CN102724887A - 固/液萃取 - Google Patents
固/液萃取 Download PDFInfo
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- CN102724887A CN102724887A CN2011800071961A CN201180007196A CN102724887A CN 102724887 A CN102724887 A CN 102724887A CN 2011800071961 A CN2011800071961 A CN 2011800071961A CN 201180007196 A CN201180007196 A CN 201180007196A CN 102724887 A CN102724887 A CN 102724887A
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- solvent
- oil
- unsaponifiable matter
- butter
- composition
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- NUMQCACRALPSHD-UHFFFAOYSA-N tert-butyl ethyl ether Chemical compound CCOC(C)(C)C NUMQCACRALPSHD-UHFFFAOYSA-N 0.000 claims abstract description 84
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- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims abstract description 44
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims abstract description 41
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 claims abstract description 32
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- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 14
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 claims abstract description 14
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Classifications
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Abstract
本发明涉及在至少一种固体植物物质或微生物中含有的油或黄油(特别是具有高含量不皂化物的油或黄油)的固/液萃取的方法。所述方法至少包括下列步骤:使用第一溶剂系统的至少一种固体植物物质或微生物的固/液萃取,所述第一溶剂系统包含浓度表示为相对于所述溶剂系统总体积的至少50体积%的溶剂,所述溶剂选自氟代芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)及其混合物;和,任选地,包含油或黄油(特别是富含不皂化物)的部分的回收。本发明还涉及使用此方法获得的不皂化物部分、油或黄油,并且涉及含有所述油或黄油的组合物。
Description
技术领域
本发明涉及来自于固体植物物质或微生物的油或黄油的固/液萃取的方法;特别地,所述油或所述黄油包含高含量不皂化物。
背景技术
脂肪的不皂化物或不皂化物部分(fraction)由化合物组成,所述化合物形成脂肪的一部分,所述部分在碱的持续作用之后仍然不溶于水并且能够采用有机溶剂萃取。
大多数植物油不皂化物包括物质的主要类别。这些主要类别包括饱和的或不饱和的烃、脂肪醇或萜烯醇、甾醇、生育酚、类胡萝卜素色素、叶黄素,以及在一些油的情况下的一种或两种具体的类别。
