CN115057899B - 一种从桑葚酒渣中提取花色苷的方法 - Google Patents
一种从桑葚酒渣中提取花色苷的方法 Download PDFInfo
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Abstract
本发明提供了一种从桑葚酒渣中提取花色苷的方法:(1)将桑葚酒渣加水粉碎,获得浆料;(2)按照体积比1:2‑1:8将浆料和提取溶剂混合,超声提取,然后固液分离,获得提取液;(3)将提取液以D101型大孔吸附树脂吸附,然后以90%v/v乙醇溶液为解吸液进行解吸,收集解吸液,去除解吸液后获得花色苷。本发明通过针对提取溶剂筛选提高了有效成分的释放量;还通过包埋的方式,解决储藏和运输过程中花色苷的不稳定问题该方法。该方法以加工剩余的桑葚酒渣为原料,提取了其中的花色苷,一方面降低了固体废渣总量,另一方面提高了桑葚利用率和附加值,为桑葚酒渣的深加工和再利用提供基础。
Description
技术领域
本发明属于食品领域,涉及一种从桑葚酒渣中提取花色苷的方法。
背景技术
桑葚,又名桑椹子、桑蔗、桑枣、桑果、桑泡儿、乌椹等,是桑树的成熟果实。桑葚果实较小、多汁的一类水果,其资源丰富,种类多,含有丰富的氨基酸、维生素、膳食纤维等营养成分,还含有大量的鞣花酸、花青素、类黄酮等生物活性物质,被称为“第三代黄金水果”。近几年全世界桑葚的种植面积和产量逐年增加,近些年来人们对桑葚的鲜食及加工利用逐年呈增强趋势,山东省已成为桑葚等特色浆果种植大省。
近几年桑葚果酒的加工量逐渐加大,加工过程中产生大量的酒渣,目前通常将作为废弃物扔掉,不仅造成果品资源的浪费,也造成了环境污染。因此,资源化利用桑葚酒渣称为亟需解决的问题。
发明内容
针对目前桑葚酒渣处理困难、利用率低的问题,本发明提供一种从桑葚酒渣中提取花色苷的方法,操作工艺简单,适于工厂规模化生产;所得的多糖纯度较高。
为实现上述目的,本发明采用如下技术方案。
一种从桑葚酒渣中提取花色苷的方法,包括以下步骤:
(1)将桑葚酒渣加水粉碎,获得浆料;
(2)按照体积比1:2-1:8将浆料和提取溶剂混合,超声提取,然后固液分离,获得提取液;
(3)将提取液以D101型大孔吸附树脂吸附,然后分离出大孔吸附树脂以水冲洗,然后以90%v/v乙醇溶液为解吸液进行解吸,分离出大孔吸附树脂,收集解吸液,去除解吸液后获得花色苷。
步骤(1)中,浆料中颗粒的平均粒径为低于50μm;在该粒径范围内,降低平均粒径能够提高花色苷提取率,尤其是粒径在20μm-45μm范围内;但细度超过一定范围,提升效果不再显著,因此,优选的平均粒径为20μm-30μm。
进一步地,粉碎的方式可以为机械剪切打浆,如采用胶体磨、打浆机,也可以采用高压均质打浆,还可以采用几种方式的组合。
步骤(1)中,浆料的固含量为30g/L。
步骤(2)中,提取溶剂为摩尔比为2:1的氯化胆碱和异丙醇的溶液。
步骤(2)中,固液分离的方式可以是过滤、离心等常规方法,并不影响目标物的提取率。
步骤(2)中,超声的条件可以根据花色苷的提取率进行筛选,优选地,超声的功率为300-800W;超声的温度为35-55℃;超声的时间为40min-90min。
步骤(3)中,D101型大孔树脂和提取液的质量体积比为3:1g/mL;D101型大孔树脂和乙醇溶液的质量体积比为5:3g/mL。
优选地,为了降低花色苷的降解,步骤(3)中还包括花色苷包埋步骤:称取花色苷2份,加入麦芽糊精1.5-2份、β-环糊精1-1.5份,羧甲基纤维素钠0.01份,卡拉胶0.01份,加入7-8份水混合,在45℃下均匀搅拌2h,通过喷雾干燥,获得花色苷包埋粉。
一种上述制备方法获得的花色苷或花色苷包埋粉。所述花色苷的纯度不低于85%ww。
一种上述花色苷或花色苷包埋粉在制备抗氧化剂、保健食品或药品中的应用。
本发明具有以下优点:
