CN107405296A - 通过用助溶溶液挤出来制备植物性来源的基质的提取物的方法 - Google Patents
通过用助溶溶液挤出来制备植物性来源的基质的提取物的方法 Download PDFInfo
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- CN107405296A CN107405296A CN201680016070.3A CN201680016070A CN107405296A CN 107405296 A CN107405296 A CN 107405296A CN 201680016070 A CN201680016070 A CN 201680016070A CN 107405296 A CN107405296 A CN 107405296A
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Abstract
本发明涉及用于制备植物性来源的基质,特别是植物基质的提取物的方法,其特征在于,与热处理联合或未联合地,在水溶液存在下,植物性来源的基质经受机械处理,所述机械处理在于在挤出机中挤出植物性来源的基质,所述水溶液含有至少一种助溶剂,特别地,所述助溶剂的浓度至少等于其最小助溶浓度,随后进行回收提取物的操作。
Description
技术领域
本发明的领域涉及通过用助溶溶液挤出来制备植物性基质提取物的方法。
背景技术
挤出是一种迫使可在各种受控条件下流动的材料以确定的速率通过模具的过程(Dziezak,J.D.(1989).Single and twin–screw extruders in food processing.FoodTechnol.,四月,164-174)。最初,这种技术在18世纪末的英国用于冶金工业中。后来,它被引入农产品工业中用于生产香肠和面食产品。食品工业目前正在大量使用这种挤出技术用于烘烤挤制淀粉制品(饼干、甜面包干、点心等),而且还用于使蛋白质组织化以及用于生产宠物食品和动物饲料产品。
并行地,挤出技术还主要被发展用于热塑性塑料工业,并导致新螺杆的设计、在该技术的进一步改进和对新应用的扩展。
数项研究集中于使用挤出机在单个步骤中连续不断地进行化学、机械、热机械作用,以用于例如提取半纤维素(N’Diaye,S.,Rigal,L.,Larocque,P.,Vidal,P.F.,1996.Extraction of hemicelluloses from poplar populus tremuloides,using anextruder type twin–screw reactor:A feasibility study.Bioresearch Technology57,61-67)、果胶(Marechal V.,Rigal L.Characterization of by-products ofsunflower culture-Commercial applications for stalks and heads(1999)Industrial Crops and Products,10(3),第185-200页)等。在这些情况中,将酸或碱性溶剂与植物性原材料同时添加到挤出机中,以促进期望的大分子的提取和溶解(反应性挤出)。
已经已知一些用于植物提取的应用:使用单螺杆挤出机将油从油种子中榨出来,而未将任何溶剂注入机筒中,这种油提取基于固体的压缩(Sriti J.,Talou T.,Faye M.,Vilarem G.and Marzouk B.Oil extraction from coriander fruits by extrusion andcomparison with solvent extraction processes.(2011)Industrial Crops andProducts,33,659-664)。
