CN111280365A - 一种大蒜多糖微胶囊及其制备方法与应用 - Google Patents

一种大蒜多糖微胶囊及其制备方法与应用 Download PDF

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CN111280365A
CN111280365A CN202010079709.0A CN202010079709A CN111280365A CN 111280365 A CN111280365 A CN 111280365A CN 202010079709 A CN202010079709 A CN 202010079709A CN 111280365 A CN111280365 A CN 111280365A
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garlic
garlic polysaccharide
polysaccharide
microcapsule
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郑金铠
安庆
赵少杰
王凤忠
赵成英
田桂芳
陆畅
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Abstract

本发明公开了一种大蒜多糖微胶囊及其制备方法与应用。本发明大蒜多糖微胶囊,为大蒜多糖作为芯材包埋于壁材形成的微胶囊。其制备方法,包括如下步骤:将大蒜多糖与所述壁材混合,通过喷雾干燥方法进行微胶囊化,即得到所述大蒜多糖微胶囊。本发明所述大蒜多糖微胶囊在制备如下1)或2)中功能的食品、药品和/或保健品中的应用;1)降低血糖调节人体免疫力;2)选择性地增殖双歧杆菌,促进肠道的蠕动。本发明制备工艺简单,成本低,且成分天然,出粉率和包埋率高,便于工业化生产。

