CN114644719A - 一种海茸多糖提取液及其制备方法与应用 - Google Patents
一种海茸多糖提取液及其制备方法与应用 Download PDFInfo
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- CN114644719A CN114644719A CN202210297784.3A CN202210297784A CN114644719A CN 114644719 A CN114644719 A CN 114644719A CN 202210297784 A CN202210297784 A CN 202210297784A CN 114644719 A CN114644719 A CN 114644719A
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- polysaccharide
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- seaweed
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Abstract
本发明属于天然多糖提取技术领域,公开了一种海茸多糖提取液及其制备方法与应用。所述海茸多糖提取液的制备方法,包括以下步骤:将海茸粉碎后与乙醇混合,离心取沉淀;采用包含左旋肉碱和天然有机酸的离子液体对所述沉淀进行萃取,制得海茸多糖提取液。本发明采用乙醇对海茸进行前处理后,再以特定离子液体为载体对海茸多糖进行提取,可以有效提高海茸多糖的提取率,且所制得海茸多糖水凝胶具备更好的抗氧化性能,可有效清除各类自由基。
Description
技术领域
本发明属于天然多糖提取技术领域,特别涉及一种海茸多糖提取液及其制备方法与应用。
背景技术
海茸是海藻中褐藻类里一种营养丰富、口感鲜美的绿色天然食品,是野生天然的深海植物,是深海植物中最珍贵稀有的一员。现代研究还发现,从海茸中所提取的海茸多糖不仅可以有效降低活性氧和丙二醛,还能提高超氧化物歧化酶、谷胱甘肽过氧化物歧化酶和过氧化氢酶的含量来提高机体抗氧化能力。此外,海茸多糖还可以激活磷酸肌醇-3激酶、蛋白激酶B和糖原合成激酶3β途径来促进机体抗氧化。
在现阶段,通常仅采用水浸提法、超声波法和微波提取法等常规多糖提取手段对海茸多糖进行提取,并未有对海茸多糖的提取工艺和方法进行优化的相关报导。因此,本发明希望开发得到一种全新的海茸多糖提取方式,以提高海茸多糖的提取率,并使制得的海茸多糖产物具有更好的抗氧化性能,从而使其在日化、化妆品等领域具备更好的应用前景。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此,本发明提出一种海茸多糖提取液及其制备方法与应用。本发明采用乙醇对海茸进行前处理后,再以特定离子液体为载体对海茸多糖进行提取,可以有效提高海茸多糖的提取率,且具备更好的抗氧化性能,可有效清除各类自由基。
本发明提供一种海茸多糖提取液的制备方法,包括以下步骤:
将海茸粉碎后与乙醇混合,离心取沉淀;采用包含左旋肉碱和天然有机酸的离子液体对所述沉淀进行萃取,制得海茸多糖提取液。
本发明在对多种提取方式进行反复筛选后,最终发现采用乙醇对海茸进行前处理后,再采用包含左旋肉碱和天然有机酸的特定离子液体对海茸多糖进行提取,其海茸多糖的提取率最佳,且所制得产物的抗氧化性能优良。
优选的,所述天然有机酸选自顺丁烯二酸、柠檬酸、苹果酸、酒石酸、丙二酸、丙酸、脯氨酸、草酸中的至少一种。
更优选的,所述天然有机酸选自柠檬酸、苹果酸或酒石酸。上述天然有机酸均可作为食品级添加剂,安全性良好。
最优选的,所述天然有机酸为苹果酸。