还将挤出用于预处理与固体介质如玉米淀粉混在一起的果渣(苹果、黑醋栗、蔓越莓)以增加酚类化合物的提取(White Brittany L.,Howard Luke L.,Prior Ronald L.,Polyphenolic composition and antioxidant capacity of extruded cranberrypomace.(2010),J.Agric.Food Chem.58,4037-4042.)。
在植物提取的领域中,根据所用的溶剂,植物细胞的细胞膜或多或少地变弱,这会使得或不会使得释放它们所含有的化合物。
水无疑是一种天然溶剂,其被认为是可再生的;然而,其强烈的极性不允许某些感兴趣的亲脂性分子的提取。
助溶剂(agents hydrotopes)是水溶性有机化合物,其在达到称为“CMH”(最小助溶浓度Concentration Minimale Hydrotropique)的某一浓度以上,使得在常规条件下几乎不溶于水的有机化合物的溶解度显著增加。助溶剂是两亲性的,其可以是离子型(阴离子、阳离子、两性离子)或非离子型(间苯二酚、烟酰胺、烷基多糖苷等),并且可以具有各种结构例如芳香族、脂肪族、环状或非环状的结构。助溶剂是以任何比例溶于水的、且没有任何表面活性剂性质的化合物。
最小助溶浓度(CMH)是一种浓度,自该浓度以上,助溶剂开始形成聚集体,即,具有一些物理性质的新的微环境,所述物理性质不同于当化合物被稀释时所观察到的那些,并且不同于胶束行为。这种最小助溶浓度对于每种助溶剂而言是特异性的,并且通常具有摩尔浓度的数量级。其能够通过数种物理化学方法来确定,例如通过测量表面张力、电导率或者动态或静态光散射来确定(Self-association of Nicotinamide in aqueoussolution:Light-scattering and vapor pressure osmometry studies(1996)85(8):848-853)。
CMH能够使用数种物理化学方法来确定,例如通过测量表面张力、电导率、动态和静态光散射来确定(Self-association of Nicotinamide in aqueous solution:Light-scattering and vapor pressure osmometry studies(1996)85(8):848-853),或者非常简单地通过绘制亲脂性化合物的溶解曲线(溶解的溶质含量相对于助溶剂浓度)来确定。苏丹红(一种易于通过分光光度法测定的亲脂性染料)能够被用作参比。该浓度的值取决于助溶剂的类型,而不取决于溶质的类型。其对应于最小浓度,达到该最小浓度以上,溶质的溶解曲线变成指数曲线。
已经研究了助溶剂为某些分子在水性介质中作为溶解佐剂的潜力(Da SilvaR.C.,Spitzer M.,Da Silva L.H.M.,Loh W.Investigations on the mechanism ofaqueous solubility increase caused by some hydrotropes.(1999)ThermochimicaActa 328,161-167)。也已证实了离子助溶剂在水性介质中用于提取植物源代谢物时作为佐剂的潜力(Dandekar D.V.,Jayaprakasha G.K.,Patil B.S.,Hydrotropic extractionof bioactive limonin from sour orange(Citrus aurantium L.)seeds.(2008)FoodChemistry,109,515-520)。
仍然需要改进现有的提取方法,以达到尤其是减少它们的环境影响并提高所得提取物的质量的目的。
发明内容
本申请人已经证明通过用助溶溶液(solution hydrotropique)挤出来制备植物性基质的提取物的方法是特别有利的,因为它使得获得的提取物富含感兴趣的化合物并且处于更宽的极性范围内;同时降低能耗。有利地,该方法还提供了用替代性溶剂替代源自石化工业的常规溶剂的可能性,所述替代性溶剂是环境友好型的并且还促使获得特别适用于药物、化妆品或农产品用途的提取物。
