CN101622043A - 高能超声提取 - Google Patents
高能超声提取 Download PDFInfo
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- CN101622043A CN101622043A CN200780051211A CN200780051211A CN101622043A CN 101622043 A CN101622043 A CN 101622043A CN 200780051211 A CN200780051211 A CN 200780051211A CN 200780051211 A CN200780051211 A CN 200780051211A CN 101622043 A CN101622043 A CN 101622043A
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Abstract
本发明描述了一种从固体材料中水提法提取化合物的方法和装置,其中所述固体材料被夹带在提取液相中,所述提取液相在发出径向的或聚焦的高能超声波的浸没的超声焊极周围流动。观测到提取物明显增加且提取时间明显缩短。
Description
技术领域
本发明涉及通过使用优选地被浸没的超声焊极(sonotrode)对改进材料中重要化学成分的液相提取。
背景技术
木桶作为液体和食物的常用容器长期以来占有重要地位。然而,随着材料处理方法和其他在当今条件下更实用的结构材料的发展,除了用来进行葡萄酒和烈酒的陈酿外,木桶几乎被完全替代。
橡木桶中储藏的葡萄酒和烈酒具有理想诱人的感官特性、组成和感官品质。因此,许多精酿的餐饮红酒和白酒的生产都会使用橡木桶。全世界用来进行酒陈酿的木桶大多具有190至500升的容积。对于餐饮酒而言,约225升的容积最为常见。
橡木含有纤维素、半纤维素、鞣质和木质素,后三者在酒与橡木接触的过程中对酒有影响。半纤维素(无气味)的影响是间接的——加热桶板会使其发生化学转化,由此使其成为其他有气味的化合物的来源。木材释放出的鞣质(不挥发)由鞣花酸和没食子酸的聚合物构成,并且可以水解。经桶储藏后酒中鞣质的量最高可达100mg/L。可溶性的木质素部分被降解为芳香醛,所述芳香醛可通过氧化作用形成相应的酚酸。新的橡木桶的贡献主要在于提对木材组成中的挥发性酚类(鉴定出了200种以上)级分。
通过简单扩散进入酒中的重要化合物为具有椰子样气味(对感官刺激最重要的气味)的顺式-b-甲基辛内酯(octalactoned)和反式-b-甲基辛内酯(橡木内酯可通过糠醛改造成具有焦糖味);醛(特别是香草醛);提升香草醛气味的酚酮(phenolics ketones);其他挥发性酚酮;挥发性酚,例如丁香酚(辛辣、丁香和石竹味);愈创木酚及其衍生物(烟味和药味);烘烤产生的呋喃衍生物和许多其他化合物;以及降异戊二烯类(nor-isoprenoid)(约30种,包括B-紫罗兰酮)。
烘烤能增加(i)酒中愈创木酚(烟味和药味)、4-甲基愈创木酚(烟味和丁香样气味)、香草醛(香草气味)、丁香醛、松柏醛(coniferaldehyde)、芥子醛(sinapaldehyde)和橡木内酯(木材气味和椰子样气味)的量,和(ii)促使橡木中多糖(约50%)生成糠醛、麦芽酚和甲基环戊烯酮(cyclotene),从而产生焦香甜气。
美国橡木含有比法国橡木更多的橡木内酯和降异戊二烯成分。
在一个新的大桶(300L)中,每渗入木头1mm的酒提取约11g橡木。最初的1mm要约1周来渗入。按每升酒的桶表面积计算,对于200L的桶,酒每渗入桶内1mm提取约7.6g的木材提取物,对于500L的桶,每渗入桶内1mm提取约5.6g的木材提取物。
一个225L的新桶可在约两个月时被渗透至0.5mm深处,提供约3.8g木材提取物。按味觉结果计算,这是在酒中产生可检测差异所需量的约3-10倍。经过较长时间后,渗透最深可达6mm。
这表明在一个225L的桶中可提取最多至46g木材。这是大多数酒的最小气味检测水平的约100倍,或者可将桶中加满酒并倒出100次,使桶以可检测水平为所有酒增添风味。