优选的,所述离子液体中左旋肉碱和天然有机酸的摩尔比约为1:1。进一步的,上述约为1:1可理解为1:(0.95-1.05)。
优选的,所述离子液体中还包括质量分数为4-40%的水。
优选的,所述制备方法还采用超声辅助萃取。
本发明还提供了一种海茸多糖提取液,由上述制备方法所制得。
本发明还提供了上述海茸多糖提取液在化妆品领域中的应用。上述海茸多糖提取液具备优良的抗氧化性能,因而可用于制备具有抗衰、祛皱等功效的化妆品产品。
本发明还提供了一种水凝胶乳液,包括以下组分:保湿剂、凝胶剂、乳化剂、交联剂、螯合剂、水、上述海茸多糖提取液。
上述水凝胶乳液可进一步用于制备如面膜、眼贴等具体产品。例如,将水凝胶乳液均匀倒入眼贴或面膜模具中,降温至室温,待乳液冷却结胶,即制得相应眼贴或面膜产品。
优选的,所述水凝胶乳液包括以下重量份数的组分:保湿剂1-10份、凝胶剂1-5份、乳化剂0.1-5份、交联剂0.1-5份、螯合剂0.01-1份、水50-70份、上述海茸多糖提取液2-30份。
优选的,所述保湿剂包括甘油、丙二醇、丁二醇、聚乙二醇、尿囊素、尿素、山梨醇中的至少一种。
优选的,所述凝胶剂包括角叉菜胶、魔芋胶、长脚豆角、结冷胶、海藻酸钠、聚乙烯醇、聚丙烯酸钠中的至少一种。
优选的,所述乳化剂包括白油、鲸蜡硬脂醇、单硬脂酸甘油酯、脂肪醇聚氧乙烯醚中的至少一种。
优选的,所述交联剂包括氯化钾、氯化钙、甘氨酸铝、氢氧化铝、氯化钠中的至少一种。
优选的,所述螯合剂包括乙二胺四乙酸二钠、乙二胺四乙酸三钠、乙二胺四乙酸四钠中的至少一种。
优选的,所述水凝胶乳液中还含有防腐剂。更优选的,所述防腐剂包括尼泊金甲酯、尼泊金乙酯、尼泊金丙酯、尼泊金丁酯、苯氧乙醇、苯甲酸钠、山梨酸钾中的至少一种。
本发明还提供了上述水凝胶乳液的制备方法,包括以下步骤:
将凝胶剂、螯合剂分散于保湿剂中,再投入水中进行搅拌,得到水相;将水相与乳化剂混合后,加入交联剂的水溶液;最后再加入海茸多糖提取液,制得所述水凝胶乳液。
相对于现有技术,本发明的有益效果如下:
(1)本发明采用乙醇对海茸进行前处理后,再以左旋肉碱和天然有机酸组成的离子液体提取海茸多糖,以该海茸多糖为原料制得的水凝胶对DPPH、ABTS、羟基自由基和超氧阴离子具有良好的清除效果,表现出优异的抗氧化性能。
(2)本发明采用乙醇对海茸进行前处理,可以沉淀得到更多的多糖;然后再以具有无毒、促渗以及本身具备抗氧化活性的天然离子液体作为提取载体,有效提高了海茸多糖的提取效率,并对海茸多糖的抗氧化性能起到了增效的作用;
(3)本发明还提出可将所得海茸多糖提取液应用于水凝胶产品,提高了保水性,显著降低了挥发性,延长了作用效果的持续时间。
附图说明
图1表示不同海茸多糖水凝胶的ABTS自由基清除测试结果;
图2表示不同海茸多糖水凝胶的DPPH自由基清除测试结果;
图3表示不同海茸多糖水凝胶的羟基自由基清除测试结果;
图4表示不同海茸多糖水凝胶的超氧阴离子清除测试结果。
具体实施方式
为了让本领域技术人员更加清楚明白本发明所述技术方案,现列举以下实施例进行说明。需要指出的是,以下实施例仅为本发明的优选实施例,对本发明要求的保护范围不构成限制作用,任何未违背本发明的精神实质和原理下所做出的修改、替代、组合,均包含在本发明的保护范围内。
以下实施例中所用的原料、试剂或装置如无特殊说明,均可从常规商业途径得到,或者可以通过现有已知方法得到。
实施例1
本实施例提供一种海茸多糖提取液,其制备方法包括以下步骤:
(1)将左旋肉碱与苹果酸按照摩尔比1∶1混合,加入左旋肉碱与苹果酸总质量的40%的去离子水,室温下超声(40KHz,30W)30min,直至形成均一、稳定、透明的天然离子液体溶液;
(2)将100g南极海茸丝用粉碎机打碎,过40目筛得到海茸粉末;
