂预先混合形成油相混合物,所述油相混合物中所述乳化剂的质量百分比优选为1~3%,更优选1.8~2.2%。
优选油包水乳液与海藻酸钠胶体溶液的体积比为1:0.8~1:5,优选1:1~1:2。乳液胶体比中胶体比例越高,对乳液的保护程度越大,乳液的消化分解更困难,多肽释放量越少,从保护乳液以及多肽释放量平衡的角度来看,更优选1:1~1:2。
所述氯化钙水溶液的质量百分比浓度优选为0.5~6%,更优选1~4%,最优选2%,在优选范围内可形成更稳定的微凝胶。
所述海藻酸钠胶体溶液的质量百分比浓度优选为0.2~2%,更优选0.5~1.5%,进一步优选0.8~1%。实验证实如果海藻酸钠浓度太小,形成不了微凝胶颗粒,如果海藻酸钠浓度太高,则微凝胶变得较硬,而0.8~1%的范围能形成圆润颗粒,并且有适度弹性。此外,在上述浓度范围内,海藻酸钠的浓度越高,感官分析中的评分越高,其可接受程度越高。
下面将结合具体的实例和实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列的实例和实施例仅用于说明本发明,而不应视为限制本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
油包水W/O乳液的制备
将牡蛎肽溶于超纯水利用例如均质机在9000rpm均质5min,制备出质量百分比5%的牡蛎肽水溶液,以下制备过程中使用的牡蛎肽的分子量小于1000道尔顿。将鱼油和乳化剂在9000rpm均质5min制备乳化剂的质量百分比1%、2%或3%的混合油相。在12000rpm下以1:1的体积比在混合油相中缓慢加入牡蛎肽水溶液,均质5min以获得均匀乳液。
通过染色法辨别乳液是水包油型(O/W)还是油包水型(W/O)乳液,这里是将脂溶性染色剂苏丹Ⅲ溶液加进乳液中,然后放置在生物显微镜下观察,如果是红色液体包裹着透明液体,则是油包水乳液,如果不是,则是水包油乳液。当然也可以用水溶性染色剂检测,例如曙红Y溶液。也可要使用稀释法、电导法等方法检测。
上述的乳化剂分别采用司盘80和聚甘油蓖麻醇酸酯(PGPR)。在经过染色法辨别后,发现两种乳化剂都形成了油包水型乳液。
此外,在形成均匀乳液后,在30min,1h,2h,4h,6h,8h时观察乳液稳定性。测试结果见下表1:
表1不同乳化剂的乳液稳定性
由以上测试结果可以看出,乳化剂优选采用司盘80。此外,在混合油相中,乳化剂的质量百分比浓度可优选1~3%,更优选1.8~2.2%,进一步优选2%。
此外,还针对牡蛎肽水溶液的pH值进行了调节,以确定不同pH值下对于乳化稳定的影响,利用柠檬酸调pH到4.0,采用食用碱调pH到9.0,在pH为4.0的酸性条件下处理得到的乳液出现严重分层,不能得到实验需要稳定乳液,因此,在酸性条件下,乳化剂不能起到乳化作用。在pH为9.0的碱性条件下,添加乳化剂PGPR处理得到的乳液出现严重分层,不能得到预期的乳液,添加乳化剂司盘80处理得到的乳液出现轻微分层,稳定性较好,说明在碱性条件下乳液稳定性下降。因此,在制备牡蛎肽水溶液时,不添加pH调节剂的乳液的稳定性最好。
此外,针对混合油相与水相的体积比对于乳液稳定性的影响进行研究,制备过程与实例3基本相同,不同之处在于改变油水比,即混合油相和水相的比例。对比例1、2和3的油水体积比分别为2:8、3:7和4:6,实例11-14的油水体积比分别为4.5:5.5、6:4、7:3、8:2。对比例1和2中,水相比例过大,在相同均质时间,比较难以形成均匀的乳液,而在对比例3中,仍有少量肽液残留在乳液之外,因此,未利用对比例1-3进行稳定性对比。
表2不同油水比的乳液稳定性
