CN109620860B - 一种用于提取香椿多酚的溶剂及其应用 - Google Patents
一种用于提取香椿多酚的溶剂及其应用 Download PDFInfo
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Abstract
本发明公开一种用于提取香椿多酚的溶剂的制备方法,包括如下步骤:(a)将氯化胆碱与柠檬酸混合,在75‑85℃下在搅拌下进行形成均一的混合液;(b)将水加入所述均一的混合液,形成所述提取香椿多酚的溶剂。氯化胆碱、柠檬酸与水的摩尔比为:1:1.5‑2.5:3‑5。通过该方法获得的溶剂提取的香椿多酚含量明显高于水提或醇提方法获得的香椿多酚。
Description
技术领域
本发明属于医学领域,涉及一种用于提取香椿多酚的溶剂及其应用。
背景技术
香椿作为一种传统的中药材,其各个部位的组织已被用于治疗各种各样的疾病。其中茎与叶用来治疗痢疾、肠炎、湿疹和瘙痒等。其有效成分包括萜类、苯基丙烯类、类黄酮和蒽醌类等[1]。近年来其药理活性抗肿瘤、抗氧化、抗糖尿病、抗炎、抗菌、抗病毒等被研究的越来越多[2,3]。香椿多酚的提取方法,多是传统的水提、醇提、水提醇沉、丙酮-乙酸乙酯萃取法[4-6],但这些传统的方法存在原料损耗大,得率不高的问题。
近几年,低共熔溶剂法提取中药有效成分越来越显示出优势,并日益成为主流。
参考文献:
[1]Chen,G.H.,Huang,F.S.,Lin,Y.C.,Hsu,C.K.,Chung,Y.C.,2013.Effects ofwater extract from anaerobic fermented Toona sinensis Roemor on theexpression of antioxidant enzymes in the Sprague–Dawley rats.J.Funct.Foods 5,773–780.
[2]Feng,W.,Wang,M.,Cao,J.,Sun,J.,Jiang,W.,2007.Regeneration ofdenatured polyphenol oxidase in Toona sinensis(A.Juss.)Roam.ProcessBiochem.42,1155–1159.
[3]Hsieh,T.J.,Wang,J.C.,Hu,C.Y.,Li,C.T.,Kuo,C.M.,Hsieh,S.L.,2008.Effects of rutin from Toona sinensis on the immune and physiologicalresponses of white shrimp(Litopenaeus vannamei)under vibrio alginolyticuschallenge.Fish Shell-fish Immunol.25,581–588.
[4]Cheng,D.,Du,G.S.,Han,X.Y.,Zhang,T.L.,2007.Study of toxicityofToona sinensis health care tea.Chin.Prev.Med.18,576–579.
[5]Wu,C.C.,Liu,C.H.,Chang,Y.P.,Hsieh,S.L.,2010.Effects of hot-waterextract of Toona sinensis on immune response and resistance to Aeromonashydrophila in oreochromis mossambicus.Fish Shellfish Immunol.29,258–263.
[6]Cheng,K.W.,Yang,R.Y.,Tsou,S.C.,Lo,C.S.,Ho,C.T.,Lee,T.C.,Wang,M.,2009.Analysis of antioxidant activity and antioxidant constituents of Chinesetoon.J.Funct.Foods 1,253–259.
[7]王晓敏,杨慧,张乐,史冠莹,梁万平,王赵改.不同产地红油香椿各部位废弃材料主要活性物质含量比较[J].河南农业科学.2016(07).
[8]杨京霞,张鹏鹏.微波提取太和香椿黄酮类物质研究[J].黑龙江农业科学.2015(12)
[9]黄筑艳,刘力,乐意.Folin-Ciocalteu比色法测定香椿皮中多酚的含量.[J]广州化工.201442(4).