(3)将海茸粉末放入烧杯中,再加入1000mL体积分数为80%的乙醇,用磁性搅拌拌和,强烈搅拌2小时,离心(3000g×20min),去除上清后,在60℃真空干燥沉淀,得到预处理后的海茸粉末;
(4)将预处理后的海茸粉末与天然离子液体水溶液混合,在超声细胞破碎系统中进行双超声辅助萃取(150W,25min),再以2500rpm的转速离心5min,离心后收集上清液,重复洗涤三次,合并上清并用去离子水定容至100mL,得到海茸多糖提取液。
实施例2
本实施例提供一种海茸多糖提取液,其制备方法包括以下步骤:
(1)将左旋肉碱与酒石酸按照摩尔比1∶1混合,加入左旋肉碱与酒石酸总质量的40%的去离子水,室温下超声(40KHz,30W)30min,直至形成均一、稳定、透明的天然离子液体溶液;
(2)将100g南极海茸丝用粉碎机打碎,过40目筛得到海茸粉末;
(3)将海茸粉末放入烧杯中,再加入1000mL体积分数为80%的乙醇,用磁性搅拌拌和,强烈搅拌2小时,离心(3000g×20min),去除上清后,在60℃真空干燥沉淀,得到预处理后的海茸粉末;
(4)将预处理后的海茸粉末与天然离子液体水溶液混合,在超声细胞破碎系统中进行双超声辅助萃取(150W,25min),再以2500rpm的转速离心5min,离心后收集上清液,重复洗涤三次,合并上清并用去离子水定容至100mL,得到海茸多糖提取液。
实施例3
本实施例提供一种海茸多糖提取液,其制备方法包括以下步骤:
(1)将左旋肉碱与柠檬酸按照摩尔比1∶1混合,加入左旋肉碱与柠檬酸总质量的40%的去离子水,室温下超声(40KHz,30W)30min,直至形成均一、稳定、透明的天然离子液体溶液;
(2)将100g南极海茸丝用粉碎机打碎,过40目筛得到海茸粉末;
(3)将海茸粉末放入烧杯中,再加入1000mL体积分数为80%的乙醇,用磁性搅拌拌和,强烈搅拌2小时,离心(3000g×20min),去除上清后,在60℃真空干燥沉淀,得到预处理后的海茸粉末;
(4)将预处理后的海茸粉末与天然离子液体水溶液混合,在超声细胞破碎系统中进行双超声辅助萃取(150W,25min),再以2500rpm的转速离心5min,离心后收集上清液,重复洗涤三次,合并上清并用去离子水定容至100mL,得到海茸多糖提取液。
对比例1
本对比例提供一种海茸多糖提取液,其制备方法包括以下步骤:
(1)将100g南极海茸丝用粉碎机打碎,过40目筛得到海茸粉末;
(2)将海茸粉末放入烧杯中,再加入1000mL体积分数为80%的乙醇,用磁性搅拌拌和,强烈搅拌2小时,离心(3000g×20min),去除上清后,在60℃真空干燥沉淀,得到预处理后的海茸粉末;
(4)将预处理后的海茸粉末与去离子水混合,在超声细胞破碎系统中进行双超声辅助萃取(150W,25min),再以2500rpm的转速离心5min,离心后收集上清液,重复洗涤三次,合并上清并用去离子水定容至100mL,得到海茸多糖提取液。
本对比例以去离子水作为提取载体。
对比例2
本对比例提供一种海茸多糖提取液,其制备方法包括以下步骤:
(1)将水苏碱与丁酯戊酸按照摩尔比1∶1混合,加入水苏碱与丁酯戊酸总质量的40%的去离子水,室温下超声(40KHz,30W)30min,直至形成均一、稳定、透明的天然离子液体溶液;
(2)将100g南极海茸丝用粉碎机打碎,过40目筛得到海茸粉末;
(3)将海茸粉末放入烧杯中,再加入1000mL体积分数为80%的乙醇,用磁性搅拌拌和,强烈搅拌2小时,离心(3000g×20min),去除上清后,在60℃真空干燥沉淀,得到预处理后的海茸粉末;
(4)将预处理后的海茸粉末与天然离子液体水溶液混合,在超声细胞破碎系统中进行双超声辅助萃取(150W,25min),再以2500rpm的转速离心5min,离心后收集上清液,重复洗涤三次,合并上清并用去离子水定容至100mL,得到海茸多糖提取液。