在油水比为5:5时,在静止8h后未发现分层,在油水比为6:4、7:3、8:2时,随着油的体积比例的增加,乳液随着时间的延长,分层状况逐渐愈加严重,稳定性变差。
水包油包水W/O/W乳液的制备
制备质量百分比浓度1.0%的海藻酸钠胶体溶液,然后利用均质机将海藻酸钠胶体溶液在12000rpm下均质,再将实例3中的W/O乳液按照下表3中示出的比例缓慢加入到海藻酸钠胶体溶液中,均质1min获得均匀乳液,即为W/O/W型乳液。
蛎肽-鱼油复合微凝胶的制备
将制得的W/O/W型乳液用2mm针头的注射器均速滴进2%氯化钙溶液中以形成牡蛎肽-鱼油复合微凝胶。
表3不同乳液胶体比的蛎肽-鱼油复合微凝胶
当乳液胶体比在2:1、3:1、4:1时,W/O/W型乳液在滴进氯化钙溶液时形成微凝胶颗粒的难度逐渐增高,部分乳液分开,漂浮于溶液表面,较难形成成型的微凝胶颗粒。乳液胶体比为1:1、1:2、1:3、1:4均能形成微凝胶颗粒。
此外,研究了牡蛎肽水溶液的浓度对于微凝胶颗粒形成的影响,与实施例4基本相同地制备微凝胶颗粒,不同之处在于:在制备水包油包水乳液时,实施例8、实施例9、实施例10和实施例11分别采用2%、3%、4%和7%的肽液浓度。
表4不同牡蛎肽水溶液的蛎肽-鱼油复合微凝胶
图2示出了实施例8、9、10和4中形成的微凝胶颗粒外观示意图。2%牡蛎肽水溶液制备的W/O/W乳液在滴进2%氯化钙溶液中时无法形成圆润的完整球形,采用的3%牡蛎肽水溶液时会有部分微凝胶存在破损,采用4%以及5%的牡蛎肽水溶液时能够形成圆润光滑的微凝胶珠。尽管未图示,但是采用7%的牡蛎肽水溶液时部分微凝胶也存在破损,浓度太高时,影响水凝胶形成,并且影响乳液pH值整体环境。
此外,参见下表5,针对采用不同浓度的海藻酸钠胶体溶液所形成微凝胶进行研究。实施例12-14、15-17、18-20、21-23分别与实施例4-6对应,不同之处在于海藻酸钠胶体溶液的浓度,海藻酸钠的浓度分别为0.2%、0.4%、0.6%、0.8%、1.0%。
表5不同海藻酸钠浓度及乳液胶体比
牡蛎肽-鱼油复合微凝胶性质分析
SEM结果分析
将各个实施例的牡蛎肽-鱼油复合微凝胶进行脱水处理后,将脱水处理后的微凝胶颗粒贴在有双面胶的样品平台上,用小镊子稍稍压实,使颗粒末陷入双面胶中,用小镊子刀面刮去表面粉末,并把多余的微凝胶颗粒吹净,然后置于离子溅射仪中在10mA电流下喷金,等处理完毕立即进行电镜扫描,利用扫描电子显微镜观察其微结构,发现牡蛎肽-鱼油复合微凝胶形成了三维网状结构。例如,图1示出了经脱水处理的实施例5的牡蛎肽-鱼油复合微凝胶的SEM图像。由SEM图像可以看出,脱水处理后的微凝胶颗粒形成大小不一的空洞,说明乳液在经过脱水处理后从空洞处脱离,使微凝胶颗粒形成空洞。由SEM图可以看出,牡蛎肽-鱼油复合微凝胶形成了三维网状结构,三维网状结构中形成大约几微米至十几微米的孔洞。牡蛎肽-鱼油复合微凝胶体外模拟消化
根据下表6制备模拟口腔液、模拟胃液和小肠液,进行体外消化模拟实验,并用福林酚法测牡蛎肽释放量,分析不同乳液胶体比对体外消化释放牡蛎肽效果的影响。
表6消化液的配制
胆汁盐溶液由0.375g胆盐和10mM pH7.0磷酸盐缓冲液组成配制成;脂肪酶悬液由0.06g脂肪酶和10mM pH7.0磷酸盐缓冲液配制而成。