本发明涉及一种通过挤出在水助溶溶液存在下来提取干燥或新鲜的植物性基质的方法,其中所述水助溶溶液以足以提取出亲脂性化合物的量含有至少一种离子型或非离子型助溶剂。该挤出使得总提取物在非常短的时间内获得,具有要比常规提取低得多的重量/溶剂比例,并具有相当的、甚至是更好的质量。因此,该方法的环境影响在很大程度上得以改进。此外,在本发明中,提取物可以是总提取物(含有极性、中等极性和亲脂性的化合物),或者由于用助溶溶液选择提取性而富含感兴趣的亲脂性化合物。
更具体地,本发明涉及一种获得植物性基质提取物的方法,其特征在于,与热处理联合或未联合地,在水溶液存在下,所述新鲜或干燥的植物性基质经受机械处理,由此在挤出机中挤出基质,所述水溶液优选以最小助溶浓度含有至少一种助溶剂,随后进行回收提取物的操作。
根据本发明,以至少等于最小助溶浓度(CMH)的浓度含有至少一种助溶剂的水溶液,是指以等于或高于先前指出的最小助溶浓度(CMH)的浓度含有至少一种助溶剂的水溶液。还必须考虑到可能含于植物性基质中的水含量,从而相应地调节助溶剂的浓度以使得将其适当地用在本发明的方法中。
根据本发明的另一个特征,助溶剂在所述水溶液中的浓度为最小助溶浓度(CMH)的1至10倍,优选1至6倍,更优选1至2倍,进一步优选1.4至1.8倍。有利地,在实践中,助溶剂能够以1.5mol/L的浓度用在水溶液中。
根据本发明的另一个有利的特征,助溶剂以如下浓度包含于水提取溶液中:以相对于所述溶液的重量计小于60重量%,优选以相对于所述溶液的重量计小于50重量%,更优选以相对于所述溶液的重量计小于40重量%,进一步优选以相对于所述溶液的重量计小于30重量%。将特别地观察到,该浓度阈值隐含地排除使用乙醇作为溶剂以提取亲脂性化合物,因为乙醇通常以高得多的含量,在80%数量级使用。此外,由于通过这种特定溶剂的挥发性和易燃性而引起的风险,乙醇在挤出机中的使用必然意味着安全环境。
在本发明的一个特别的实施方案中,离子或非离子助溶剂能够选自:正丁基苯磺酸钠,枯烯磺酸钠,对甲苯磺酸钠或二甲苯磺酸钠,庚基葡萄糖苷烷基糖苷(heptyglucoside alkylglycosides)和烷基多糖苷,二甲基异山梨醇,N,N-二乙基烟酰胺,N,N-二甲基苯甲酰胺,异戊二醇,单独或混合使用它们。
在本发明中,“亲脂性化合物”是指具有正的正辛醇-水分配系数(也被称为log P或log kow)的化合物。
根据本发明的一个特征,助溶剂为离子型,特别地选自烷基苯磺酸盐如枯烯磺酸钠和二甲苯磺酸钠。
根据本发明的一个有利的特征,助溶剂为非离子型,优选为农业来源的,特别地选自通式Alk-O-Zp的烷基-(多)糖苷,其中:
·Alk表示具有3至7个碳原子的、饱和或不饱和的、直链或支链疏水性脂肪族烃片段;以及
·Z为亲水性糖苷基团,例如葡萄糖、木糖和阿拉伯糖;以及
·1<p<5。
根据一个特别的实施方案,Z为葡萄糖基团。
根据本发明的另一个特别的实施方案,Z为木糖基团。
根据本发明的另一个特别的实施方案,Z为阿拉伯糖基团。
根据本发明的一个特别的实施方案,Alk表示具有7个碳原子的、饱和或不饱和的、直链或支链疏水性脂肪族烃片段。
根据本发明的另一个特别的实施方案,Alk表示具有6个碳原子的、饱和或不饱和的、直链或支链疏水性脂肪族烃片段。
根据本发明的进一步特别的实施方案,Alk表示具有5个碳原子的、饱和或不饱和的、直链或支链疏水性脂肪族烃片段。
根据本发明的进一步特别的实施方案,Alk表示具有4个碳原子的、饱和或不饱和的、直链或支链的疏水性脂肪族烃片段。
在本发明的另一个实施方案中,助溶剂为农业来源的(非石化来源的)。
根据本发明的另一个特征,农业来源的助溶剂为源自蓖麻属(ricin)的C7脂肪醇与小麦葡萄糖(非转基因(sans OGM))的组合。
根据本发明的一个有利的特征,所述助溶剂为戊基糖苷,其疏水性戊基片段对应于通过使甜菜根或马铃薯淀粉发酵而获得的C5醇,该糖苷片段源自谷物。
根据本发明的一个有利的特征,所述助溶剂为C4脂肪醇与木糖苷的组合。
