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用GC-MS方法测定了小茴香挥发油的全组分,其中对-丙烯基茴香醚的含量为82.65%。采用包结结晶方法对小茴香挥发油中的对-丙烯基茴醚进行了选择性分离,以1,1,6,6-四苯基-2,4-已二炔-1,6-二醇(简称D.D)作为主体分子,小茴香挥发油中的对-丙烯基茴香醚作为客体分子,D.D选择性地与之形成超分子包结物晶体。采用IR,1^HNMR,单日XRD确定了包结物的形成及其主客体分子摩尔比为2:1。包结物晶体属于P1空间群,晶胞参数:a=1.2972(2)nm,b=1.5119(2)nm,c=1.6799(2)nm,α=100.57(1)°,β=104.89(1)°,γ=113.58(1)°,Z=2。利用Kugelrohr真空蒸馏技术从包结物晶体中蒸出被分离的化学组分,用IR,1^HNMR和MS方法,确定了反式对-丙烯基茴香醚。用GC方法测定了选择分离出的挥发油化学,GC分析结果表明,分离的反式对-丙烯基茴香醚的化学纯度为97%,回收率为75.28%。 相似文献
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采用[CoCl4]2-为第一配体,质子化的N,N,N′,N′-四(对甲基苄基)乙二胺为第二配体,构筑二次球形配位主体框架,选择性地将蒿本挥发油中的肉豆蔻醚作为客体,与其形成超分子包结物晶体。 采用红外光谱(IR)、核磁共振(NMR)、粉末X射线衍射(PXRD)等测试技术确定了包结物的形成及其主客体分子摩尔比为2∶1,利用Kugelrohr真空蒸馏技术将肉豆蔻醚从包结物晶体中分离出来。 用IR、NMR等方法确定了被分离的化学组分为肉豆蔻醚。 用GC方法测定了选择分离挥发油化学组分,蒿本挥发油中肉豆蔻醚的含量为60.4%,分离的肉豆蔻醚气相色谱纯度为100%。 相似文献
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以1,1,6,6-四苯基-2,4-己二炔-1,6-二醇为主体分子, 可简单、迅速地从青椒挥发油中选择分离出化学成分烯丙基茴香醚, 基于挥发油的用量, 收率为3.78%. IR, 1H NMR, 13C NMR光谱和单晶衍射证实了包结化合物结构, 用气相色谱法评价了选择分离效果, 分离的烯丙基茴香醚气相色谱纯度为94.5%. 同时, 主体分子形成的隧道框架对茴香醛具有识别作用, 形成2∶1(主/客)物质的量比的特殊结构包结物晶体, 它是主客体分子物质的量比为1∶2包结物的超分子异构体. 相似文献
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次级化学平衡反相高效液相色谱法分离银杏酚酸 总被引:4,自引:0,他引:4
采用LC/(-)ESI-MS法对银杏叶中的致敏性成分银杏酚酸进行了鉴定。利用次级化学平衡理论,建立了银杏酚酸的反相银化高效液相色谱分离方法。从色谱热力学角度对银离子分离银杏酚酸的影响进行了考察。在流动相中添加银离子,降低了具不饱和侧链银杏酚酸的保留时间,且银离子浓度与容量因子的对数之间存在良好线性关系。在确定的色谱条件下,四种银杏酚酸均获得较高的分离度,表明反相银化液相色谱是分离碳数与饱和度不相同的银杏酚酸同系物的有效方法。 相似文献
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采用水蒸气蒸馏法从火棘叶中提取挥发油,利用气相色谱-质谱(GC-MS)联用方法分析火棘叶挥发油化学成分,并以面积归一法测定各成分的相对含量。从火棘叶挥发油中共鉴定出69种化合物,占挥发油总量的80.52%,主要成分为(-)-b-杜松烯(22.62%)、植物醇(19.90%)、二环倍半水芹烯(5.95%)、β-桉叶醇(5.78%)、1,2,3,4,4a,7-六氢-1,6-二甲基-4-(1-甲基乙基)-萘(2.78%)、表圆线藻烯(2.34%)等。 相似文献
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螯形主体分子的设计、包结性能及其在细辛挥发油 有效成分选择分离中的应用 总被引:4,自引:0,他引:4
设计了两种新的具有螯形骨架的主体分子反式-1,2-二苯基-1,2-苊二醇(1)和顺式-1,2-二(1'-萘基)-1,2-苊二醇(2),主体(1),(2)可与许多有机小分子化合物形成配位包合物。用IR和粉末XRD表征了主体分子(1)和(2)的包结物,用^1NMR测定了包结物的主客体分子摩尔比:(1)·DMF(1:2),(1)·DMSO(1:2),(1)·THF(1:2),(1)·二氧六环(1:1),(1)·吡啶(1:1),(2)·DMF(1:1)和(2)·DMSO(1:1)。单晶X射线衍射分析了包结物的晶体结构,(1)·DMF:空间群Pnaa,a=0.9377(1)nm,b=1.4351(1)nm,c=4.0463(3)nm;(1)·DMSO:空间群Pbcn,a=1.6278(1)nm,b=1.0751(1)nm,c=1.4980(1)nm;(2)·DMF:P2~1/n,a=0.9796(1)nm,b=1.2377(1)nm,c=2.2344(3)nm,β=93.02(1)°;游离主体(1):空间群P1,a=1.0461(1)nm,b=1.1213(1)nm,c=1.5496(1)nm,α=81.74(1)°,β=75.71(1)°,γ=89.00(1)°;分析了主体分子的刚性和柔韧性对包结性能的影响。并研究了主体分子(1)选择分离细辛挥发油,将顺甲基异丁香酚从挥发油中分离出来。 相似文献
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香樟树叶挥发油的化学成分研究 总被引:8,自引:0,他引:8
用同时蒸馏萃取法(SDE)和气相色谱-质谱连用技术(GC-MS)对香樟树叶挥发油成分进行了分离分析,共鉴定出98种化合物。其中主要成分为樟脑与β-芳樟醇(24.099%)、桉油醇(15.723%)、α-松油醇(11.204%)、石竹烯(4.957%)、蛇床-6-烯-4-醇(5.724%)、β-水芹烯(3.394%)等。 相似文献
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Piras A Cocco V Falconieri D Porcedda S Marongiu B Maxia A Frau MA Gonçalves MJ Cavaleiro C Salgueiro L 《Natural product communications》2011,6(10):1523-1526