从植物油中获得不皂化物的通常方法旨在萃取其中含有的全部或部分所述主要类别,适合于制备部分的或全部的不皂化物部分。
特别地,为了其药学、化妆品和营养学属性,研究部分的或全部的不皂化物部分。
从植物油中获得不皂化物的通常方法尤其包括脂肪的皂化步骤和采用有机溶剂萃取目标产物(所述不皂化物)。
从固体植物物质中萃取油(特别是富含不皂化物的那些油)的最常用的溶剂是脂肪族溶剂,特别是己烷。
特别地,己烷涉及具有毒性的缺点;特别地,其在EU1(法语缩写为UE1)CMR列表中或者在EU2(法语缩写为UE2)CMR列表中被分类为3级CMR。
由于己烷的理化属性,特别是其闪点(-23.3℃)和/或其自燃温度(233.9℃),其进一步具有操作危险的缺点。
最后,考虑到相对于所述油和/或相对于获得的所述油的所述不皂化物的收率、选择性、简易性、成本、毒性、便利性、步骤数目(特别是萃取)和/或迅速性,涉及这些常规脂肪族溶剂(特别是己烷)的方法可能不令人满意。
发明内容
因此,本发明的目的在于解决上述全部或部分问题。特别地,本发明的目的在于提供一种更经济、更直接、更环境友好的方法,所述方法需要更少量的有机溶剂,更容易实施,更迅速,产生更少的毒性条件,适合于获得油(特别是具有高含量不皂化物的油)。考虑到收率和/或选择性,所述方法至少比得上现有方法或者优于现有方法。
特别地,令人渴望的是所涉及的溶剂毒性更小,尤其是未被分类为CMR物质(尤其是EU2 CMR列表物质),和/或适合于萃取油,且收率和/或选择性至少比得上使用常规脂肪族溶剂(特别是己烷)获得的收率和选择性。
所谓的“被分类为CMR物质”的溶剂可以是在2009年1月15日的2009/2/CE指令的附件中的列表中包括的那些溶剂,特别地,可以从http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2009:011:0006:0082:FR:PDF的地址中获得,该第一列表在下文中指的是“EU1 CMR列表”;在2009年第31次ATP中的致癌、致突变、有毒的化学品欧洲管理分类(la Classification européenne réglementaire des produitschimiques cancérogènes,mutagènes et toxiques pour la reproduction-31eATP,2009)中列出的那些溶剂,特别地,可以从http://www.prc.cnrs-gif.fr/en_telechargement/cmr31.pdf的地址中获得,该第二列表在下文中指的是“EU2 CMR列表”;和/或在与“2005年加利福尼亚化妆品安全法案(California Safe Cosmetics Act of2005)”相关的,由“加利福尼亚公共卫生部门,职业卫生分支机构,加利福尼亚安全化妆品项目(California department of public health,occupational healthbranch,California safe cosmetic program)”起草的,日期为2009年12月1日的“已知或疑似引起癌症或生殖毒性的化学品(Chemicals knownor suspected to cause cancer or reproductive toxicity)”的列表中列出的那些溶剂,该第三列表在下文中指的是“US CMR列表”。
文中使用的表述EU CMR列表指的是EU1 CMR列表和EU2 CMR列表,特别是EU2 CMR列表。
因此,本发明涉及一种在至少一种固体植物物质或微生物中含有的油或黄油(特别是具有高含量不皂化物的油或黄油)的固/液萃取的方法,所述方法包括下列步骤:
-使用第一溶剂系统的至少一种固体植物物质或微生物的固/液萃取,所述第一溶剂系统包含浓度表示为相对于所述溶剂系统总体积的至少50体积%的溶剂,所述溶剂选自氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)及其混合物。
-任选地,包含油或黄油(特别是富含不皂化物的油或黄油)的部分的回收。