在进行体外消化实验前,需制备肽含量相同其他制备条件不同的微凝胶颗粒,本实验采用2ml的牡蛎肽W/O乳液,制备成不同的微凝胶颗粒,然后进行体外消化实验,在三组实验组(实施例4至6的微凝胶颗粒)以及一组空白组(无微凝胶颗粒)中加入6mL模拟口腔液,利用恒温振荡水浴锅,在37℃100rpm条件下反应10s,然后向反应后的溶液中加入12mL模拟胃液,在37℃pH 2.5 100rpm条件下反应2h,2h后分别取各组溶液1ml,用福林酚法进行多肽含量分析;用1M NaHCO3溶液将反应后的溶液pH调至7.0,静置5min后,分别取各组溶液1ml,用福林酚法进行多肽含量分析;然后向溶液中加入模拟小肠液,用0.1M NaOH溶液滴定,使溶液pH始终保持在7.0,在37℃100rpm条件下反应2h,2h后分别取各组溶液1ml,用福林酚法进行多肽含量分析。表7示出了牡蛎肽体外模拟消化释放情况。
对于实施例4(乳液胶体比1:1),在利用模拟口腔液与胃液处理约2小时后,凝胶颗粒没有明显的外形变化,在碳酸氢钠调节pH至7.0后,凝胶颗粒开始溶解分散,在模拟小肠液处理2小时后,凝胶颗粒溶解消失。对于实施例5(乳液胶体比1:2),在利用模拟口腔液与胃液处理约2小时后,凝胶颗粒没有明显的外形变化,在碳酸氢钠调节pH至7.0后,凝胶颗粒开始溶解分散,在模拟小肠液处理2小时后,凝胶颗粒溶解消失。而对于实施例6(乳液胶体比1:3),在利用模拟口腔液与胃液处理约2小时后,凝胶颗粒没有明显的外形变化,在碳酸氢钠调节pH至7.0后,凝胶颗粒依旧没有明显的外形变化,在模拟小肠液处理2小时后,凝胶颗粒膨胀变大。
表7牡蛎小分子肽体外模拟消化释放情况(mg/mL)
从表7的体外消化模拟实验各过程中多肽含量的释放量的分析中可以得出结论:①调节pH至7.0后空白组多肽含量变化不大,说明模拟液在调节pH过程中对凝胶中多肽的释放影响不大,1:1乳液胶体比的多肽含量上升,说明在pH调节过程中1:1乳液胶体比微凝胶分解释放了部分多肽,而1:2乳液胶体比以及1:3乳液胶体比多肽释放不明显,说明在调节pH过程中,此条件下的微凝胶几乎不分解。②在经过模拟小肠液消化2h后,空白组多肽含量也明显上升,说明模拟消化液在消化过程中作用微凝胶使多肽释放,各实验组的多肽含量均大量上升,且与空白组对照后多肽含量仍是大量增加。③经过消化过程,三个乳液胶体比的多肽释放量由大到小排列1:1>1:2>1:3,说明乳液胶体比中胶体比例越高,对乳液的保护程度越大,乳液的消化分解更困难,因此多肽释放量越少。
表8不同粒径大小对牡蛎肽释放情况的影响
由表8的数据可以看出,微凝胶在1.8~2.3mm的粒径范围时能更有效地释放牡蛎肽。
感官分析
对实施例4至6以及实施例12至23进行了微凝胶的感官分析。
表9感官评价得分表
表10感官评价得分标准
注:得分越高表示其可接受程度越高。
由表9的感官评价得分可以看出,同一浓度海藻酸钠的感官评价中,得分基本上由高到低排列为乳液胶体比1:3>1:2>1:1,说明当海藻酸钠浓度相同时,在1:1到1:3范围内,乳液胶体比越高,其可接受程度越高。在不同浓度的海藻酸钠溶液的相同乳液胶体比比较中可以看出,海藻酸钠浓度越高,各项目评分越高,其可接受程度越高。
鱼油氧化稳定性分析
对实施例4的微凝胶颗粒以及对照鱼油进行了鱼油氧化性的分析,在100℃的烘箱中保存实施例4的微凝胶颗粒和对照鱼油,每天分析相应鱼油的过氧化物值以及TBARS值。图3示出了实施例4的微凝胶颗粒以及对照鱼油在烘箱中保存后的过氧化物值测试结果示意图。图4示出了实施例4的微凝胶颗粒以及对照鱼油在烘箱中保存后的TBARS值测试结果示意图。
以上的测试结果显示,在本发明的复合微凝胶体系下,显著地抑制了鱼油的氧化。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
此外,本领域的技术人员能够理解,尽管在此的一些实施例包括其它实施例中所包括的某些特征而不是其它特征,但是不同实施例的特征的组合意味着处于本发明的范围之内并且形成不同的实施例。例如,在上面的权利要求书中,所要求保护的实施例的任意之一都可以以任意的组合方式来使用。公开于该背景技术部分的信息仅仅旨在加深对本发明的总体背景技术的理解,而不应当被视为承认或以任何形式暗示该信息构成已为本领域技术人员所公知的现有技术。