本对比例以包含水苏碱和丁酯戊酸的离子液体作为提取载体。
产品效果测试
1.提取率测试
使用苯酚-硫酸法对实施例1-3、对比例1-2中的海茸多糖提取液进行多糖含量检测。首先绘制葡萄糖标准曲线,吸取葡萄糖标准溶液(0.1mg/mL)0、0.2、0.4、0.6、0.8和1.0mL置于试管中,各加蒸馏水至补足体积2mL,再加6%苯酚溶液1mL,摇匀,迅速加入5mL浓硫酸,摇匀后放置30min,吸取200μL待测液置于96孔板中,与490nm处测定吸光度,以葡萄糖浓度与吸光度绘制葡萄糖标准曲线:y=33.269x+0.0712;R2=0.9928。
再按上述方法进行对比例1-2和实施例1-5种中的海茸多糖提取液多糖含量测定,根据标准曲线计算浓度,从而获得提取率数值。
提取率=C*8*V/m
C:海茸多糖浓度(mg/mL);
V:提取液体积(mL);
m:海茸丝重量(g);
测试结果如表1所示:
表1提取率测试结果
海茸多糖提取液 | 吸光度A | 海茸多糖浓度C | 提取率(%) |
对比例1 | 0.270 | 0.005975533 | 4.78% |
对比例2 | 0.265 | 0.005825243 | 4.66% |
实施例1 | 0.670 | 0.017998738 | 14.40% |
实施例2 | 0.541 | 0.014121254 | 11.30% |
实施例3 | 0.520 | 0.013490036 | 10.79% |
由表1可知,对比例2中使用其他类型离子液体与对比例1中用水提取海茸多糖的提取率无明显差异;而相比于对比例1-2,实施例1-3海茸多糖提取液中海茸多糖的浓度显著更高。以上结果表明,采用以左旋肉碱和天然有机酸组成的离子液体对海茸多糖进行提取,其提取效率要明显优于去离子水或其他类型的离子液体。除此之外,通过实施例1-3的比较可知,不同有机酸与左旋肉碱配合后,所产生的效果也会产生差异,其中以苹果酸作为有机酸的实施例1提取效果最佳。
2.抗氧化性能测试
以实施例1-3、对比例1-2所制得海茸多糖提取液为原料,制得相应水凝胶乳液。
其中,水凝胶乳液包括以下重量份数的组分:
海茸多糖提取液20份、甘油4.5份、K型角叉菜胶0.5份、I型角叉菜胶0.6、魔芋粉0.42份、乙二胺四乙酸二钠0.01份、尿囊素0.1份、白油0.3份、鲸蜡硬脂醇0.15份、单硬脂酸甘油酯0.03份、脂肪醇聚氧乙烯醚0.03份、氯化钾0.2份、尼泊金甲酯0.1份、尼泊金丙酯0.01份和水73.05份。
水凝胶乳液的制备方法为:
(1)将K型角叉菜胶、I型角叉菜胶、魔芋粉、乙二胺四乙酸二钠、尿囊素、尼泊金甲酯均质分散于甘油中,然后再投入水中,充分搅拌并均质,升温至80℃,称为A相;将白油、鲸蜡硬脂醇、单硬脂酸甘油酯、脂肪醇聚氧乙烯醚、尼泊金丙酯混合,加热至80℃,称为B相;
(2)将B相加入A相中,充分搅拌、均质3分钟,降温到65℃,保温,称为C相;
(3)将氯化钾溶解于水中,然后加入C相,充分搅拌、均质3分钟,保温,称为D相;
(4)将海茸多糖提取液加入D相中,充分搅拌,保温,得到水凝胶乳液。
采用上述制备方法,分别制得包含实施例1-3、对比例1-2所制得海茸多糖提取液的相应水凝胶乳液。将所得水凝胶乳液倒至模具中,降温至室温,待乳液冷却结胶,得到相应的水凝胶。
以上述水凝胶作为待测样品,进行抗氧化性能测试。
2.1ABTS自由基清除测试
测试试剂
ABTS储备液(7mmol/L):取ABTS 0.0384g,加蒸馏水10mL。
K2S2O8储备液(2.45mmol/L):取K2S2O8 0.0066g,加蒸馏水10mL。
ABTS工作液:将0.2mL 7mmol/L ABTS储备液与0.2mL 2.45mmol/L K2S2O8混匀,静置12-16小时,配制成ABTS工作液。