这些不同溶剂的CAS号如下,BTF:98-08-8;BHF:392-56-3;ETBE:37-92-3;MTBE:1634-04-4;HMDS:107-46-0;TMS:75-76-3;和MeTHF:96-47-9。
根据本发明,术语“高含量不皂化物”是指所述油或黄油包括至少1重量%,尤其是至少2重量%,特别是至少3重量%的最初存在于所述固体物质中的不皂化的化合物。
所述第一溶剂系统可以包括浓度表示为相对于所述第一溶剂系统总体积的至少60体积%,尤其是至少75体积%,特别是至少90体积%,更特别是至少95体积%,甚至更特别是至少99体积%的溶剂,所述溶剂选自氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)及其混合物。
特别地,所述第一溶剂系统由氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)或其混合物组成。
所述第一溶剂系统可以包括浓度表示为相对于所述第一溶剂系统总体积的至少50体积%,尤其是至少75体积%,特别是至少90体积%,更特别是至少95体积%,甚至更特别是至少99体积%的溶剂,所述溶剂选自氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)及其混合物。
根据一个可选的实施方案,所述第一溶剂系统由溶剂组成,所述溶剂选自氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)。
本发明还涉及一种获得特别地全部或部分不皂化物部分的方法,所述方法包括下列步骤:
-使用第一溶剂系统的至少一种固体植物物质或微生物的固/液萃取,所述第一溶剂系统包含浓度表示为相对于所述溶剂系统总体积的至少50体积%的溶剂,所述溶剂选自氟化芳香族溶剂(特别是三氟甲苯(BTF)和六氟苯(BHF))、叔丁基醚(特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE))、包含至少一个硅原子的溶剂(特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS))、甲基四氢呋喃(MeTHF)及其混合物,
-任选地,富含油或黄油的有机溶剂的回收,或者油或黄油的回收,特别地,所述油或黄油富含不皂化物,
-特别地,借助于选自皂化和酯化的步骤,将所述油或黄油转化为水醇溶液,
-水醇溶液的萃取,其中借助于液/液萃取或蒸馏,将脂肪部分从不皂化物部分中分离,和
-特别地部分或全部不皂化物部分的回收。
根据本发明,术语“全部部分(fraction totale)”是指该部分包括在考虑中的植物油或黄油中或者微生物中含有的所述不皂化物的全部物质组成类别。
根据本发明,术语“部分部分(fraction partielle)”是指该部分包括在考虑中的植物油或黄油中或者微生物中含有的所述不皂化物的至少一种物质组成类别。
第一溶剂系统被定义为用于油或黄油的固/液萃取的方法。
在常规溶剂系统中,所述油或黄油可以被转化为水醇溶液。
根据一个特别的可选的实施方案,在第二溶剂中将所述油或黄油转化为水醇溶液,所述第二溶剂包含至少一种所述第一溶剂系统的溶剂或者由至少一种所述第一溶剂系统的溶剂组成,特别是甲基四氢呋喃(MeTHF)。
更特别地,无需所述油或黄油的全部纯化即可进行所述转化。特别地,在富含油或黄油的有机溶剂的基础(base)上直接进行所述转化,特别地包含相对于所述富含油或黄油的有机溶剂的总重量的至少2重量%,特别是至少5重量%,或者至少10重量%的油。
根据第一可选的实施方案,在特别地部分蒸发的部分上进行所述转化,向其中加入至少50重量%的其他溶剂,或者不加入其他溶剂。
根据另一个可选的实施方案,可以向富含油的,特别地蒸发的有机溶液中加入至少10%的至少一种其他溶剂,如C2至C4醇(特别是乙醇、正丙醇、异丙醇、丁醇,特别是正丁醇)、甲基四氢呋喃(MeTHF)及其混合物。
有利地,所述第一和第二溶剂系统包含甲基四氢呋喃(MeTHF)。在该情况下,例如考虑收率、毒性(非CMR溶剂)和选择性,所述方法可以具有相对于常规方法被增强的优势。
如果使用液/液萃取执行水醇溶液的萃取,那么采用第三溶剂系统,特别是采用与在所述第一和/或所述第二溶剂系统中使用的那些溶剂相同的一些溶剂,可以进行所述液/液萃取,所述第三溶剂系统以与所述第一溶剂系统相同的方式被定义。