在本发明的另一个特别的实施方案中,所述农业来源的助溶剂优选为二醇,特别是异戊二醇(3-甲基-1,3-丁二醇)。
根据本发明的一个特征,助溶剂为非离子型,特别地选自异戊二醇、庚基葡萄糖苷和丁基木糖苷。
在本发明中有用的非离子两亲性化合物可有利地为市售原材料SEPICLEAR(SociétéSEPPIC)、(Société WHEATOLEO)、Kuraray的异戊二醇之一。
根据本发明的另一个特征,在挤出前对植物性基质进行预处理。根据本发明,“预处理”是指选自以下处理中的处理:超声,微波,酶消化,在助溶溶液中的浸渍,植物性基质的制备如低温研磨、粉碎、研磨等。
在本发明的一个特别的实施方案中,预处理包括在挤出步骤之前的在助溶溶液中的浸渍。
根据本发明,“挤出”是指机械处理,由此在单螺杆挤出机或双螺杆挤出机(具有同向旋转或反向旋转的螺杆)中,优选在双螺杆挤出机中挤出植物性基质,无论是否与热处理联合。
挤出在20至200℃,优选60至120℃的温度进行。
根据本发明的另一个特征,挤出在双螺杆挤出机中进行。
根据本发明的一个有利的特征,双螺杆挤出机包括第一同向旋转和同向穿透的双螺杆区,在该处进行所述植物性基质的研碎。
该方法使用挤出机,优选双螺杆挤出机,其具有末端为过滤机筒的数个机筒,允许温度变化,并且在同时施加剪切下,植物性原材料的强烈混合导致大量化合物的夹带以及物质的分解。
以确定的流速向挤出机输送植物性基质和助溶溶液,以获得1P/1V至1P/10V,优选1P/2V至1P/6V的植物性基质重量(千克)/溶剂体积(升)的比例。
本发明还涉及以最小助溶浓度含有至少一种助溶剂的水溶液在提取新鲜或干燥的植物性基质的方法中的应用,通过在挤出机中进行的机械处理来实施。挤出的条件和所用植物性基质的类型与结合本发明方法所描述的那些相同。
在本发明中,“植物性基质(matrice végétale)”是指植物、真菌、地衣、藻类、微藻类培养物或去分化的植物细胞培养物的全部或部分。
所述植物、真菌、地衣、藻类是干燥的或新鲜的,冷冻的或解冻的,并且是完整的(未经粉碎的且未经研磨的)、经粉碎的或经研磨的。所述微藻类培养物或去分化的植物细胞培养物是完整的,经研磨的,优选新鲜的或干燥的,经过滤以回收生物质,可以已经经受或未经受预处理,例如通过超声方法预处理以释放细胞内的内容物。
“植物部分”尤其是指地上部分,例如茎、枝、叶子、果实、种子和/或花;和/或地下部分,例如根茎、根和/或球茎。
“地衣、真菌或藻类部分”是指这些生物体的任何器官,例如叶状体(thalles)、子实体、大型真菌(macromycetes)、菌丝体和/或丝状体。
在本发明的一个特别的实施方案中,使用整个植物(未经粉碎的、未经研磨的)的全部或部分。
能够在本发明中使用的植物中,可以特别地提及:灯笼草(Physalis peruviana)的果实、白花酸藤果(Embelia ribes)的果实、香桃木(Myrtus communis)的叶子、蓝桉树(Eucalyptus globulus)的叶子、山竹(Garcinia mangostana)的果皮、啤酒花(Humuluslupulus)的雌花序、金鸡钠树属物种(Cinchona sp.)的树皮、荨麻(Urtica dioica)的地上部分、蜡菊属物种(Helichrysum spp.)的地上部分、香荚兰属物种(Vanilla spp.)的果实、生姜(Zingiber officinale)的根茎、姜黄属物种(Curcuma spp.)的根茎、卡瓦胡椒(Pipermethysticum)的根茎、胡椒属物种(Piper spp.)的叶子、油橄榄(Olea europaea)的果实和叶子……
能够在本发明中使用的藻类中,特别是指蓝藻(algues bleues)或蓝藻(Cyanobactéries),以及真核生物中的裸藻,隐藻(Cryptophytes),定鞭藻(Haptophytes),灰胞藻;红藻(algues rouges)或红藻(Rhodophyta),不等鞭毛门(Stramenopiles)特别地集合了硅藻和褐藻(algues brunes)或褐藻(Phéophycées),以及最后的绿藻特别地包括石莼纲。