发明内容
香椿Toona sinensis(A.Juss.)Roemor(syn.Cedrela sinensis)叶中的多酚类具有降血压、降血糖、抗氧化等作用,其研究一直备受关注。目前香椿多酚的提取主要以水提法、醇提法为主,其得率相当的低,而使用绿色安全的溶剂作为溶媒的研究前所未见。
较为具体地,本发明第一方面提供了一种用于提取香椿多酚的溶剂,所述溶剂的原料包括氯化胆碱、柠檬酸与水。
在一些实施方式中,所述氯化胆碱、所述柠檬酸与所述水的摩尔比为:1:1.5-2.5:3-5。
本发明第二方面提供了一种用于提取香椿多酚的溶剂的制备方法,所述方法包括如下步骤:
(a)将氯化胆碱与柠檬酸混合,在75-85℃下形成均一的混合液;
(b)将水加入所述均一的混合液,形成所述提取香椿多酚的溶剂。
在一些实施方式中,所述氯化胆碱、所述柠檬酸与所述水的摩尔比为:1:1.5-2.5:3-5。
在一些实施方式中,步骤(a)中氯化胆碱与柠檬酸混合是在搅拌下进行的。
本发明第三方面一种用于提取香椿多酚的溶剂,所述溶剂是根据本发明第二方面所述的方法制备得到的。
本发明第四方面一种用于提取香椿多酚的提取方法,所述方法包括如下步骤:
(i)将香椿放置在本发明第一方面或第三方面所述的溶剂中,50-70℃,3500-4500rpm下均质化20-40min得到匀质化液;
(ii)将所述匀质化液在2000-3000rpm下离心1.5-2.5min,取上清液,即香椿多酚的粗品。
在一些实施方式中,所述方法还包括如下步骤:
(iii)将所述香椿多酚的粗品纯化,得到香椿多酚的纯品。
在一些实施方式中,所述方法还包括如下步骤:
将所述香椿多酚的粗品用AB-8树脂进行纯化,得到所述香椿多酚纯品。
在一些实施方式中,所述纯化包括如下步骤:
用分液漏斗萃取AB-8树脂纯化所述香椿多酚粗品后的流出液,回收上层得到如本发明第一方面或第三方面所述的溶剂。
通过该方法获得的溶剂提取的香椿多酚含量明显高于水提或醇提方法获得的香椿多酚。
附图说明
图1为没食子酸的吸光度标准曲线。
图2为DESS、醇、水所提取的香椿叶多酚浓度比较柱状图。
具体实施方式
为了更好的解释本发明的技术方案,下面结合附图详细介绍本发明的实施例。以下实施例用于进一步说明本发明,但不应理解为对本发明的固定或限制。若未特别指明,实施例中所用的技术特征可以替换为具有在不背离发明构思前提下等同或相似功能或效果的其他本领域已知的技术特征。
1.材料与方法
1.1材料
香椿老叶由安徽省抗衰老中草药研究中心提供(购自阜阳市太和县);柠檬酸(购自无锡市展望化工试剂有限公司);(购自天津市富宇精细化有限公司)和氯化胆碱(购自国药集团化学试剂有限公司);乙醇(>95%)等其他试剂均为分析纯。
1.2仪器
紫外分光光度计(BECKMAN COULTER,Germany);电子天平(上海精密科学仪器有限公司);智能恒温水浴锅(北京东方精瑞科技发展有限公司);旋转蒸发仪(安徽沃特科学仪器有限公司);KQ-50B型超声波清洗器。
1.3实验方法
1.3.1本发明溶剂的技术方案
本发明溶剂的合成步骤如下:
将氯化胆碱与柠檬酸按照摩尔比1:2置于锥形瓶中,80℃油浴并搅拌,直至形成均一的混合液。待均一的混合液形成后,将水加入前述混合液(按照摩尔比1:2)溶剂中,放置备用,下文简称DESS。
1.3.2香椿老叶多酚的提取
1.3.2.1本发明的方法提取香椿老叶多酚
将2g香椿老叶混合于25mL 1.3.1节所述本发明溶剂中,60℃,4000rpm,均质化30min,得匀质化液,将均质化液低速离心(2500rpm)2分钟,取上清液体,弃去沉淀,然后利用AB-8树脂进行纯化,最后将纯化后的总多酚溶液进行减压回收至小体积。放置用于后续实验。
AB8树脂的的预处理:大孔树脂用无水乙醇在室温下浸泡9h,使其充分溶胀。然后无水乙醇洗至白色浑浊,蒸馏水洗至中性,再用4%的的氢氧化钠溶液浸泡4小时,蒸馏水冲洗至中性,最后用4%的盐酸溶液浸泡4h,蒸馏水洗至中性,备用。
AB8树脂的纯化:准确称取AB8树脂15g置于柱子中,将预处理液(抽提液、DESS溶液)加入到柱子里(流速:1.5ml/min),待预处理溶液加入完全后,静置4小时,用分别用65%、70%、75%乙醇各20ml(流速:1.5ml/min)进行清洗,待流出的溶液透明后,收集香椿总多酚溶液。在55℃进行减压回收至2-3ml小体积。备用。