当表面逐渐用尽时,橡木成分向酒中的扩散将在一定程度上发生改变,因为较大分子扩散花费时间更长。但是能够扩散通过半透木系统的分子最终会被提取,并且不出所料的是,甚至在桶经长期连续使用后,它仍可为在其中储藏足够长时间的酒增添可检测水平的橡木味。
通常,为酒品增添木材特性的唯一途径就是通过在橡木桶或橡木罐中进行接触。但过去10年中,随着购买橡木桶的成本不断增加,想保留橡木优点的酒品制造商出于经济上的考虑转向使用橡木备用品、橡木替代品或橡木的备选物。橡木备用品实际上可以是橡木(不被制成桶)的任何部分。各种备选物的名称依供应商而定,但基本选择包括多种长度和烘烤水平的狭板和插件、木块、立方块、“多米诺骨牌”、木屑、刨花、橡木棒分支和橡木粉。这种橡木的品质媲美于橡木桶,但其成本却不同。
目前广泛采用水提法和化学提取法来从原料中提取重要组分例如油、香料、色素、药物化合物或营养化合物。这些方法的速度和产量对生产成本具有重要影响。
农业生产中释放大量被发现含有显著量的高价值组分和膳食纤维(它们是有价值的物质)的废弃物。从食品中提取高价值组分可为生产者提供额外的收入。常规的提取法存在许多问题,包括有机化学品消耗高、操作时间长以及产量低等。
已进行了一些尝试通过利用超声振动促进原料和提取剂之间的接触来改进对某些物质的提取过程。
欧洲专利583200公开了一种用连有超声换能器的提取柱来提取月见草油的方法。
美国专利5859236公开了一种微晶纤维素的提取方法,其中对提取液进行超声搅拌。
这些现有的专利表明,在小批量环境下,产生波振动的低功率超声技术有助于提取。但低功率超声技术无法用于连续流动过程。在这种情况中,超声能量密度低,超声保留时间短并且体积/生产速度高。
此外,现有专利中使用的技术在用于流动的流体或介质时不可能不发生故障、过热、电力过载,原因是发生器和换能器的电/电子设计规格并不是设计用于处理物理条件和化学条件(例如,流速、压力、温度、气体夹带、液体蒸气压、表面张力)不断发生改变的流动流体的。低功率超声被设计成只用于小批量体积,并且是静态的(非流动)。使用低功率超声的经验已经表明,其成本效益在商业上没有吸引力或者在技术上/经济上不可行。
发明内容
本发明的一个目的是提供一种更加行之有效的从原料中提取化学成分的方法。
本发明的一个目的是克服或者至少基本改善现有技术的缺点和不足。
参照附图,本发明的其他目的和优点将从以下描述中显而易见,其中通过图示和举例说明公开了本发明的实施方案。
不应认为以任何方式限制本发明,本发明提供了一种从材料中以水提法提取化合物的方法,其中提取液相中夹带的材料在被浸没的超声焊极周围流动,所述超声焊极以0.01至1000W/cm3(或0.01至1000W/cm2)的能量强度向橡木流体介质中发出径向或聚焦的超声波,但最优选地,该过程将在0.1至100W/cm3或0.1至100W/cm2的能量强度下有效地进行。
该高能量波可在待处理介质中形成高能量空洞、机械冲击波、微流动、高能量振动和高能量压力波。
使用浸没于液相中的超声焊极可促进超声波向材料内部的穿透。这与现有技术中将换能器钳定于/螺接到/焊接到钢制容器/室外部的情况不同。该效应在液体中产生低能量、低效的驻波/定波,这样就只能进行外表面提取,并且只有在停留时间非常长(>1小时)时才可行。驻波/定波的能量强度仅在0.0001W/cm3区域内。
此外,现有技术常限于批处理而不适于连续流式提取。
使用高强度的超声径向波或聚焦能量可在橡木材料表面及结构内部产生微流效应/空化效应,从而移出/移去组分并增强水的渗透。相比之下,使用将换能器钳定于/螺接到/焊接到钢制容器/室外部的概念的现有超声方法在材料中产生低能、低效的驻波/定波,其不会产生增强水渗透和组分移出的微流效应。相比之下,在液流中引入高强度超声焊极可产生0.01-1000W/cm3的强度,使得可以形成高速微流效应(780km/h),从而增强水渗透和组分移出。
本发明使用低频超声(16kHz-100kHz)从材料中提取物质,优选的频率为20至30kHz。使用本发明的方法可以提取大量物质,包括但不限于材料中存在的着色剂、调味剂和营养化合物(neutraceuticalcompound)。