在后者的情况下,所述方法在经济和时间方面具有优势,因为其特别地涉及更容易的溶剂采购和/或质量控制管理。
一般情况下,所述方法可以是更经济的、更直接的、更环境友好的,因为其需要更少量的有机溶剂,更容易实施,更迅速,产生更少的毒性条件,适合于获得油(特别是具有高含量不皂化物的油),并且考虑到收率和/或选择性,所述方法至少比得上现有方法或者优于现有方法。
特别地,根据FR 1 246 633中描述的程序可以进行皂化和萃取部分。
本方法中使用的所述固体植物物质或微生物可以获得自大豆、油菜籽、玉米、向日葵、芝麻、羽扇豆、棉花、椰子、橄榄、鳄梨、可可、印度赤铁树、乳木果、棕榈仁、花生、干椰肉、亚麻籽、蓖麻、葡萄籽、葫芦籽、黑醋栗籽、甜瓜籽、番茄籽、南瓜籽、杏仁、榛子、核桃、月见草、琉璃苣、红花、亚麻荠、罂粟籽、巨藻类、微藻类,如红球藻(Haematocococcus)、杜氏藻(Dunaliella)、螺旋藻(Spirulina)、小球藻(Chorella),和/或微生物,尤其是来自于海洋、淡水或陆地来源的微生物,特别是酵母菌、霉菌并且更特别的是细菌,及其混合物。
典型地,鳄梨油中获得的不皂化物部分的含量范围是从2%至10%,椰油中大约是0.5%,大豆油中大约是1%并且橄榄油中大约是1%。
本领域技术人员将会知道被实施以便于从植物油或黄油或者微生物中萃取所述不皂化物部分的方法,并且将会知道如何应用所述方法以便于转化、萃取和/或回收部分根据本发明的所述不皂化物。
特别地,涉及该部分的现有技术包括Laboratoires Pharmascience所有的专利FR 2 678 632中描述的和要求保护的用于制备鳄梨油不皂化物的方法。与用于制备鳄梨油不皂化物的常规方法相比,该方法适合于获得富含呋喃部分的鳄梨油不皂化物,也被称为部分H。
像这样,如专利FR 2 678 632中所描述,在油的萃取和皂化之前,可以从预先热处理的水果制备鳄梨油不皂化物。
该热处理由水果的受控干燥组成,所述水果优选是新鲜的,所述热处理在优选至少大约80℃并且优选介于大约80℃和大约120℃之间的温度下进行至少4个小时,有利地至少10个小时,优选介于大约24和大约48个小时之间。
用于制备从大豆油不皂化物浓缩物中获得的大豆油不皂化物的方法也可以被引用。
所述不皂化物浓缩物可以根据专利申请FR 2 762 512所描述的用于羽扇豆油,但是适合于大豆油的方法,借助于分子蒸馏来制备。
在该方法中,所述大豆油在离心式或刮膜式分子蒸馏器中被蒸馏,所述蒸馏在介于大约210℃和250℃之间的温度下进行并且经历介于0.01和0.001毫米汞柱(即0.13至1.3Pa)之间的高度真空。
获得的蒸馏物具有含量介于5重量%和40重量%之间的不皂化物,因此是大豆油不皂化物浓缩物。
然后在极性介质(特别是醇性介质,优选乙醇、正丙醇、异丙醇、丁醇(特别是正丁醇),甲基四氢呋喃(MeTHF),或其混合物)中采用碱(如草木灰或氢氧化钠)将所述浓缩物皂化,然后使用所述第一溶剂系统使其经历一次或多次萃取。
然后,优选将获得的萃取溶液离心、过滤并采用水洗涤以便于除去残留的痕量碱。
将萃取溶剂小心地蒸发以便于回收所述不皂化物。最后,在其皂化之前,通过分离被回收至浓缩物中的所述不皂化物的主要成分,可以使所述油或黄油富含不皂化物。可以使用各种方法:冷结晶、液/液萃取或分子蒸馏。
在先的所述油或黄油的不皂化物浓缩使其有可能减少待皂化的油或黄油的体积。
分子蒸馏是特别优选的,优选在介于大约180℃和大约230℃之间的温度下进行,维持压力介于10-3和10-2mm Hg之间,并且优选在10-3mm Hg的区域内。
蒸馏物中的不皂化物的浓度相对于总重量可以高达60重量%。
最特别地,本发明涉及一种如本说明书所描述的方法,其中获得的所述不皂化物选自大豆不皂化物、鳄梨不皂化物,特别是富含呋喃部分的鳄梨不皂化物和/或富含甾醇部分的鳄梨不皂化物,并且更特别是鳄梨和大豆不皂化物的混合物(ASU)。
根据本发明,术语“富含部分X的不皂化物”是指所述不皂化物中部分X的含量增加,特别是增加了至少10重量%,尤其是至少50重量%,更特别是至少80重量%。
本发明还涉及不含(dépourvu de)在EU1 CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂的油或黄油,特别地使用根据本发明的方法获得所述油或黄油。