本发明以加工剩余的桑葚酒渣为原料,提取了其中的花色苷,一方面降低了固体废渣总量,另一方面提高了桑葚利用率和附加值,为桑葚酒渣的深加工和再利用提供基础。本发明中,桑葚酒渣大多含有一定量的水分,因此采用湿法超细粉碎技术,可提高原料的溶解性、分散性以及有效成分的提取率;酒渣中膳食纤维、多酚、多糖等成分含量丰富,会影响花色苷的提取,通过针对花色苷的高效提取溶剂筛选,提高了有效成分的释放量;本发明还通过包埋的方式,解决储藏和运输过程中花色苷的不稳定问题。
附图说明
图1是不同浓度桑葚酒渣中提取的花色苷对DPPH的清率除;
图2是不同时间点花色苷和花色苷包埋粉中花色苷的含量。
具体实施方式
下面结合实施例对本发明做进一步说明,但本发明不受下述实施例的限制。
实施例1 桑葚酒渣中花色苷的提取
(1)将含水量为30%w/w的桑葚酒渣(花色苷含量为4.65mg/g)按照质量比1:4加水,依次打浆、过胶体磨、然后高压均质粉碎,获得平均粒径25μm左右的浆料;
(2)取等量的几份浆料,按照体积比1:5分别加入摩尔比为2:1的氯化胆碱-丙三醇(H1)、氯化胆碱-尿素(H2)、氯化胆碱-葡萄糖(H3)、氯化胆碱-异丙醇(H4)、氯化胆碱-柠檬酸(H5)和乳酸-葡萄糖(H6)混合,以80%v/v乙醇溶液为对照(C),以功率500W、温度45℃超声提取60min,然后以4000rpm离心20min,获得上清液;
(3)在提取液中按照质量体积比3:1g/mL加入D101型大孔吸附树脂静态吸附4h,然后过滤分离出大孔吸附树脂以水冲洗,然后按照质量体积比为5:3g/mL加入90%v/v乙醇溶液解吸6h,分离出大孔吸附树脂,收集解吸液进行浓缩,浓缩液冻干获得花色苷。
采用pH示差法测定花色苷总含量:将花色苷配制一定浓度的溶液,取0.1mL溶液,向其中加入4.9mL的HCl(pH=1),摇匀后避光静置50min,分别测定510nm、700 nm波长处的吸光度(A510,A700);再取0.1mL提取液,向其中加入4.9mL的NaAc-HCl缓冲液(pH=4.5),摇匀后避光静置50min,分别测定510nm、700 nm波长处的吸光度(A’510,A’700);按照以下公式计算花色苷总含量X(mg/g):
式中:
M:矢车菊素-3-O-葡萄糖苷的摩尔质量,449.2g/mol;
ε:矢车菊素-3-O-葡萄糖苷的摩尔消光系数,26900;
V:溶液体积(mL);
N:稀释倍数;
m:桑葚酒渣的干质量(g)。
表1 不同提取溶剂的花色苷提取率
注:数据以平均值±标准偏差表示;与对照组相比,*p<0.05,**p<0.01。
不同提取溶剂从桑葚酒渣中提取花色苷的提取量,如表1所示。根据表1可知,与对照相比,H4的提取率最高,即氯化胆碱-异丙醇组合溶剂提取的效果最好,因此选择H4作为最优的提取溶剂。
实施例2 桑葚酒渣中花色苷的提取
(1)将含水量为30%的桑葚酒渣(花色苷含量为4.65mg/g)按照质量比1:4加水,采用打浆、过胶体磨、高压均质等方式进行粉碎,获得不同平均粒径的浆料;
(2)取等量的几份不同粒径的浆料,按照体积比1:4分别加入摩尔比为2:1的摩尔比为2:1的氯化胆碱和异丙醇的溶液,以功率800W、温度55℃超声提取40min,然后以4000rpm离心20min,获得上清液;
(3)在提取液中按照质量体积比3:1g/mL加入D101型大孔吸附树脂静态吸附4h,然后过滤分离出大孔吸附树脂以水冲洗,然后按照质量体积比为5:3g/mL加入90%v/v乙醇溶液解吸6h,分离出大孔吸附树脂,收集解吸液,喷雾干燥获得花色苷。按照实施例1的方式测定花色苷的含量,结果如表2所示。
表2 不同细度浆料的花色苷提取率
注:数据以平均值±标准偏差表示,不同字母表示p=0.05水平差异显著。
通过表2可以看出,不同的粉碎细度对桑葚酒渣中花色苷提取有着显著的影响,平均粒径低于50μm后,花色苷的提取量明显提高;当平均粒径下降至45μm左右时,观察到了更明显的提取量的提高;当粒径继续减小,提取量增加变化不再大幅变化;然而当平均粒径小于30μm后,提取量又大幅增加;过细小的粒径会增加粉碎成本和后续固液分离的难度,而且23μm相较于27μm,花色苷的提取量并没有显著增加,因此20-30μm的浆料细度更有利于花色苷提取。