Description

一种大蒜多糖微胶囊及其制备方法与应用
技术领域
本发明涉及一种大蒜多糖微胶囊及其制备方法与应用,属于天然产物制备及功能食品技术领域。
背景技术
大蒜为百合科葱属植物蒜的鳞茎,是人们日常生活中不可缺少的调味料,自古以来就被作为药用食物。大蒜为植物广谱抗生素,对多种球菌、杆菌、霉菌、真菌、病毒、阿米巴原虫、阴道滴虫、蛲虫等都有抑制和杀灭作用,可以预防和治疗上述微生物和寄生虫引起的疾病;大蒜还具有防治冠心病,降低血脂及胃内亚硝酸盐含量等作用。目前国内外对于大蒜抑菌、抗菌作用的研究主要集中于大蒜油、大蒜素。而目前有关大蒜的专利大多集中在大蒜油有效成分的保护上,如CN107041549A、CN12742810A、CN106580916A、CN1253152C、CN100367944C等专利均利用微胶囊技术对大蒜油或大蒜素包埋,但在整个大蒜功效成分组成上,大蒜油仅占0.2%-0.4%,且提取成本高,工艺复杂,而大蒜多糖作为大蒜另一功效成分,不仅含量丰富,可达总干物质含量的80%以上,且作为一种菊糖类多糖,发挥功效明显,具有控制血脂、降低血糖调节人体免疫力作用,还可选择性地增殖双歧杆菌被双歧杆菌代谢后会产生乳酸及醋酸使肠道呈酸性抑制微生物的增殖促进肠道的蠕动。
微胶囊是将固体、液体或气体物质包埋、封存在一种微型胶内成为一种固体微粒产品的技术,微胶囊具有的防护材料可使芯材免受温度、氧气、紫外辐射、湿度、光、pH的影响,有利于芯材原有成分的特性及营养,微胶囊技术还可以将有效成分进行有序地释放,并能在确定的时间段发生作用,提高产品的功能特性。多糖进行微胶囊化处理,不仅可改善其分散性及乳化分散性等能力,还可强化多糖中易氧化成分的保护作用,增强其稳定性,延长货架期,提高营养价值,运输也更为方便,但微胶囊技术在多糖包埋方面的研究比较少,且大多数包埋过程复杂,比如CN110051647A中,利用卡拉胶:壳聚糖:β-环糊精为壁材包埋螯合锌离子的猴头菇多糖,虽然能提高抗氧化效果,但壁材选用繁多,最终产品纯度较低,且螯合过程复杂;再如专利CN107549780A中,利用喷雾干燥技术制备了金针菇多糖微胶囊粉,但制备过程中先利用醇沉和冷冻干燥的方法将金针菇多糖变为固体,再通过加稳定剂、乳化剂在水中复溶,该过程不仅能耗高,耗时长,且有机溶剂易残留在微胶囊产品上,安全性不高。目前关于大蒜多糖微胶囊制备工艺未见研究。大蒜多糖较其他多糖相比,不需要螯合其他抗氧化金属离子,其自身不仅抗氧化显著,而且其增强机体免疫功能,能显著降低疾病发病率,并在一定程度上较少抗生素/抗菌剂使用。
发明内容
本发明的目的是提供一种大蒜多糖微胶囊及其制备方法与应用,本发明制备工艺简单,成本低,且成分天然,出粉率和包埋率高,便于工业化生产。
本发明提供的一种大蒜多糖微胶囊,为大蒜多糖作为芯材包埋于壁材形成的微胶囊。
上述的大蒜多糖微胶囊中,所述壁材选自麦芽糊精、β-环糊精、牛血清白蛋白、大豆分离蛋白和壳聚糖中的至少一种。
上述的大蒜多糖微胶囊中,所述大蒜多糖微胶囊的包埋率可为70%~85%,具体可为74.5%、74.9%、75.6%、78.3%和80.2%;
所述大蒜多糖微胶囊的粒径范围可为900~10000nm,具体可为900~4000nm、900~5000nm或900~8000nm。
本发明还提供了上述大蒜多糖微胶囊的制备方法,包括如下步骤:将大蒜多糖与所述壁材混合,通过喷雾干燥方法进行微胶囊化,即得到所述大蒜多糖微胶囊。
上述的制备方法中,所述喷雾干燥的条件如下:进料温度可为150℃~190℃,具体可为150℃、160℃、170℃、180℃、190℃、160℃~170℃或160℃~180℃;进料速度可为10mL/min~15mL/min,具体可为15mL/min;蠕动泵转速可为30~50r/min,具体可为30r/min,出口温度可为75~95℃,具体可为75℃、75~80℃或75~85℃。
上述的制备方法中,所述方法包括如下步骤:
1)将大蒜泥与水混合浸提,过滤得到浸提液;将所述浸提液离心收集上清液并浓缩,得到大蒜多糖浓缩液;
2)将所述大蒜多糖浓缩液与所述壁材通过剪切混合,然后通过喷雾干燥方法进行微胶囊化,即得到所述大蒜多糖微胶囊。
上述的制备方法中,所述大蒜泥与所述水的质量比可为10~80:100,具体可为30:100、10~30:100、30~50:100、10~50:100、20~40:100或20~40:100;
所述浸提的条件:温度可为80℃~85℃,具体可为80℃,时间可为2~2.5h,具体可为2.5h;
所述过滤过程如下:先经250~300目尼龙布过滤出滤渣,得到的滤液经抽滤得到所述浸提液;具体可为经300目尼龙布过滤出滤渣。
上述的制备方法中,所述离心的条件如下:8000~10000rpm离心10~15min;具体可为8000rpm离心10min;
所述浓缩的条件如下:45℃~50℃真空浓缩至所述大蒜多糖浓缩液的质量百分浓度可为15%~75%,具体可为20%~75%。
上述的制备方法中,所述壁材与所述大蒜多糖浓缩液和所述壁材质量之和比为15~35:100,具体可为25:100、15~25:100、25~35:100或20~30:100;
所述剪切的条件如下:剪切速度可为8000~10000r/min,时间可为0~4min。
本发明所述大蒜多糖微胶囊在制备如下1)或2)中功能的食品、药品和/或保健品中的应用;
1)降低血糖调节人体免疫力;
2)选择性地增殖双歧杆菌,促进肠道的蠕动。
本发明中,所述食品具体可为固体饮料食品。
本发明具有以下优点:
1、本发明采用喷雾干燥法首次制备了大蒜多糖微胶囊,与传统大蒜多糖粉相比,壁材的加入不仅能在一定程度上掩盖不良风味,延长活性有效期,而且在有效成分发挥作用上可以很好起到缓释作用,也能充当助干剂,降低产品含水量,进而提高出粉率(传统上喷雾干燥大蒜多糖出粉率13.5%,本发明中微胶囊化出粉率达最优工艺下达到28.2%),增加企业收益。
2、本发明工艺简单,成本低,且壁材使用量少,成分天然纯度高(52%),包埋率高(80.2%),具有良好的速溶性和稳定性,可应用于固体饮料食品,保证营养物质被人体充分吸收,易于实现工业化生产,效益明显。
附图说明
图1为本发明大蒜多糖微胶囊制备工艺流程图。
图2为本发明大蒜多糖微胶囊的外观图,其中图2(a)为多糖浓度15%、30%、45%、60%、75%下制得大蒜多糖微胶囊;图2(b)为不同壁材浓度5%、15%、25、35%、55%下制得的大蒜多糖微胶囊;