本发明还涉及不含在EU1 CMR列表、EU2 CMR列表和/或USCMR列表中被分类的溶剂的特别地部分或全部不皂化物部分,特别地使用根据本发明的萃取方法获得所述部分。
本发明还涉及所述黄油或油的所述部分在制备组合物,特别是药物组合物、营养组合物和/或化妆品组合物,或者营养补充品中的用途。
本发明还涉及一种组合物,特别是药物组合物、营养组合物或化妆品组合物,或者营养补充品,其包含至少一种植物的油或黄油或者微生物的至少一种油、黄油或不皂化物部分,所述油、黄油或部分不含在EU1 CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂和/或所述油、黄油或部分适合于使用根据本发明的方法而获得,或者使用根据本发明的方法直接获得,并且所述组合物任选地包含赋形剂,特别是化妆品上、营养学上或药学上可接受的赋形剂。
根据一个特别的实施方案,本发明涉及一种组合物,特别是药物组合物、营养组合物和/或化妆品组合物,或者营养补充品,其包含适合于使用根据本发明的方法获得的或者直接获得的至少一种不皂化物,特别是大豆不皂化物、鳄梨不皂化物,更特别是富含呋喃部分的鳄梨不皂化物和/或富含甾醇部分的鳄梨不皂化物,甚至更特别是鳄梨和大豆不皂化物的混合物(ASU)。
所述药物组合物可以旨在预防和/或治疗结缔组织障碍,特别是关节病、牙周病和/或皮肤老化。
所述营养组合物或营养补充剂可以旨在预防和/或治疗结缔组织障碍,特别是关节病、牙周病和/或皮肤老化和/或皮肤炎症。
所述化妆品组合物可以旨在预防和/或治疗表皮的、真皮的和/或皮下的皮肤障碍。
根据本发明,术语“不含在EU1 CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂”是指在EU1 CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂的总含量低于10ppm,尤其是低于5ppm,特别是低于2ppm或者低于1ppm。
本发明还涉及一种化妆品治疗方法,因此可以将根据本发明的化妆品组合物局部地应用,并且本发明还涉及根据本发明获得的植物油或黄油或者微生物的油、黄油或不皂化物在制备医用产品中的用途,特别地,所述医用产品旨在治疗和预防结缔组织障碍,特别是关节病。
显而易见的是,本说明书中描述的各种特征可以被结合在一起。
进行下列实验作为解释本发明的实施例。
具体实施方式
在所有实施例中,进行使用己烷的参照(référence)测试。
实施例1:从干燥的鳄梨中的萃取
采用己烷(参照)和下列溶剂:HMDS、MeTHF、BTF、BHF、MTBE、ETBE进行从干燥的鳄梨中的萃取。
将干燥的鳄梨粉碎并加入到纤维素圆柱筒(cartouche)中(30至40g)。在索氏提取器(BUCHI B-811)中进行萃取。然后平行进行四组萃取,并且每一组萃取由20个萃取/虹吸循环组成。一旦所述萃取已经终结,就将萃取溶剂蒸发并且将已经从中除去溶剂的残留物称重。然后比较重量收率。结果在表1中给出。
表1
该结果说明:根据本发明的溶剂具有与己烷相当的萃取能力。
相对于己烷而言,使用根据本发明的溶剂得到的萃取油中不皂化物的含量较高;在ETBE和MeTHF的情况下,所述含量增加了50%。
实施例2:从冻干的鳄梨果肉粉中的萃取
根据实施例1中所描述的方法,采用己烷(参照)和下列溶剂:HMDS、MeTHF、BTF、MTBE、ETBE萃取冻干的鳄梨果肉粉。结果在表2中给出。
表2
该结果说明:根据本发明的溶剂具有与己烷相当的萃取能力。
相对于己烷而言,使用根据本发明的溶剂得到的萃取油中不皂化物的含量较高;在MeTHF的情况下,所述含量增加了50%。
实施例3:从干燥的鳄梨中的油的萃取
采用己烷(参照)和下列溶剂:BTF和ETBE进行从干燥的鳄梨中的萃取。
将干燥的鳄梨粉碎并加入到纤维素圆柱筒中(30至40g)。在索氏提取器(BUCHI B-811)中进行萃取。然后平行进行四组萃取,第一组萃取由5个萃取循环组成,第二组萃取由10个循环组成,第三组萃取由15个循环组成,并且第四组萃取由20个循环组成。一旦所述萃取已经终结,就将萃取溶剂蒸发并且将已经从中除去溶剂的残留物称重。然后比较重量收率。