DESS的回收:对55摄氏度蒸出的溶液,用分液漏斗,进行萃取,将上层DESS溶液倒出,回收循环利用。
1.3.2.2醇提法提取香椿老叶多酚
参照赵大洲[7]方法制备醇法提取香椿老叶多酚,具体步骤为:
将2g香椿老叶按照固液比1:10,加入去75%乙醇,提取2次,每次30min,温度为70℃,抽滤,过AB8树脂,减压回收乙醇,得香椿多酚醇提浓缩液。过AB8树脂的详细步骤与1.3.2.1节相同。
1.3.2.1水提法提取香椿老叶多酚
参照杨京霞[8]方法制备水法提取香椿老叶多酚,具体步骤为:
将2g香椿老叶按照液固比1:30,加入去离子水,提取3次,每次25分钟,温度为60℃,抽滤,过AB8树脂,减压回收乙醇,得香椿多酚水提浓缩液。过AB8树脂的详细步骤与1.3.2.1节相同。
1.3.3绘制标准曲线
参照黄筑艳等的方法[9]称取没食子酸0.020g于100mL容量瓶中70%乙醇定容至刻度线(C=0.2mg/mL);各取0.0、1.0、2.0、3.0、4.0、5.0、6.0mL已配置好的溶液于25mL容量瓶中用70%乙醇定容至刻度线,所得溶液溶度各为0.000、0.008、0.016、0.024、0.032、0.040、0.048(mg/mL)。取所得溶液1mL,加入3mL 10%碳酸钠、5mL蒸馏水、1mL福林酚试剂,混匀后50℃水浴5min,757nm处测吸光值,用所得吸光值绘制标准曲线。
1.3.4香椿老叶多酚含量的测定
分别取1.3.2.1、1.3.2.2、1.3.2.3节的香椿多酚回收液0.1mL、用去离子水稀释100倍,测定香椿多酚浓度,以1.1.3节方法所制备的标准曲线进行浓度测定。
1.3.5数据分析
采用统计学的方法,对数据进行分析,文中所用的数据都是以(平均数±标准差)表示,采用SPSS 19.0对DESS和对醇、水提取香椿叶总多酚浓度进行显著性差异分析。
2结果
2.1标准曲线的绘制
根据1.3.3节的方法绘制标准曲线,回归方程Y=13.608X+0.0002,相关系数R2=0.9998。表明没食子酸浓度在0-0.056mg/mL范围内与吸光度存在较好的线性关系,标准曲线如图1所示。
2.2香椿老叶多酚含量的比较
1.3.4节中三种香椿老叶多酚含量的测定结果参见图2,具体数字参见表1。从中可以看出,本发明的DESS溶剂明显优于醇法与水法提取香椿老叶多酚含量。
表1三种方法提取的香椿多酚浓度比较
香椿多酚提取方法 | DESS法 | 醇提法 | 水提法 |
平均浓度(mg/ml) | 0.0592 | 0.0543 | 0.0398 |
3.结论与讨论
本研究以香椿老叶为原料,利用DESS作为提取溶剂,采用单一的多酚提取的最优匀质化法对香椿老叶总多酚进行快速提取。通过紫外分光光度法测定香椿老叶总多酚浓度,为香椿资源的充分利用提供了一定的依据。
实验结果表明,DESS基于匀质化法所提取的香椿总多酚浓度与对照组醇和水所提取的总多酚浓度相比增加显著,说明绿色低共熔溶剂匀质化提取香椿老叶的总多酚具有操作简单、成本低、便捷快速、绿色、环保等特点,提取多酚的量高于传统的提取方法。
随着香椿药理活性在临床的广泛应用,DESS作为一种新的有效成分的提取方法,不仅为香椿深加工提供了新的手段,也为香椿从科学研究转向工业化生产提供了技术创新。
以上各个实施例只是用于进一步说明本发明,并不是用来限制本发明的保护范围,凡是基于本发明的构思所作出的等同变换及对本发明的各个技术方案显而易见的改进,均落入本发明的保护范围。
Claims (4)
1.一种用于提取香椿多酚的提取方法,所述方法包括如下步骤:
(i)将香椿放置在溶剂中,50-70℃,3500-4500rpm下均质化20-40min得到匀质化液,其中,所述溶剂的原料包括氯化胆碱、柠檬酸与水,所述氯化胆碱、所述柠檬酸与所述水的摩尔比为1:2:4;
(ii)将所述匀质化液在2000-3000rpm下离心1.5-2.5min,取上清液,即香椿多酚的粗品。
2.如权利要求1所述的方法,所述方法还包括如下步骤:
(iii)将所述香椿多酚的粗品纯化,得到香椿多酚的纯品。
3.如权利要求2所述的方法,所述方法还包括如下步骤:
将所述香椿多酚的粗品用AB-8树脂进行纯化,得到所述香椿多酚纯品。
4.如权利要求2所述的方法,所述纯化包括如下步骤:
用分液漏斗萃取AB-8树脂纯化所述香椿多酚粗品后的流出液,回收上层得到溶剂。
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