图3为本发明大蒜多糖微胶囊的扫描电镜图。
图4为本发明大蒜多糖微胶囊的红外光谱图。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1、大蒜多糖微胶囊的制备
料液中多糖浓度对大蒜多糖微胶囊制备工艺的探究实验:
a:选用干净去皮的150g新鲜大蒜,用绞碎机绞碎,加入不同体积的蒸馏水(大蒜与水的质量比为10%~50%),制备多糖浸提液,在80℃水浴锅内恒温提取2.5h,300目尼龙布过滤出滤渣,抽滤得到粗浸提液;
b:浸提液进行8000rpm离心10min操作,先弃去沉淀,再将上清液于50℃真空浓缩,使其浓缩后的多糖浸提液浓度达到15%~75%(计为进料液浓度,如表1所示);并收集浓缩液;
c:壁材与浓缩液混合时,使用剪切混合,保证混合均匀,所述剪切的条件包括:剪切速度为8000r/min,时间控制在4min内;壁材添加量25%;
d:喷雾干燥的操作参数设置进料温度170℃,进料速度:15mL/min,蠕动泵转速30r/min,出口温度为75℃;
e:出粉率和包埋率按以下公式计算。
Figure BDA0002379852410000041
Figure BDA0002379852410000042
表1进料多糖浓度对微胶囊出粉率影响
Figure BDA0002379852410000043
随着进料液浓度的升高,多糖出粉率先增加后降低趋势。这是因为浓度高时,喷雾前料中大蒜多糖的含量相对较高,溶质过浓会导致喷雾时出现粘壁、堵塞喷头等现象,降低了出粉率;随之含水量增加,物料被稀释,含糖量降低,出粉率有所增加;随着大蒜多糖浓度的上升,微胶囊产品包埋率先增加后减小,这是因为当多糖浓度超过30%时,芯材含量过高,会导致多糖向麦芽糊精发生渗透,包埋率降低,综合考虑选用进料液浓度在30%比较好。
实施例2、大蒜多糖微胶囊制备
壁材添加量对微胶囊化的工艺探究实验:
a:选用干净去皮的150g新鲜大蒜,用绞碎机绞碎,加入1.5L蒸馏水,制备多糖浸提液,在80℃水浴锅内恒温提取2.5h,300目尼龙布过滤出滤渣,抽滤得到粗浸提液;
b:浸提液进行8000rpm离心10min操作,先弃去沉淀,再将上清液于50℃真空浓缩,使其浓缩后的多糖浸提液浓度达到30%;并收集浓缩液;
c:壁材与浓缩液混合时,使用剪切混合,保证混合均匀,所述剪切的条件包括:剪切速度为8000r/min,时间控制在4min内;壁材添加量10%~55%,具体如表2中所示;
d:喷雾干燥的操作参数设置进料温度170℃,进料速度:15mL/min,蠕动泵转速30r/min,出口温度为75℃;
e:出粉率和包埋率按以下公式计算。
Figure BDA0002379852410000051
Figure BDA0002379852410000052
表2 170℃时每150克大蒜多糖微胶囊化结果
Figure BDA0002379852410000053
随着麦芽糊精添加量的增加出粉率也随之增高,超过25%时,出粉率上升速率减缓,且大蒜多糖的颜色由淡黄色逐渐变深,香味逐渐变小;而包埋率随麦芽糊精量的增加,先升高后降低,在25%时包埋率可达80.2%;综合考虑,选择麦芽糊精添加量为25%最佳。
实施例3、大蒜多糖微胶囊制备
进风温度对微胶囊出粉的影响实验:
a:选用干净去皮的150g新鲜大蒜,用绞碎机绞碎,加入1.5L蒸馏水,制备多糖浸提液,在80℃水浴锅内恒温提取2.5h,300目尼龙布过滤出滤渣,抽滤得到粗浸提液;
b:浸提液进行8000rpm离心10min操作,先弃去沉淀,再将上清液于50℃真空浓缩,使其浓缩后的多糖浸提液浓度达到30%;并收集浓缩液;
c:壁材与浓缩液混合时,使用剪切混合,保证混合均匀,所述剪切的条件包括:剪切速度为8000r/min,时间控制在4min内;壁材添加量25%;
d:喷雾干燥的操作参数设置进料温度160℃~200℃(具体如表3所示),进料速度:15mL/min,蠕动泵转速30r/min,出口温度为75℃。
e:出粉率和包埋率按以下公式计算。
Figure BDA0002379852410000061
Figure BDA0002379852410000062
表3进口温度对大蒜多糖微胶囊喷雾干燥影响
Figure BDA0002379852410000063
结果表明160℃-170℃之间,随着进风温度的升高,出粉率随之增加。这是因为进风温度过低,由于产品水分含量高,喷雾干燥时容易粘结在一起结块黏壁,使得产品的产率下降,但是继续升温时,料液雾滴与强热风接触,雾滴表面容易焦化黏连影响喷嘴出口喷料,并产生焦糊味,大大降低出料率,因此确定170℃为适宜的进风温度。
综上,最佳大蒜多糖微胶囊制备条件为:进料多糖浓度30%,壁材添加量25%,进风温度170℃,该制备条件下大蒜多糖微胶囊出粉率28.2%,包埋率可达80.2%,粒径为933.5nm。
实施例4、大蒜多糖微胶囊的制备
按照本发明实施例1中方法,并在最佳大蒜多糖微胶囊制备条件下制备,得到大蒜多糖微胶囊。
上述大蒜多糖及微胶囊的表征方法如下:
(1)理化性质表征:用蒽酮硫酸法测大蒜多糖微胶囊中大蒜多糖含量计算出粉率、包埋率;含水率参照GB5497-1985测定;堆积密度用质量体积比表示;溶解度根据重量法计算
(2)红外光谱表征:采用溴化钾压片法进行大蒜多糖微胶囊的红外扫描,扫描范围:4000-400cm-1,透射模式。
对本发明实施例4制备得到的大蒜多糖微胶囊经上述表征方法测定,其理化性质结果如表4;其品质评价结果如表5所示。通过表1和表2数据可知,本发明制备的大蒜多糖微胶囊成分天然纯度高(52%),包埋率高(80.2%),粒径小(933.5nm),不仅能在一定程度上掩盖不良风味,延长活性有效期,而且在有效成分发挥作用上能很好起到缓释作用,具有良好的速溶性和稳定性,可应用于固体饮料食品,保证营养物质被人体充分吸收,易于实现工业化生产,效益明显。
表4大蒜多糖微胶囊的理化性质
Figure BDA0002379852410000071
表5大蒜多糖微胶囊的品质评价
Figure BDA0002379852410000072
对比例、
与本发明实施例1中方法相同,不同步骤为采用传统上喷雾干燥,具体操作是:将步骤b中所得多糖浓缩液直接进行喷雾干燥,中间不添加任何壁材,其他过程不变。
该对比例中大蒜多糖出粉率仅为13.5%,喷雾过程中粘壁较为严重,粉体发褐色。