结果在下列表3中给出。
表3
采用ETBE获得的重量收率类似于采用己烷参照获得的重量收率:因此,ETBE提供了在固/液萃取方法中己烷使用的替代物。
BTF的萃取能力适合于仅以5个萃取循环即可获得与采用己烷或ETBE以20个萃取循环获得的收率相同的收率。因此,BTF提供了令人满意的己烷使用的替代物,其适合于显著减少所涉及的溶剂的量和/或接触时间。
实施例4:从干燥的小球藻中的萃取
根据实施例1中所描述的方法,采用己烷(参照)和下列溶剂:BTF和MTBE进行从干燥的小球藻粉中的萃取。结果在表4中给出。
表4
该结果说明:根据本发明的溶剂具有与己烷相当的萃取能力。
相对于己烷而言,使用根据本发明的溶剂得到的萃取油中不皂化物的含量较高。
Claims (19)
1.一种在至少一种固体植物物质或微生物中含有的油或黄油,特别是具有高含量不皂化物的油或黄油的固/液萃取的方法,所述方法至少包括下列步骤:
-使用第一溶剂系统的至少一种固体植物物质或微生物的固/液萃取,所述第一溶剂系统包含浓度为相对于所述溶剂系统总体积的至少50体积%的溶剂,所述溶剂选自氟化芳香族溶剂,特别是三氟甲苯(BTF)和六氟苯(BHF);叔丁基醚,特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE);包含至少一个硅原子的溶剂,特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS);甲基四氢呋喃(MeTHF)及其混合物,
-任选地,包含油或黄油的部分的回收。
2.一种获得特别地全部或部分不皂化物部分的方法,所述方法包括下列步骤:
-使用第一溶剂系统的至少一种固体植物物质或微生物的固/液萃取,所述第一溶剂系统包含浓度为相对于所述溶剂系统总体积的至少50体积%的溶剂,所述溶剂选自氟化芳香族溶剂,特别是三氟甲苯(BTF)和六氟苯(BHF);叔丁基醚,特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE);包含至少一个硅原子的溶剂,特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS);甲基四氢呋喃(MeTHF)及其混合物,
-任选地,富含油或黄油的有机溶剂的回收,或者油或黄油的回收,
-特别地,借助于选自皂化和酯化的步骤,将所述油或黄油转化为水醇溶液,
-水醇溶液的萃取,其中借助于液/液萃取,将脂肪部分从不皂化物部分中分离,和
-不皂化物部分的回收。
3.根据权利要求1或2所述的方法,其特征在于所述第一溶剂系统包括浓度表示为相对于所述第一溶剂系统总体积的至少60体积%,尤其是至少75体积%,特别是至少90体积%,更特别是至少95体积%,甚至更特别是至少99体积%的溶剂,所述溶剂选自氟化芳香族溶剂,特别是三氟甲苯(BTF)和六氟苯(BHF);叔丁基醚,特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE);包含至少一个硅原子的溶剂,特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS);甲基四氢呋喃(MeTHF)及其混合物。
4.根据权利要求1至3中任一项所述的方法,其特征在于所述第一溶剂系统由2-甲氧基-2-甲基丙烷(MTBE)、2-乙氧基-2-甲基丙烷(ETBE)、甲基四氢呋喃(MeTHF)、三氟甲苯(BTF)、六氟苯(BHF)、六甲基二硅氧烷(HMDS)、四甲基硅烷(TMS)或其混合物组成。
5.根据权利要求1至4中任一项所述的方法,其特征在于所述第一溶剂系统包括浓度为相对于所述第一溶剂系统总体积的至少50体积%,尤其是至少75体积%,特别是至少90体积%,更特别是至少95体积%,甚至更特别是至少99体积%的溶剂,所述溶剂选自氟化芳香族溶剂,特别是三氟甲苯(BTF)和六氟苯(BHF);叔丁基醚,特别是2-乙氧基-2-甲基丙烷,也被称为乙基叔丁基醚(ETBE),和2-甲氧基-2-甲基丙烷或甲基叔丁基醚(MTBE);包含至少一个硅原子的溶剂,特别是六甲基二硅氧烷(HMDS)和四甲基硅烷(TMS);甲基四氢呋喃(MeTHF)及其混合物。