Claims (10)
1.一种牡蛎肽-鱼油复合微凝胶,其特征在于,包括牡蛎肽水溶液、鱼油和乳化剂的油包水型乳液,并且所述油包水型乳液分散在海藻酸钠与氯化钙交联形成的三维网状凝胶结构中。
2.根据权利要求1所述的牡蛎肽-鱼油复合微凝胶,其特征在于,所述乳化剂包括司盘80。
3.根据权利要求1所述的牡蛎肽-鱼油复合微凝胶,其特征在于,所述鱼油和乳化剂的总体积与所述牡蛎肽水溶液的体积之比为4.5:5.5至8:2,优选5:5至6:4,更优选5:5。
4.根据权利要求1至3中任一项所述的牡蛎肽-鱼油复合微凝胶,其特征在于,所述牡蛎肽水溶液中牡蛎肽的质量百分比浓度为3~7%,优选4~6%;
所述乳化剂相对于所述乳化剂和所述鱼油之和的质量百分比为1~3%,优选1.8~2.2%;
牡蛎肽的分子量小于5000道尔顿,优选小于3000道尔顿,更优选小于1000道尔顿;
所述牡蛎肽-鱼油复合微凝胶的粒径为1.5~2.5mm。
5.一种牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于,包括:
利用牡蛎肽水溶液、鱼油和乳化剂形成油包水乳液;
将所述油包水乳液与海藻酸钠胶体溶液混合形成水包油包水乳液;
将所述水包油包水乳液滴加至氯化钙水溶液中,使得氯化钙与海藻酸钠交联后形成所述牡蛎肽-鱼油复合微凝胶。
6.根据权利要求5所述的牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于,所述乳化剂包括司盘80;采用注射器将所述水包油包水乳液滴加至氯化钙水溶液中。
7.根据权利要求5所述的牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于,所述鱼油和乳化剂的总体积与所述牡蛎肽水溶液的体积之比4.5:5.5至8:2,优选5:5至6:4,更优选5:5。
8.根据权利要求5所述的牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于,所述牡蛎肽水溶液中牡蛎肽的质量百分比浓度为3~7%,优选4~6%;
将鱼油和所述乳化剂预先混合形成油相混合物,所述油相混合物中所述乳化剂的质量百分比为1~3%,优选1.8~2.2%。
9.根据权利要求5所述的牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于:所述油包水乳液与海藻酸钠胶体溶液的体积比为1:0.8~1:5,优选1:1~1:3。
10.根据权利要求5至9中任一项所述的牡蛎肽-鱼油复合微凝胶的制备方法,其特征在于:
优选所述氯化钙水溶液的质量百分比浓度为0.5~6%,更优选1~4%;
优选所述海藻酸钠胶体溶液的质量百分比浓度为0.2~2%,优选0.5~1.5%,更优选0.8~1%;
牡蛎肽的分子量小于5000道尔顿,优选小于3000道尔顿,更优选小于1000道尔顿;
所述牡蛎肽-鱼油复合微凝胶的粒径为1.5~2.5mm。
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CN108969505A (zh) * | 2018-08-01 | 2018-12-11 | 青岛明月海藻集团有限公司 | 一种花青素微胶囊的制备方法 |
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