Claims (10)

1.一种大蒜多糖微胶囊,为大蒜多糖作为芯材包埋于壁材形成的微胶囊。
2.根据权利要求1所述的大蒜多糖微胶囊,其特征在于:所述壁材选自麦芽糊精、β-环糊精、牛血清白蛋白、大豆分离蛋白和壳聚糖中的至少一种。
3.根据权利要求1或2所述的大蒜多糖微胶囊,其特征在于:所述大蒜多糖微胶囊的包埋率为70%~85%;
所述大蒜多糖微胶囊的粒径范围为900~10000nm。
4.权利要求1-3中任一项所述大蒜多糖微胶囊的制备方法,包括如下步骤:将大蒜多糖与所述壁材混合,通过喷雾干燥方法进行微胶囊化,即得到所述大蒜多糖微胶囊。
5.根据权利要求4所述的制备方法,其特征在于:所述喷雾干燥的条件如下:进料温度为150℃~190℃;进料速度为10mL/min~15mL/min;蠕动泵转速为30~50r/min,出口温度为75~95℃。
6.根据权利要求4或5所述的制备方法,其特征在于:所述方法,包括如下步骤:
1)将大蒜泥与水混合浸提,过滤得到浸提液;将所述浸提液离心收集上清液并浓缩,得到大蒜多糖浓缩液;
2)将所述大蒜多糖浓缩液与所述壁材通过剪切混合,然后通过喷雾干燥方法进行微胶囊化,即得到所述大蒜多糖微胶囊。
7.根据权利要求6所述的制备方法,其特征在于:所述大蒜泥与所述水的质量比为10~80:100;
所述浸提的条件:温度为80℃~85℃,时间为2~2.5h;
所述过滤过程如下:先经250~300目尼龙布过滤出滤渣,得到的滤液经抽滤得到所述浸提液。
8.根据权利要求6或7所述的制备方法,其特征在于:所述离心的条件如下:8000~10000rpm离心10~15min;
所述浓缩的条件如下:45℃~50℃真空浓缩至所述大蒜多糖浓缩液的质量百分浓度为15%~75%。
9.根据权利要求6-8中任一项所述的制备方法,其特征在于:所述壁材与所述大蒜多糖浓缩液和所述壁材质量之和比为15~35:100;
所述剪切的条件如下:剪切速度为8000~10000r/min,时间为0~4min。
10.权利要求1-3中任一项所述大蒜多糖微胶囊在制备如下1)或2)中功能的食品、药品和/或保健品中的应用;
1)降低血糖调节人体免疫力;
2)选择性地增殖双歧杆菌,促进肠道的蠕动。
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