能够在本发明中使用的地衣中,可以特别地提及:冰岛地衣(Cetrariaislandica)的叶状体、松萝属物种(Usnea spp.)的叶状体、石蕊属物种(Cladonia spp.)的叶状体、肺衣属物种(Lobaria spp.)的叶状体。
能够在本发明中使用的真菌中,可以特别地提及:彩绒革盖菌(Coriolusversicolor)、冬虫夏草属物种(Cordyceps spp.)。
能够在本发明中使用的植物细胞的培养物中,可以特别地提及:含羞草(Mimosapudica)细胞培养物、雷公藤(Tripterygium wilfordii)细胞培养物。
在一个实施方案中,挤出的特征在于使干燥或新鲜的植物性基质通过双螺杆挤出机,所述双螺杆挤出机包括:
-进料区:进料斗;
-挤出机的主体,所述主体包括一个或多个机筒,含有旋转的环状螺杆(同向旋转或反向旋转),或螺杆段。优选地,存在数个连续的相邻的机筒。优选地,存在两个同向旋转的环状螺杆。螺杆的轮廓可以根据螺杆的螺纹(例如梯形、共轭、单或双......)和螺距而变化。这些螺杆中的每一个还可以具有不同的段,所述不同的段可以通过螺纹的形状和/或螺距而彼此不同。任选地,这些螺杆的一些构成段还可对应于单裂片或三裂片混合元件;
-用于输送充当溶剂的助溶剂水溶液的装置,所述进料装置与至少一个机筒相连接;
-至少一个过滤机筒,其:
√任选地进行用于固/液分离的操作;
√还包括过滤装置如网格,以及;
√特别地位于挤出机的出口处;
-加热和冷却装置,由于机筒必须为可调节温度的:20℃至200℃。
-挤出机驱动装置,例如:
√驱动单元:包括齿轮电机和扭矩分配器,它们提供旋转螺杆所需的机械功率;
√自动操纵装置:用于监测和控制过程。可调节的参数为:螺杆的旋转速度和每个机筒的温度。
双螺杆挤出的机械过程导致植物性堵塞物的形成,这使压力施加到材料上,从而导致细胞破裂,植物性材料的分解使得提取出最大量的被夹带且被溶解在助溶溶液中的化合物。
通过澄清和/或过滤能够达到提取物的收集,由此含有感兴趣的化合物的溶剂与植物性基质的残留固体残余物分离。
“澄清(clarification)”是指在离开挤出机时去除包含在提取物中的细胞碎片。这种去除能够使用在离心效应下的澄清技术来获得,其目的是去除会妨碍过滤介质的固体残余物。这种去除还能够直接通过用佐剂过滤来获得。
“过滤”是指正面或切向过滤,其中可以考虑过滤佐剂(珍珠岩、硅藻类等)的存在。这种过滤拦住了最后的固体残余物,目的是获得完全澄清的溶液。其后能够进行膜过滤,所述膜过滤具有根据所要考虑的分子的尺寸而确定的截断阈值。其还能够被在树脂或二氧化硅上的过滤替代,或者其后能够进行在树脂或二氧化硅上的过滤(例如吸附树脂),以获得更富集含量的感兴趣的化合物。
在一个特别的实施方案中,使用整合在挤出机末端处的过滤机筒进行澄清-过滤步骤。
在一个特别的实施方案中,提取物被按原样储存或者冷冻干燥,其包含感兴趣的分子与助溶剂,后者允许在终产物中更好地溶解。
由此获得含有宽范围极性(极性、中等极性、非极性)的化合物的总提取物。
还能够将提取物在一定体积的水中稀释,向其可以添加或不添加一种或多种选自盐、酸或碱的佐剂,从而得到低于CMH的助溶剂的最终浓度。因此,可以通过沉淀和固/液分离(例如过滤或离心)来回收亲脂性化合物。
以这种方式,获得富含亲脂性化合物的提取物。
感兴趣的亲脂性化合物可以为黄酮类、酚酸类、萜烯化合物(单-萜烯、二-萜烯、三萜烯)和甾醇化合物、二芳基庚烷衍生物、木脂素类、香豆素类、醌类、蒽醌类、呫吨酮类、间苯三酚类、环烯醚萜类、倍半萜内酯类、生物碱类、蔗糖酯类、极性脂质......
特别地,它们可以为卡瓦内酯类、香桃木醇类(myrtucommulones)、蒽贝素、奎宁及其衍生物、香草醛及其衍生物,α-倒捻子素、黄腐酚、单半乳糖二酰基丙三醇和二半乳糖二酰基丙三醇、山楂酸、熊果酸、迷迭香酸、鼠尾草酚、高良姜素、短叶松素、小豆蔻明、姜黄素类、姜辣素、姜烯酮......