超声频率和超声焊极设计以及流通池设计需与待提取材料相适应。有机负载的程度和材料的结构类型将决定超声焊极设计的类型。特定的超声焊极的设计将可以使超声波/空化能量更好地穿透、能量和产品的偶联更强并且提高能量效率,从而增强组分的提取、水的渗透和组分从正在被提取材料中的移去。
优选地,本发明的应用可包括用水性溶剂、有机溶剂或这两者的组合来从葡萄皮中提取有色化合物和调味化合物,从葡萄皮中提取花色苷(anthracyanin),从葡萄籽中提取抗氧化剂。
例如,低有机负载的橡木处理过程或具有强超声能量吸收因子的产品可使用级联设计径向式超声焊极。相反,具有高有机负载或者低超声吸收系数的处理过程可使用具有增大的直径比长度(波长)因子/比率的径向式超声焊极,所述超声焊极可产生传播距离更长,并且穿透具有高有机负载的产物流或具有低超声吸收系数的产品的能力更强的超声波。使用焊接/螺接于容器/室/管外部的换能器的现有技术装置并不是被设计用于特定类型的有机负载和具有不同超声吸收特性的产品。
使用针对不同类型产品的自动频率扫描系统可提高水渗透和组分提取的效能。例如,对于从橡木中提取化合物,有机负载(浓度、粘度)越高,决定该系统/橡木产品的共振频率的橡木表面/组织/结构的类型就越多。超声共振频率为超声单元产生最高能量效率时的频率。
本发明还提供一种超声系统,该系统自动跟踪(1ock)特定产品的共振频率,并在整个处理过程中每0.001秒重新扫描一次新的共振频率。如果不进行共振频率跟踪扫描,共振频率仅10Hz的变化将会导致能量效率的数量级减小10%-40%。这样就会显著降低水渗透、组分提取和组分移去。
例如,莴苣的共振频率为20,350Hz,而胡萝卜的共振频率为20,210Hz。使用焊接/螺接于容器/室/管外部的换能器的现有技术装置未被设计成带有用于特定类型橡木产品的共振频率自动跟踪系统,因此就不能以正确的共振频率和最高的功率效率处理产品。
优选使用高功率和高振幅超声(0.001W/cm2-1000W/cm2)以及1μm-500μm(优选的振幅范围可以是20-60μm)的位移进行提取。现有技术的装置不能产生这样的能量水平和振幅水平。
本发明特别用于促进以水作为溶剂进行的橡木产品的组分提取。使用能产生高速微流、高能量空洞的高功率、能量效率的聚焦及径向系统可以使水穿过疏水表面并深入橡木材料的组织/结构内部以移出/移去组分。
因此,使用本发明的系统时,有机溶剂可被水完全或部分替代,从而减少了由于使用例如己烷等溶剂所致的安全隐患。
但本发明也可应用于联合使用超声波与水和有机溶剂的混合物(例如,水和乙醇)或者联合使用超声波和有机溶剂(例如,醇、己烷、丙酮),从产品例如橡木产品中提取化合物。低频超声还可以和高压下的超临界流体(例如,液体CO2)联合用于从橡木材料中提取组分和化合物。
超声换能器可连接于已有的含有超临界液体的高压容器上。
本发明的另一方面是联合使用低频/高强度超声和温热(0℃-60℃)从橡木产品中提取组分、化合物。超声能量和热能的协同效应可提高提取动力学和提取产量。
本发明的另一方面是联合使用低频/高强度超声和压力(0.5至10巴(bar),但优选2-4巴)从橡木产品中提取组分、化合物。这种超声能量和压力之间的协同效应可明显促进超声波和介质之间的偶联和阻抗匹配,特别是在流体具有高固体含量时尤其如此。超声波和产品之间偶联的增强可提高提取动力学和提取产量。
在优选的设备设计中,本发明涉及使用径向式超声焊极,该焊极可发出高能量超声波。但也可使用其他超声焊极,例如高振幅聚焦式超声焊极,该焊极能在超声焊极表面周围形成高浓度的局部空泡。
根据本发明的超声焊极和流动池的排布是基于应用这样一种径向式超声焊极,所述超声焊极浸没于液相中且能被调至具有16kHz-100kHz范围的频率,所述排布可产生0.01至1000W/cm3的能量强度。
一种排布,包括纵向或横向固定于一个敞口的罐、沟或槽中的径向式超声焊极。底部安装反射罩以将超声能量反射和/或聚焦到产品流路上。
另一种合适的排布利用固定于流通池中的聚焦式或径向式超声焊极,在所述流通池中,水/橡木产品或直接流入超声焊极面或跨过超声焊极面。停留时间可通过调节从超声焊极流出的微流、流速、换能器/超声焊极的功率和大小、串联和并联的换能器超声焊极的数目以及容器几何形状来控制。