Satureja thymbra L. is well known in Italy by the popular name of "Santoreggia sarda". It grows only in Sardinia and nowadays it is restricted to the slope of the Colle San Michele in Cagliari. The composition of the aromatic extracts obtained by supercritical CO2 and by hydrodistillation and their antifungal activity is reported. The collected extracts were analyzed by GC-FID and GC-MS methods. No significant differences were observed in the composition of the volatile extracts depending on the extraction method. The results showed the presence of thymol, gamma-terpinene, beta-caryophyllene, p-cymene, carvacrol and borneol as main components. The minimal inhibitory concentration (MIC) and the minimal lethal concentration (MLC) were used to evaluate the antifungal activity of the oils against Candida albicans, C. tropicalis, C. krusei, C. guillermondii, C. parapsilosis, Cryptococcus neoformans, Trichophyton rubrum, T. mentagrophytes, T. mentagrophytes var. interdigitale, Trichophyton rubrum, T. verrucosum, Microsporum canis, M. gypseum, Epidermophyton floccosum, Aspergillus niger, A. fumigatus and A. flavus. The volatile extracts revealed a wide-spectrum antifungal activity. They were fungicidal and similarly potent against yeasts, dermatophyte and Aspergillus stains, with MICs ranging from 0.16 to 0.32 pL x mL(-1). 相似文献
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van Hee P Elumbaring AC van der Lans RG Van der Wielen LA 《Journal of colloid and interface science》2006,297(2):595-606
Selective dissolved-air flotation for the separation of medium-chain-length polyhydroxyalkanoate (PHA) inclusion bodies (IBs) from Pseudomonas putida cell debris is investigated. Measurements show that both P. putida cell debris and PHA IBs have an iso-electric point of approximately pH 3.5. Selective aggregation and as a result selective flotation of PHA IBs was observed near this pH. Qualitative prediction of the aggregation behaviour was possible on the basis of the Van der Waals, hydrophobic and electrostatic interactions. In some cases however, the stability of the suspension could not be explained with these forces alone. It was therefore suggested that additional interactions, such as steric/brush effects, play an important role in the aggregation process. 相似文献
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Hydrodistillation-adsorption method for the isolation of water-soluble, non-soluble and high volatile compounds from plant materials 总被引:1,自引:0,他引:1
Proposed method of hydrodistillation–adsorption (HDA) on activated carbon and hydrodistillation (HD) with solvent trap were compared for the isolation of water-soluble, non-soluble and high volatile compounds, such as acids, monoterpenes, isothiocyanates and others from carob (Certonia siliqua L.), rosemary (Rosmarinus officinalis L.) and rocket (Eruca sativa L.). Isolated volatiles were analyzed by GC and GC/MS. The main advantages of HDA method over ubiquitous HD method were higher yields of volatile compounds and their simultaneous separation in three fractions that enabled more detail analyses. This method is particularly suitable for the isolation and analysis of the plant volatiles with high amounts of water-soluble compounds. In distinction from previously published adsorption of remaining volatile compounds from distillation water on activated carbon, this method offers simultaneous hydrodistillation and adsorption in the same apparatus. 相似文献