Trolox标准液(0.3mmol/L,9.6mL,0.1042mg/mL):取Trolox 1mg,加蒸馏水9.6mL(MW=346.0)。
测试方法
取0.8mL ABTS工作液,用PBS溶液稀释40-50倍,要求在常温下734nm处吸光值为0.7±0.02。去0.8mL上述溶液与0.2g待测样品混合,常温避光静置6min,在734nm波长处测吸光度,平行3次。
清除率(%)=[A0-Ai/A0]×100%。
其中,A0为不加待测样品,仅加入ABTS的吸光度;Ai为加入待测样品和ABTS的吸光度。
由图1的测试结果可知,相比于对比例1,对比例2中使用其他类型离子液体作为提取载体,最终所制得的海茸多糖水凝胶对ABTS自由基清除率无明显提高。而采用实施例1-3中海茸多糖提取液所制得的水凝胶对于ABTS自由基的清除率均要高于对比例1-2,说明以含有左旋肉碱与天然有机酸组成的天然离子液体作为提取载体,所制得的海茸多糖水凝胶具有更强的ABTS自由基清除能力。
2.2DPPH自由基清除测试
测试试剂
除有另外说明外,所用试剂均为分析纯,水为符合GB/T 6682规定的一级水。
95%乙醇;
1,1-二苯基-2-三硝基苯肼(购自Sigma公司);
0.2mmol/L DPPH乙醇溶液:称取1,1-二苯基-2-三硝基苯肼(DPPH)0.0078g于250mL烧杯中,加入100mL无水乙醇,用玻棒搅拌至溶解,即得;
阳性对照:维生素E,纯度≥96%。
测试方法
将阳性对照用95%乙醇溶解稀释成0.08mg/mL、0.04mg/mL、0.02mg/mL、0.01mg/mL系列浓度梯度,以用以验证试验系统。
受试物处理:用水稀释为多级浓度样品。
参照下表2,使用10mL试管设立样品管(T)、样品本底(T0)、DPPH管(C)和溶剂本底(C0),每一样品的每个受试浓度的样品管(T)需设立3支平行管,同时DPPH管(C)也需设立3支平行管。
表2DPPH自由基清除测试体系
在样品管(T)和样品本底(T0)中各加入1mL相同浓度的样品溶液。
在所有试管中(T、T0、C、C0)用水补充至3mL,混匀。
在样品管(T)和DPPH管(C)中加入DPPH乙醇溶液1mL,样品本底(T0)和溶剂本底。
清除率(%)=[1-(T-T0)/(C-C0)]×100%。
T—样品管吸光值,即样品与DPPH反应后溶液吸光值;
T0—样品本底吸光值;
C—DPPH管吸光值3次平均值,即未加样品时DPPH溶液吸光值;
C0—溶剂本底吸光值
由图2的测试结果可知,相比于对比例1,对比例2中使用其他类型离子液体作为提取载体,最终所制得的海茸多糖水凝胶对DPPH自由基清除率无明显提高。而采用实施例1-3中海茸多糖提取液所制得的水凝胶对于DPPH自由基的清除率均要高于对比例1-2,说明以含有左旋肉碱与天然有机酸组成的天然离子液体作为提取载体,所制得的海茸多糖提取液具有更强的ABTS自由基清除能力。其中,采用实施例1-2中海茸多糖提取液所制得水凝胶的DPPH自由基清除率还优于实施例3,表明不同有机酸与左旋肉碱配合后,所产生的效果也会产生差异。
2.3羟基自由基清除测试
测试试剂
9mmol/L乙醇-水杨酸:称1.243g水杨酸,乙醇溶解,定容至100mL,然后稀释10倍;
9mmol/L硫酸亚铁:称2.502g FeSO4 7H20,去离子水溶解,定容至100mL,然后稀释10倍;
8.8mmol/L H2O2:称9.926g 30%H2O2,去离子水定容至100mL,然后稀释100倍。
测试方法
在比色管中依次先加入9mmol/L FeSO4,9mmol/L乙醇-水杨酸,接着加入适量去离子水,最后加入8.8mmol/L H2O2后摇匀,于37℃,水浴加热15min后取出,测其吸光度A0。A0测定时,参比溶液为不加双氧水的体系。按上述方法,加入下列表3所示的各溶液,来测定吸光度Ax、Axo。Ax和Axo测定时,参比溶液为去离子水。