本发明涉及从基于橡木的材料中以高功率超声提取化合物,但上述技术也可用提取基于园艺/农艺的其他材料(例如,水果、蔬菜、谷物、草、种子)的营养物质、抗氧化剂、油、调味剂、着色剂、生物活性化合物和食品材料。
优选地,本发明包括超临界流体/提取技术(例如,液体CO2)以提高产率和工艺动力学。
附图说明
通过示例的方式,下文参照附图更充分地描述本发明的应用,其中:
图1示出了纵向固定于槽中的本发明的径向式超声焊极;
图2示出了用于封闭流通池的本发明的横向超声焊极;
图3示出了在转鼓式提取器中的本发明的聚焦式超声焊极;
图4示出了在封闭流通池中的本发明的径向式超声焊极;
图5示出了用水从橡木材料中进行10秒钟的化合物提取的本发明结果;
图6示出了用水从橡木材料中进行30秒钟的化合物提取的本发明结果;
图7示出了用12%乙醇/水从橡木材料中进行10秒钟的化合物提取的本发明结果;
图8示出了在100%和30%振幅时以不同超声时间提取鲜食葡萄的色谱图(聚焦式);
图9示出了在100%振幅时以不同超声时间提取鲜食葡萄的色谱图(径向式);
图10示出对照组;搅拌不同时间段提取的鲜食葡萄的色谱图;
图11a和11b,酒业中用于质量控制的色度分析的两个标准波长处的颜色吸收度。11b代表颜色强度,即每个波长处的吸收之和。数据取自图8-10;
图12示出了图8-10的提取在不同超声时间后的pH;
图13示出了不同实验条件下进行的柠檬提取;
图14示出了以wt%表示的茶中可提取的固体。[F=聚焦式,R=径向式,100%和25%=振幅];
图15示出了所提取的茶的紫外-可见光吸收度。[F=聚焦式,R=径向式,100%和25%=振幅];
图16示出了提取的咖啡的紫外-可见光吸收度。[F=聚焦式,R=径向式,100%和25%=振幅];
图17示出了用水和12%乙醇/水进行的橡木屑提取。[F=聚焦式,R=径向式,100%和25%=振幅]。
具体实施方式
本发明的系统包括电源、将电能转换成机械振动能的换能器,所述机械振动能通过超声焊极5传送到液相提取系统。根据应用,所述超声焊极5可提供径向波、驻波或聚焦式发射。所述超声焊极材料可由钛或陶瓷、钢、铸造合金或玻璃制成。
所述换能器系统可以是PZT(压电陶瓷换能器)、Terfenol-D磁致伸缩换能器或者镍-铁-钒磁致伸缩材料。
正如现在可被充分理解地,可在使用传送器运输产物时使用本发明的浸没的超声焊极5。此外,本发明还可以是用于低有机负载的液体的级联超声焊极,以及直径与长度的比率更高以改善在高有机负载液体中的渗透的径向式超声焊极。
超声范围(10kHz至100kHz)、强度(0.01W/cm3-1000W/cm3)和振幅(1微米位移-500微米位移)的应用。换能器/电源可各自具有100W至16000W的功率。所述电源优选地包括共振频率自动跟踪器,从而使得在提取过程中设备运行时,该单元还能一直扫描由于液流12中的变化所致的新的共振频率(与最大功率输出有关)。所述超声焊极/换能器可被安装于或改装到含有提取液相流12中夹带的固体材料的罐、容器(圆形、方形、椭圆形)、沟、管、流通池10。图1示出了浸没于提取液相7中的超声焊极5,其中反射器9在槽11中。
此外,所述发明还可联合使用超临界流体/提取技术(例如,液体CO2)以提高产率和工艺动力学。可将换能器置于提取管的外壳上,从而使该提取管成为超声焊极。之后,在该超临界溶剂和固体基质所处的超临界提取管内产生超声波。或者,超声焊极可通过超临界提取管内部的凸缘连接于内部,在超临界提取管内直接固体基质和超临界流体接触。
超声波和产生的空洞有助于超临界流体向固体基质中的溶剂质量传递。这类应用的实例为从姜中提取姜辣素(gingerol)。
本领域技术人员可能不太容易理解的是,上述发明也可被容易地用于从茶叶中提取(水提法提取)茶固体、着色剂、调味剂和多酚,从咖啡中提取咖啡因,从完整的及研碎的烘烤咖啡豆中提取(水提法提取)咖啡、调味剂和着色剂,从例如水果、果浆、果皮等的农产品中提取抗氧化剂、营养物质、生物活性物质和类胡萝卜素。
从蔬菜、蔬菜浆、蔬菜外皮和坚果中进行提取的实例可以是从番茄浆或番茄皮中提取番茄红素,从胡萝卜浆和胡萝卜皮中提取α和β胡萝卜素,从例如柑橘、葡萄柚、酸柠檬、柠檬等的柑橘类水果外皮中提取柠檬油(citrus oil)。这可以是用水或溶剂例如乙醇,或者水和溶剂的组合物从例如水果、果浆、果皮等的农产品中提取油。