总提取物或富含亲脂性化合物的提取物可以被稀释、浓缩、干燥,或者通过向期望的终产物中加入合适的经批准的防腐剂(例如二醇类、或山梨酸、苯甲酸、柠檬酸及其盐等),或酒精(最低15°)来按原样储存。
为了提供干燥的提取物,可以考虑真空干燥、冻干或喷雾干燥技术。所获得的提取物可以用或不用介质干燥,和/或溶解在液体介质中。
获得的如上所定义的液体、糊剂或干燥的提取物可以被按原样用于旨在通过局部途径或口服途径施用的化妆品、药物或食品组合物中。
与反应器提取相比,通过挤出的助溶提取的优势是:
-所使用的溶剂量显著减少(平均低2至5倍);
-提取时间显著减少(2至5分钟,相较于至少1小时);
-能够使用替代的农业来源的溶剂(例如特别是聚烷基糖苷),而不是石化来源的污染性溶剂(乙酸乙酯、丙酮、己烷……)
-获得的提取物的质量(提取物具有宽范围的极性或提取物富含感兴趣的亲脂性化合物;以及在感兴趣的亲脂性化合物中还观察到选择性)。
根据一个优选的实施方案,除了助溶溶液之外,在恰当所谓的挤出步骤中不使用其它溶剂。助溶溶液是在通过挤出的提取方法中所涉及的唯一溶剂。
作为非限制性的指示例给出以下实施例。
具体实施方式
实施例
实施例1:香桃木(Myrte)提取物
将1.3kg的香桃木(Myrtus communis)的干燥叶子以8kg/H的速率输送至ClextralBC45双螺杆挤出机的第一机筒中。然后以1.5mol/L和24L/H的速率添加戊基木糖苷的水溶液。施加到不同机筒的温度为60℃/60℃/60℃/60℃/60℃。在5分钟后,通过允许固/液分离的过滤机筒在出口处回收香桃木叶子的提取物。在澄清后,获得干燥香桃木的提取物,其相对于所用溶剂的产率为81%,相对于植物进料的产率为1184%。将溶液稀释在4体积的水中。在离心后,获得对应于富含香桃木的提取物的残余物,其相对于植物进料的重量产率为1.2%。
为了比较,在相同的条件下,在水中提取1.3kg的香桃木的干燥叶子。在澄清后,获得相对于植物进料的产率为8.5%的香桃木提取物。
在两种提取物中和在反应器中获得的两种提取物中测定了香桃木醇B'、S和A。
虽然提取重量产率较低,但是通过使用在反应器中不可行(不足以使植物润湿)的植物重量/溶剂体积比例的,并且使用相当快的提取时间的挤出所获得的提取物,具有比通过在反应器中使用相同溶剂的常规提取所获得的提取物略高的香桃木醇浓度。它还具有比在反应器中使用乙酸异丙酯所获得的提取物更高的香桃木醇浓度。富含在通过挤出获得的助溶提取物中的香桃木醇A(为最非极性的)是在使用乙酸异丙酯的提取物中的两倍,这证明了该方法的选择性。通过用水而不是用戊基木糖苷的挤出所获得的提取物不能提取出感兴趣的化合物。
实施例2:通过挤出的蜡菊(Helichrysum gymnocephalum)的提取物
将5kg的蜡菊整个的、干燥的地上部分以10kg/H的速率输送至Clextral BC45双螺杆挤出机的第一机筒中。以60L/H的速率添加含有50%庚基葡萄糖苷m/m(1.5M)的水溶液。施加到不同机筒的温度为60℃/60℃/60℃/60℃/60℃。在5分钟后,通过允许固/液分离的过滤机筒在挤出机的出口处回收蜡菊提取物。在澄清后,获得蜡菊提取物,其相对于所用溶剂的产率为69.5%,相对于植物进料的产率为407%。
虽然产率较低,但是通过使用降低直至5倍的溶剂体积(在反应器中不可行(不足以是植物润湿)的重量/溶剂比例)的,并且使用相当快的提取时间的挤出所获得的提取物质量,与通过使用相同溶剂的常规提取所获得的提取物质量相当。通过用水而不是用庚基葡萄糖苷挤出所获得的提取物不能提取出这些感兴趣的化合物。
实施例3:干燥荨麻(ortie)和新鲜荨麻的提取物
将0.67kg的荨麻的地上部分以8kg/H的速率输送至Clextral BC45双螺杆挤出机的第一机筒中。以36kg/H的速率添加含有10%庚基葡萄糖苷m/m的水溶液,其对应于使用1/4.5的重量/体积比例的提取,而考虑到干燥荨麻的地上部分的低密度,在分批操作中却并不可行。施加到不同机筒的温度为60℃/60℃/60℃/60℃/60℃。在5分钟后,通过允许固/液分离的过滤机筒在挤出机的出口处回收干燥荨麻提取物。在澄清后,获得荨麻提取物,其相对于所用溶剂的产率为48.7%,相对于植物进料的产率为218%。