6.根据权利要求2至5中任一项所述的方法,其特征在于在第二溶剂中将所述油转化为水醇溶液,所述第二溶剂包含至少一种所述第一溶剂系统的溶剂或者由至少一种所述第一溶剂系统的溶剂组成,特别是甲基四氢呋喃(MeTHF)。
7.根据权利要求2至6中任一项所述的方法,其特征在于在富含油或黄油的有机溶剂的基础上直接进行所述转化,特别地所述有机溶剂包含相对于所述富含油或黄油的有机溶剂的总重量的至少2重量%,特别是至少5重量%,或者至少10重量%的油。
8.根据权利要求7所述的方法,其特征在于在特别地部分蒸发的部分上进行所述转化,向其中加入至少50重量%的其他溶剂,或者不加入其他溶剂。
9.根据权利要求7所述的方法,其特征在于可以向富含油的,特别地蒸发的部分中加入至少10%的至少一种其他溶剂,如C2至C4醇,特别是乙醇、异丙醇、丁醇,特别是正丁醇;甲基四氢呋喃(MeTHF)及其混合物。
10.根据权利要求6至9中任一项所述的方法,其特征在于所述第一和第二溶剂系统包含甲基四氢呋喃(MeTHF)。
11.根据权利要求1至10中任一项所述的方法,其特征在于使用液/液萃取执行水醇溶液的萃取,采用第三溶剂系统进行所述液/液萃取,所述第三溶剂系统包括在所述第一和/或所述第二溶剂系统中使用的全部或一些相同溶剂。
12.根据权利要求1至11中任一项所述的方法,其特征在于所述固体植物物质或微生物获得自大豆、油菜籽、玉米、向日葵、芝麻、羽扇豆、棉花、椰子、橄榄、鳄梨、可可、印度赤铁树、乳木果、棕榈仁、花生、干椰肉、亚麻籽、蓖麻、葡萄籽、葫芦籽、黑醋栗籽、甜瓜籽、番茄籽、南瓜籽、杏仁、榛子、核桃、月见草、琉璃苣、红花、亚麻荠、罂粟籽、巨藻类、微藻类,如红球藻、杜氏藻、螺旋藻、小球藻,和/或微生物,尤其是来自于海洋、淡水或陆地来源的微生物,特别是酵母菌、霉菌并且更特别的是细菌,及其混合物。
13.根据权利要求1至12中任一项所述的方法,其特征在于获得的所述不皂化物选自大豆不皂化物、鳄梨不皂化物,特别是富含呋喃部分的鳄梨不皂化物和/或富含甾醇部分的鳄梨不皂化物,并且更特别是鳄梨和大豆不皂化物的混合物(ASU)。
14.一种不含在EU1 CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂的油或不皂化物部分,所述部分适合于根据权利要求1至13中任一项而获得,特别地使用根据权利要求1至13中任一项所述的萃取方法获得所述油或部分。
15.一种组合物,特别是药物组合物、营养组合物或化妆品组合物,或者营养补充品,其包含至少一种植物的油或黄油或者微生物的至少一种油、黄油或不皂化物部分,所述油、黄油或部分不含在EU1CMR列表、EU2 CMR列表和/或US CMR列表中被分类的溶剂,或者所述油、黄油或部分适合于使用根据权利要求1至13中任一项所述的方法而获得,并且所述组合物任选地包含赋形剂,特别是化妆品上、营养学上或药学上可接受的赋形剂。
16.一种组合物,特别是药物组合物、营养组合物或化妆品组合物,或者营养补充品,其包含适合于使用根据权利要求1至13中任一项所述的方法获得的或者直接获得的至少一种不皂化物,特别是大豆不皂化物、鳄梨不皂化物,更特别是富含呋喃部分的鳄梨不皂化物和/或富含甾醇部分的鳄梨不皂化物,甚至更特别是鳄梨和大豆不皂化物的混合物(ASU)。
17.根据权利要求15或16所定义的药物组合物,其特征在于所述药物组合物旨在预防和/或治疗结缔组织障碍,特别是关节病、牙周病和/或皮肤老化。
18.根据权利要求15或16所定义的营养组合物或营养补充品,其特征在于所述营养组合物或营养补充品旨在预防和/或治疗结缔组织障碍,特别是关节病、牙周病、皮肤老化和/或皮肤炎症。
19.根据权利要求15或16所定义的化妆品组合物,其特征在于所述化妆品组合物旨在预防和/或治疗表皮的、真皮的和/或皮下的皮肤障碍。
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- 2011-01-31 BR BR112012018900-0A patent/BR112012018900B1/pt active IP Right Grant
- 2011-01-31 ES ES11701288T patent/ES2769627T3/es active Active