可从玉米或玉米芽、大豆、橄榄、油菜籽、棕榈植株和棕榈果/纤维中提取玉米油,从植物材料/花瓣材料中提取玫瑰油。上述提取可以是用水或溶剂例如乙醇、己烷、丁烷或者水和溶剂的组合进行的提取。
可从包括水果、蔬菜和坚果等的农产品中提取调味料,例如,从可可豆中提取巧克力、从肉中提取蛋白质、从乳制品中提取肾素、从甜菜或甘蔗中提取糖,从玉米、大豆、小麦(和其他农业材料)以及这些材料的纤维中提取淀粉,从基于水果和蔬菜的材料中提取汁液。
实施例
橡木调味剂提取
用150ml自来水或12%乙醇/水或100%乙醇对40g橡木进行提取。将样品搅拌(对照样品)或超声处理10秒和30秒,然后取液体样品过筛(约0.8mm网孔),之后用1号Whantman滤纸过滤。用水将滤液子样品稀释3.5倍,并将其送往澳大利亚酒品研究所(the AustralianWine Research Institute)通过GC-MS进行橡木调味剂分析。
结果
GC-MS鉴定的化学物质的定量限值(稀释的提取物中以μg/L表示的量)为愈创木酚3.5、丁香酚35、橡木内酯35、香草醛35以及糠醛35。分析出的但低于定量限值的其他化学物质为:4-甲基愈创木酚、4-乙基苯酚、4-乙基愈创木酚和5-甲基愈创木酚。
该提取数据表明,在相同的提取时间内,相对于对照样品而言,使用上述方法进行超声处理可促进对所需化合物的提取。
在径向模式中,12%乙醇(图5)最为有效,但在聚焦模式中,水(图6和7)是最有效的。
从上述结果可知,超声处理可显著增进对橡木调味剂的提取,这正如GC-MS对橡木调味剂的测量结果。在聚焦模式中,水最为有效,而12%乙醇在径向模式和聚焦模式中的效力相似。将振幅降至25%也不会明显减弱对调味化合物的提取。
使用不同的超声方法和时间从红色鲜食葡萄中提取着色剂(花色苷)。
进行了10个提取试验;每个都使用150m1去离子水和从20粒红色鲜食葡萄上剥下的葡萄皮。将对照样品搅拌10、60和120秒,然后取液体样品进行pH分析,之后用紫外-可见分光光度计进行色度测量。超声样品为以100%的振幅处理相同时间段(10、60和120秒),一个样品为以30%的振幅处理60秒。超声仪以聚焦或径向模式工作。表1中示出了不同的实验组合。对照样品的pH被调至4.3,从而与pH在4.3至4.5之间变化的超声样品相一致。所有样品均在不进行过滤时以及用0.2μm针头式滤器过滤后分别进行色度测量。
结果
通过特定波长下的光吸收度测得,随着提取时间增长颜色强度增加,见表1,图8-10和11的对照(搅拌)和超声样品。图8的x-和y-轴刻度和图9相同,通过比较可清楚看出,聚焦模式的提取物比径向模式的提取物颜色更深。波长420nm和520nm处的吸收度的总和被定义为该提取物的颜色强度,这也是酒业中通常所测量的。结果示于图11b中,而每个波长下各自的吸收度示于图11a中。显然,超声处理大幅促进了花色苷的提取,由此增加了颜色强度。
表1
提取时间 | 10 | 60 | 120 |
径向式100%420nm | 0.0196 | 0.0942 | 0.1832 |
径向式100%520nm | 0.0148 | 0.0884 | 0.198 |
聚焦式100%420nm | 0.033 | 0.1356 | 0.3368 |
聚焦式100%520nm | 0.0264 | 0.1254 | 0.376 |
对照420nm | 0.004 | 0.0076 | 0.0152 |
对照520nm | 0.002 | 0.002 | 0.002 |
聚焦式30%420nm | 0.0296 | ||
聚焦式30%520nm | 0.0224 |
将超声时间从60秒延长至120秒导致吸收度增加2倍以上。
图12示出了各样品的pH。该pH随超声时间延长而略有下降,这可能是由于从水果和水果皮中释放酸所致。不改变对照pH时的吸收度并没有明显不同,这可能是由于花色苷的存在量处于仪器的检测限之故。
结论
使用所述方法进行超声处理可增加对葡萄皮中存在的红色着色化学物质花色苷的释放。正如使用聚焦模式可加强颜色强度,延长超声时间对颜色强度也具有积极的影响(图11)。将振幅降至30%可如预期地减弱提取。
从胡萝卜中提取胡萝卜素以及从柠檬和酸柠檬中提取柠檬烯