将4.4kg的新鲜荨麻的地上部分以33kg/H的速率输送至Clextral BC45双螺杆挤出机的第一机筒中。以17kg/H的速率添加含有10%庚基葡萄糖苷m/m的水溶液,其对应于使用1/0.5的重量/体积比例的提取,但如果考虑到植物的水含量,实际上为1/6的重量/体积比例。这是不可能在分批操作中进行的。施加到不同机筒的温度为60℃/60℃/60℃/60℃/60℃。在8分钟后,通过允许固/液分离的过滤机筒在挤出机的出口处回收新鲜荨麻提取物。在澄清后,获得荨麻提取物,其相对于所用溶剂的产率为162.6%,相对于植物进料的产率为85%。
然后用pH 3的适量硫酸酸化获得的两种提取物,并在水中对其稀释6倍,以便获得1.4%的庚基葡萄糖苷终浓度。出现浑浊,然后在3500tr/min下离心20秒后收集残余物。
在附图1中的薄层色谱分析表明,在这两种提取物中存在极性脂质如半乳糖脂类和甾醇类,这些条带并未显示出通过在相同条件(挤出,干燥/新鲜的植物,植物和溶剂进料速率)下仅使用水挤出所获得的提取物。MGDG表示单-半乳糖苷基二酰基甘油和DGDG表示二-半乳糖苷基二酰基甘油。
实施例4:胶囊
如在实施例1中的香桃木提取物: 200mg
淀粉: 45mg
硬脂酸镁: 2mg
实施例5:霜剂
Claims (18)
1.一种用于获得植物性基质的提取物的方法,特别是植物基质的提取物的方法,其特征在于,与热处理联合或未联合地,在水溶液存在下,植物性基质经受机械处理,所述机械处理在于在挤出机中挤出植物性基质,所述水溶液含有至少一种助溶剂,特别地,所述助溶剂的浓度至少等于其最小助溶浓度,随后进行回收提取物的操作。
2.根据权利要求1所述的方法,其特征在于,助溶剂为离子型,特别地选自正丁基苯磺酸钠、枯烯磺酸钠、对甲苯磺酸钠或二甲苯磺酸钠。
3.根据权利要求1所述的方法,其特征在于,助溶剂为非离子型,优选为农业来源的,特别地为通式Alk-O-Zp的烷基-(多)糖苷,其中:
·Alk表示具有3至7个碳原子的、饱和或不饱和的、直链或支链疏水性脂肪族烃片段;以及
·Z为亲水性糖苷基团,例如葡萄糖、木糖和阿拉伯糖;以及
·1<p<5。
4.根据权利要求1至3中任一项所述的方法,其特征在于,所述热处理在20℃至200℃,优选60℃至120℃的温度进行。
5.根据权利要求1至4中任一项所述的方法,其特征在于,在助溶剂的水溶液存在下经受热机械处理的植物,由完整的、经粉碎的或经研磨的干燥植物或新鲜植物的地上部分和/或地下部分的全部或部分构成。
6.根据权利要求5所述的方法,其特征在于,植物部分表示为地上部分,例如茎、枝、叶子、果实、种子和/或花;和/或地下部分,例如根茎、根和/或球茎。
7.根据权利要求1至6中任一项所述的方法,其特征在于,在助溶剂的水溶液存在下经受热机械处理的干燥或新鲜的植物选自灯笼草Physalis peruviana的果实、白花酸藤果Embelia ribes的果实、香桃木Myrtus communis的叶子、蓝桉树Eucalyptus globulus的叶子、山竹Garcinia mangostana的果皮、啤酒花Humulus lupulus的雌花序、金鸡钠树属物种Cinchona sp.的树皮、大荨麻Urtica dioica的地上部分、蜡菊属物种Helichrysum spp.的地上部分、香荚兰属物种Vanilla spp.的果实、生姜Zingiber officinale的根茎、姜黄属物种Curcuma spp.的根茎、卡瓦胡椒Piper methysticum的根茎、胡椒属物种Piper spp.的叶子、油橄榄Olea europaea的果实和叶子。