实施例3 桑葚酒渣中花色苷提取、包埋及抗氧化性
(1)将含水量为30%w/w的桑葚酒渣(花色苷含量为4.65mg/g)按照质量比1:4加水,依次打浆、过胶体磨、然后高压均质粉碎,获得平均粒径25μm左右的浆料;
(2)将浆料按照体积比1:5分别加入摩尔比为2:1的氯化胆碱-异丙醇混合,以功率600W、温度45℃超声提取40min,然后以4000rpm离心20min,获得上清液;
(3)在提取液中按照质量体积比3:1g/mL加入D101型大孔吸附树脂静态吸附4h,然后过滤分离出大孔吸附树脂以水冲洗,然后按照质量体积比为5:3g/mL加入90%v/v乙醇溶液解吸6h,分离出大孔吸附树脂,收集解吸液进行浓缩,浓缩液冻干获得花色苷样品;
按重量称取花色苷2份,加入麦芽糊精1.5份、β-环糊精1.5份,羧甲基纤维素钠0.01份,卡拉胶0.01份,加入7份水混合,在45℃下均匀搅拌2h,然后喷雾干燥,获得花色苷包埋粉;
按照实施例1中的方法进行测定,并按照以下公式计算花色苷样品和包埋粉中花色苷的含量(%):
式中:
M:矢车菊素-3-O-葡萄糖苷的摩尔质量,449.2g/mol;
ε:矢车菊素-3-O-葡萄糖苷的摩尔消光系数,26900;
V:溶液体积(mL);
N:稀释倍数;
m’:称取花色苷的质量(mg);
经计算,花色苷样品的纯度为(87.92±0.557)%,花色苷包埋粉中花色苷的含量为(35.29±0.297)%。
称取花色苷样品配制成约20μg/mL、40μg/mL、60μg/mL、80μg/mL、100μg/mL的溶液,以同浓度的Vc为对照进行DPPH自由基清除实验。结果见图1,自由基清除能力与花色苷质量浓度成正相关性;当花色苷的质量浓度在20-80μg/mL范围内,清除能力显著性增强。Vc对DPPH自由基一直保持着较高的清除率。
将花色苷样品和花色苷包埋粉存放于45℃的烘箱内,每隔24h测定其花色苷的含量,计算花色苷的保留率:花色苷保留率= 储存后花色苷的总含量/花色苷原始含量×100%。结果如图2所示,在45℃的条件下,未包埋的花色苷浓缩物中花色苷含量下降较为明显,从刚开始100%的保留率,到第五天保留率仅有(27.67±0.23)%,花色苷含量损失较大;通过包埋后花色苷的保存率从刚开始的100%降至(96.68±3.10)%,花色苷含量损失较少。
Claims (4)
1.一种从桑葚酒渣中提取花色苷的方法,其特征在于,包括以下步骤:
(1)将桑葚酒渣加水粉碎,获得浆料;
(2)按照体积比1:2-1:8将浆料和提取溶剂混合,超声提取,然后固液分离,获得提取液;(3)将提取液以D101型大孔吸附树脂吸附,然后分离出大孔吸附树脂以水冲洗,然后以90%v/v乙醇溶液为解吸液进行解吸,分离出大孔吸附树脂,收集解吸液,去除解吸液后获得花色苷;
步骤(2)中,提取溶剂为摩尔比为2:1的氯化胆碱和异丙醇的溶液;
步骤(1)中,浆料中颗粒的平均粒径为20μm-30μm;
步骤(2)中,超声的功率为300-800W;超声的温度为35-55℃;超声的时间为40min-90min;
步骤(3)中,D101型大孔树脂和提取液的质量体积比为3:1g/mL;D101型大孔树脂和乙醇溶液的质量体积比为5:3g/mL。
2.根据权利要求1所述的方法,其特征在于,步骤(1)中,浆料的固含量为30g/L。
3.根据权利要求1所述的方法,其特征在于,步骤(1)中,粉碎的方式为机械剪切或高压均质或两者的组合;步骤(2)中,固液分离的方式为过滤或离心。
4.根据权利要求1所述的方法,其特征在于,步骤(3)中还包括花色苷包埋步骤:称取花色苷2份,加入麦芽糊精1.5-2份、β-环糊精1-1.5份,羧甲基纤维素钠0.01份,卡拉胶0.01份,加入7-8份水混合,在45℃下均匀搅拌2h,通过喷雾干燥,获得花色苷包埋粉。
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