胡萝卜素的提取和分析方法
将一批胡萝卜用食品搅拌器混合。通过400W的台式仪器进行超声或者通过手动混合(对照样品)将30g该混合物用150ml 20%乙醇水溶液悬浮。考虑的变量为,提取时间:10、20和30秒,聚焦式和径向式超声模式,以及径向模式中100%振幅和25%振幅。提取后立即用0.8mm孔径的不锈钢筛进行过筛移出液体组分。然后用孔径为0.45μm的针头式滤器过滤所述过筛液体的等分试样。之后,将其用20%乙醇水混合物稀释6倍,并用紫外-可见光分光光度计进行分析。本底样品为纯提取溶剂(20%乙醇水混合物)的等分试样。
柠檬和酸柠檬中柠檬烯的提取和分析方法
用食品搅拌器将各水果的水果皮混合。对于柠檬,通过400W台式仪器(制造商)进行超声或者通过手动混合(对照样品)将30g混合物用150ml水悬浮。考虑的变量为,提取时间:5、10和30秒,聚焦式和径向式超声模式,以及径向模式中的100%和25%振幅。对于酸柠檬,通过400W台式仪器进行超声或者通过手动混合(对照样品)将15g混合物用75ml水悬浮。考虑的变量为,提取时间:10和30秒,聚焦式超声和径向式超声模式,以及径向式超声中100%和25%振幅。对柠檬和酸柠檬进行提取后,立即用0.8mm孔径的不锈钢筛过筛将液体组分移出。将10ml己烷加至每种液体样品中并手动强力混合30秒,然后使其静置至当日结束。通过在约-15℃下冷冻过夜以除去水组分,并倾出液体己烷。
用紫外-可见光分光光度计分析每个样品的等分试样,以己烷为本底样品。
结果
在特定波长处吸收度增加表明存在的分析物增加。针对一幅图中每个坐标卡(chart)所示的每种波长,可对各变量(时间、超声模式和振幅)进行描绘。图13为一代表性实例,显示出各变量对柠檬和酸柠檬提取的影响。
该数据表明,与对照样品相比,在相同提取时间内,使用所述方法进行超声可促进提取。延长提取时间可增加测得的胡萝卜、柠檬和酸柠檬提取物。
茶、咖啡和橡木的提取
针对茶和咖啡的方法
利用200ml自来水(在80℃下,对于咖啡,还在50℃下测两个数据点)和40g茶或咖啡分别进行提取。将样品搅拌(对照样品)或超声10、20和30秒,然后取液体样品过筛(约0.8mm网孔),再对咖啡进行0.45μm孔径过滤,对茶进行0.2μm孔径过滤。立即取滤液子样品,用1∶1(重量)的乙醇/水混合物将茶滤液稀释10倍,用水将咖啡滤液稀释50倍,然后用紫外-可见光分光光度计进行测量。对剩余的过滤样品称重,并使其在80℃下干燥。在干燥前后对所有提取样品称重,从而使得能够以所提取液体/溶液的a%计算可提取固体。
针对橡木的方法
用150ml自来水或12%乙醇/水对40g橡木进行提取。对于橡木屑,仅用12%乙醇混合物提取一次。将样品搅拌(对照样品)或超声10、20和30秒,然后取液体样品过筛(约0.8mm网孔),之后用1号Whatman滤纸过滤。立即取滤液子样品,用其中任一种提取溶剂稀释5倍,然后用紫外-可见光分光光度计进行测量。用水将另一份滤液子样品稀释3.5倍,并送去作GC-MS橡木调味剂分析。
使用的橡木粉:Medium toast,约1mm颗粒大小
使用的橡木屑:Heinrich Coorperage,American Oak Medium.颗粒大小约为10-18mm长,2-7mm宽,1-2mm厚。
结果和讨论
图1和图2示出了茶的可提取固体(过滤后溶液的固体百分比)和320nm波长处的紫外-可见光吸收度。除了在350nm处进行光谱学测量外,图3和4显示出的针对咖啡的信息与茶相同。橡木提取物仅显示出在270nm处有紫外-可见光吸收。
结果
所有数据表明,与对照样品相比,在相同提取时间内超声处理可促进提取。
可对所述方法步骤和系统的部分或全部进行任意改进。本文所引用的所有参考文献,包括出版物、专利申请和专利均通过引用的方式纳入本文。除非另外声明,本文使用的任何的以及所有的实例或示例性用语(如“例如”)均旨在阐释本发明,而不是对本发明范围的限制。本文中关于本发明的本质或益处或者优选的实施方案的任何陈述并非旨在进行限制,并且不应认为随附的权利要求受到这类陈述的限制。通常,说明书中的用语都不应被理解为指明了任何非本发明所要求的要素对于本发明的实施是必需的。本发明包括施行的法律所允许的本文随附权利要求所引述的主题的所有变换形式和等同形式。此外,除非本文另外指明,或者明显与上下文相矛盾,上述要素所有可能的变形形式的任何组合均包括在本发明内。