8.根据前述权利要求中任一项所述的方法,其特征在于,在挤出前对植物进行预处理,通过超声、微波、酶消化、在助溶溶液中的浸渍、植物的制备如低温研磨、粉碎、研磨进行处理,特别是通过在助溶溶液中的浸渍进行处理。
9.根据前述权利要求中任一项所述的方法,其特征在于,使回收的提取物经受澄清和/或过滤的后续步骤。
10.根据权利要求1至8中任一项所述的方法,其特征在于,将回收的提取物稀释、浓缩、干燥或者通过添加合适的防腐剂来按原样储存。
11.根据权利要求1至8中任一项所述的方法,其特征在于,将回收的提取物用足够量的水稀释,以回收富含亲脂性化合物的干燥提取物。
12.根据前述权利要求中任一项所述的方法,其特征在于,在双螺杆挤出机中进行挤出。
13.根据权利要求12所述的方法,其特征在于,双螺杆挤出机包括具有同向旋转和同向穿透的双螺杆的第一区,在该处进行所述植物的研碎。
14.根据权利要求12或13所述的方法,其特征在于,双螺杆挤出机包括第二双螺杆区,在该处进行固/液分离。
15.根据权利要求1至14中任一项所述的方法,其特征在于,所述挤出机包括至少一个机筒,并且优选地数个连续的相邻的机筒。
16.食品、化妆品和/或药物组合物,其含有通过实施如权利要求1至15中任一项所述的方法获得的总植物性基质提取物或具有浓缩的亲脂性化合物。
17.根据权利要求16所述的组合物,其特征在于,所述组合物被制备成适合于局部施用的形式。
18.根据权利要求16所述的组合物,其特征在于,所述组合物被制备成适合于口服施用的形式。
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CN116898885A (zh) * | 2023-07-25 | 2023-10-20 | 中国科学院西北高原生物研究所 | 一种用于抑制covid-19 xbb 1.5变异株感染的水浸提活性物及其应用 |
CN116898885B (zh) * | 2023-07-25 | 2024-04-16 | 中国科学院西北高原生物研究所 | 一种用于抑制covid-19 xbb 1.5变异株感染的水浸提活性物及其应用 |
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Publication number | Publication date |
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BR112017019469B1 (pt) | 2021-04-06 |
KR102626151B1 (ko) | 2024-01-16 |
FR3033682A1 (fr) | 2016-09-23 |
EP3270887B1 (fr) | 2020-10-21 |
CA2979611A1 (fr) | 2016-09-22 |
EP3270887A1 (fr) | 2018-01-24 |
ES2843976T3 (es) | 2021-07-21 |
CA2979611C (fr) | 2023-10-17 |
PT3270887T (pt) | 2021-01-22 |
CN107405296B (zh) | 2020-10-02 |
FR3033682B1 (fr) | 2018-04-06 |
US20180055900A1 (en) | 2018-03-01 |
US10532078B2 (en) | 2020-01-14 |
JP2018516157A (ja) | 2018-06-21 |
WO2016146838A1 (fr) | 2016-09-22 |
BR112017019469A2 (pt) | 2018-05-15 |
KR20170129133A (ko) | 2017-11-24 |
JP6755880B2 (ja) | 2020-09-16 |
HK1245141A1 (zh) | 2018-08-24 |
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