- 2011-01-31 CN CN201610034758.6A patent/CN105647640A/zh active Pending
- 2011-01-31 RS RS20200131A patent/RS59903B1/sr unknown
- 2011-01-31 PL PL11701288T patent/PL2528458T3/pl unknown
- 2011-01-31 CN CN2011800071961A patent/CN102724887A/zh active Pending
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2019
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US6146616A (en) * | 1997-04-24 | 2000-11-14 | Laboratories Pharmascience | Antioxidant and/or antielastase composition based on lupine oil |
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CN109022141A (zh) * | 2018-09-30 | 2018-12-18 | 海南煊烨生物科技有限公司 | 一种提取微生物油脂的方法 |
Also Published As
Publication number | Publication date |
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FR2955783B1 (fr) | 2014-02-07 |
CN105647640A (zh) | 2016-06-08 |
DK2528458T3 (da) | 2020-02-17 |
KR102025056B1 (ko) | 2019-09-25 |
EP3613412A1 (fr) | 2020-02-26 |
US10493303B2 (en) | 2019-12-03 |
HRP20200208T1 (hr) | 2020-05-15 |
JP5992336B2 (ja) | 2016-09-14 |
PL2528458T3 (pl) | 2020-05-18 |
EP2528458B1 (fr) | 2019-11-27 |
PT2528458T (pt) | 2020-02-21 |
SI2528458T1 (sl) | 2020-04-30 |
US20200069978A1 (en) | 2020-03-05 |
JP2017014485A (ja) | 2017-01-19 |
LT2528458T (lt) | 2020-02-25 |
JP2013518165A (ja) | 2013-05-20 |
WO2011092334A3 (fr) | 2012-03-01 |
RS59903B1 (sr) | 2020-03-31 |
KR20120123390A (ko) | 2012-11-08 |
KR20190033664A (ko) | 2019-03-29 |
FR2955782A1 (fr) | 2011-08-05 |
ES2769627T3 (es) | 2020-06-26 |
JP6541040B2 (ja) | 2019-07-10 |
US20120294887A1 (en) | 2012-11-22 |
HUE047899T2 (hu) | 2020-05-28 |
CY1122706T1 (el) | 2021-03-12 |
FR2955783A1 (fr) | 2011-08-05 |
BR112012018900A2 (pt) | 2015-09-01 |
WO2011092334A2 (fr) | 2011-08-04 |
BR112012018900B1 (pt) | 2020-12-01 |
EP2528458A2 (fr) | 2012-12-05 |
FR2955782B1 (fr) | 2014-02-14 |
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