Claims (17)
1.一种从固体材料中提取化合物的方法,其中所述固体材料被夹带在提取液相中,所述提取液相在浸没于其中的超声焊极周围流动,所述超声焊极以约0.1至100W/cm2的能量强度向所述液相发出超声波。
2.权利要求2的方法,其中发出的超声波为径向式或聚焦式。
3.权利要求3的方法,其中所述方法进一步包括将所述液相脱气。
4.权利要求4的方法,其中所述材料为食品。
5.权利要求1-5中任一项的方法,其中所述方法进一步包括调节所述超声焊极以自动跟踪所述夹带于提取液相中的材料的共振频率。
6.权利要求6的方法,其中所述液相为水性液体。
7.权利要求7的方法,其中所述水性液体为水。
8.权利要求6的方法,其中所述液相为超临界液体。
9.权利要求1-5中任一项的方法,其中所述液相被加热至0-60℃。
10.权利要求1-10任一项的方法,其中所述液相保持于某一压力下。
11.权利要求11的方法,其中所述压力为0.5巴至10巴。
12.权利要求12的方法,其中所述压力为2巴至4巴。
13.权利要求5的方法,其中所述食品材料选自水果、蔬菜、谷物、草、种子和它们的混合物。
14.一种从固体材料中提取化合物的装置,包括一个提取器本体;
i.一个引导所述材料周围的提取液相从而使所述材料夹带于其中的导管;
ii.至少一个与至少一个超声焊极有效连接的超声发生器,所述至少一个超声焊极与所述液相相接触;
iii.使得所述超声发生器工作时产生作用于所述液相中夹带的固体材料的超声能量。
15.权利要求14的装置,其中所述超声发生器以约0.1至100W/cm2的能量强度工作。
16.权利要求15的装置,其中所述的与超声发生器有效连接的超声焊极可被调节以自动跟踪所述提取液相中夹带的材料的共振频率。
17.基本上如本申请所述的、用于从固体材料中提取化合物的装置。
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Application Number | Priority Date | Filing Date | Title |
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AU2006907033 | 2006-12-18 | ||
AU2006907033A AU2006907033A0 (en) | 2006-12-18 | High energy ultrasound extraction | |
PCT/AU2007/001958 WO2008074072A1 (en) | 2006-12-18 | 2007-12-18 | High energy ultrasound extraction |
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CN101622043A true CN101622043A (zh) | 2010-01-06 |
CN101622043B CN101622043B (zh) | 2013-10-16 |
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US (1) | US8343562B2 (zh) |
EP (1) | EP2106278A4 (zh) |
JP (1) | JP2010512998A (zh) |
CN (1) | CN101622043B (zh) |
AU (1) | AU2007335247B2 (zh) |
BR (1) | BRPI0720541A2 (zh) |
WO (1) | WO2008074072A1 (zh) |
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WO2010138254A1 (en) * | 2009-05-28 | 2010-12-02 | Cargill, Incorporated | Improving oil recovery and reducing the oxygen demand of palm oil mill effluent |