羟基自由基清除率(%)=[A0-(Ax-Axo)]/A0×100%。
表3羟基自由基测试体系
由图3的测试结果可知,采用对比例2和实施例1-3中海茸多糖提取液所制得水凝胶的自由基清除率均高于对比例1,说明含有离子液体的海茸多糖提取液具有更强的羟基自由基清除能力,可对海茸多糖的羟基自由基清除能力起到增强的作用。
2.4超氧阴离子清除测试
测试试剂
邻苯三酚(5mmol/L):用10mmol/L HCl进行配制。
Tris-HCl缓冲溶液(0.05mol/L):用10mmol HCl配制浓度为0.1mol/L的三羟甲基氨基甲烷溶液。取50ml三羟甲基氨基甲烷溶液再与0.1mol/L盐酸溶液,调节pH为7.8,加水稀释至100ml,混匀。
测试方法
测试体系如下表4所示。
表4超氧阴离子清除测试体系
在4mL试管中,按表4测试体系依次加入Tris-HCl缓冲液和纯水/待测样品,再加入邻苯三酚,立即于319nm测定,每0.5min,读一次数,连续测定3min。以时间(min)为横坐标,以吸光值A为纵坐标,做回归曲线,得其斜率,即为氧化速率K。(阳性对照为:50μg/mL VC溶液)
清除率(%)=(ΔA0-ΔAs)/ΔA0×100%。
ΔA0:邻苯三酚自氧化速率;
ΔAs:加入样品后的自氧化速率。
由图4的测试结果可知,采用对比例1中海茸多糖提取液所制得水凝胶的超氧阴离子清除率为0,而对比例2和实施例1-3均具有很强的超氧阴离子清除率,以上结果表明海茸多糖本身并没有超氧阴离子清除能力,仅有离子液体本身可能具有较好的超氧阴离子清除能力。
3.挥发性测试
将上述制得水凝胶放置在室温环境下,不进行密封,测试其水分完全挥发时间,测试结果如表5所示。
表5挥发性测试结果
表5的结果表明,以实施例1-3、对比例1-2中海茸多糖提取液为原料,所制得的水凝胶乳液均具有良好的保水性,可有效延长贴敷于皮肤上的作用时间。
上面结合附图对本申请实施例作了详细说明,但是本申请不限于上述实施例,在所属技术领域普通技术人员所具备的知识范围内,还可以在不脱离本申请宗旨的前提下作出各种变化。此外,在不冲突的情况下,本申请的实施例及实施例中的特征可以相互组合。
Claims (9)
1.一种海茸多糖提取液的制备方法,其特征在于,包括以下步骤:
将海茸粉碎后与乙醇混合,离心取沉淀;采用包含左旋肉碱和天然有机酸的离子液体对所述沉淀进行萃取,制得海茸多糖提取液。
2.根据权利要求1所述的制备方法,其特征在于,所述天然有机酸选自顺丁烯二酸、柠檬酸、苹果酸、酒石酸、丙二酸、丙酸、脯氨酸、草酸中的至少一种。
3.根据权利要求1所述的制备方法,其特征在于,所述离子液体中左旋肉碱和天然有机酸的摩尔比约为1:1。
4.根据权利要求1所述的制备方法,其特征在于,所述离子液体中还包括质量分数为4-40%的水。
5.根据权利要求1所述的制备方法,其特征在于,所述制备方法还采用超声辅助萃取。
6.一种海茸多糖提取液,其特征在于,由权利要求1-6中任一项所述的制备方法所制得。
7.权利要求5所述的海茸多糖提取液在化妆品领域中的应用。
8.一种水凝胶乳液,其特征在于,包括以下组分:保湿剂、凝胶剂、乳化剂、交联剂、螯合剂、水、权利要求7所述的海茸多糖提取液。
9.权利要求8所述的水凝胶乳液的制备方法,其特征在于,包括以下步骤:
将凝胶剂、螯合剂分散于保湿剂中,再投入水中进行搅拌,得到水相;将水相与乳化剂混合后,加入交联剂的水溶液;最后再加入海茸多糖提取液,制得所述水凝胶乳液。
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