IT1399668B1 (it) * | 2010-04-09 | 2013-04-26 | Gambardella | Processo ed impianto di estrazione di oli ed essenze da sostanze organiche e loro eventuale deodorizzazione |
US10334870B2 (en) | 2010-10-07 | 2019-07-02 | Tropicana Products, Inc. | Processing of whole fruits and vegetables, processing of side-stream ingredients of fruits and vegetables, and use of the processed fruits and vegetables in beverage and food products |
DE102010052052A1 (de) * | 2010-11-23 | 2012-05-24 | Abel und Schäfer GmbH & Co. KG | Verfahren zur Behandlung von Mohnsamen |
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- 2007-12-18 CN CN2007800512116A patent/CN101622043B/zh not_active Expired - Fee Related
- 2007-12-18 WO PCT/AU2007/001958 patent/WO2008074072A1/en active Application Filing
- 2007-12-18 JP JP2009541691A patent/JP2010512998A/ja active Pending
- 2007-12-18 EP EP07845399A patent/EP2106278A4/en not_active Withdrawn
- 2007-12-18 US US12/520,062 patent/US8343562B2/en not_active Expired - Fee Related
- 2007-12-18 BR BRPI0720541-4A2A patent/BRPI0720541A2/pt not_active IP Right Cessation
- 2007-12-18 AU AU2007335247A patent/AU2007335247B2/en not_active Ceased
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CN108604882A (zh) * | 2014-03-20 | 2018-09-28 | 彼得·哈格尔施泰因 | 振动能的转换 |
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EP2106278A4 (en) | 2011-02-02 |
AU2007335247A1 (en) | 2008-06-26 |
WO2008074072A1 (en) | 2008-06-26 |
US8343562B2 (en) | 2013-01-01 |
JP2010512998A (ja) | 2010-04-30 |
US20100015302A1 (en) | 2010-01-21 |
AU2007335247B2 (en) | 2011-11-17 |
CN101622043B (zh) | 2013-10-16 |
BRPI0720541A2 (pt) | 2014-02-18 |
EP2106278A1 (en) | 2009-10-07 |
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