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1.
电化学氧化法合成茴香醛(Ⅱ)   总被引:3,自引:0,他引:3  
杨爱云  胡云楚 《合成化学》1995,3(3):239-243
研究了茄香脑电氧化合成茄香醛的最佳条件:以乙醇和水为溶剂,以含1.9%茄香脑和1.6%NH4NO3(支持电解质)的乙醇溶液作阳极液;不含茄香脑的混合溶液的阴极液。溶液PH=1-2,池温25-28℃,控电流电解,电流效率60-62%,反应总级数n=1。  相似文献   

2.
本文系统地研究了酱香型酒主体香的分离方法,摸索出“溶剂萃取-自然挥发-溶解”的酱香型酒空杯香的分离方法,首次从珍酒、茅台酒中分离出典型的空杯香。用在线色谱闻香系统研究了酱香型酒空杯香的化学成分,同时进行色谱测定及嗅闻。结果表明,空杯香是多种成分构成的复合香。  相似文献   

3.
以间苯三醛和茄香醛为原料,经Hoesch-Houben反应,羟基保护、缩合、Algar-Flynn-Oyamade反应、甲基化、等6步反应合成了3,4′-二甲氧基莰菲醇。  相似文献   

4.
土木香内酯的电化学研究   总被引:3,自引:1,他引:3  
用单扫示波极谱法,在01mol/LLiCl中,土木香内酯有两个极谱还原波:P1(-141V)和P2(-151V)(vs.SCE),峰P1的峰高与浓度在43×10-7~12×10-6mol/L和13×10-6~15×10-5mol/L范围内呈线性关系,可进行定量分析,用标准加入法能作定性分析,其检测限为26×10-7mol/L。测定了中药土木香中总内酯的含量,其结果令人满意。实验证明土木香内酯的电极过程为带有吸附性的不可逆的逐级电子反应过程,另外,还证明了H2O2可催化峰P1和羟基自由基可催化峰P2,讨论了土木香内酯清除由邻苯三酚自氧化产生的活性氧自由基(O-·2)的作用。  相似文献   

5.
每个农民都知道下列两个事实:不是每一棵玉米杆都甜,而是少数不长棒子的(不结穗)才甜。春天种的玉米远不如夏天种的(麦收后种)甜,夏天种的有的即使长棒子也甜。为了使每棵玉米都变甜,我采取了两种方法:(1)密植;(2)在玉米穗刚刚生出来时就用人工方法除掉它。两种措施的目的都是为了使玉米不结穗。  相似文献   

6.
超临界CO2萃取石菖蒲有效成分的GC-MS分析   总被引:7,自引:1,他引:7  
采用超临界CO2流体萃取技术从石菖中萃取分离挥发油,用气相色谱-质谱联用技术测定其化学成分,从中鉴定出26种成分,并测定了其相对含量,主要成分为:顺-细辛脑、反-细辛脑、绿叶烯、石竹烯、蛇麻烯、甲基丁子香酚、榄香纱,顺-罗勒烯等。  相似文献   

7.
闫吉昌  曾宪录 《分析化学》1994,22(12):1214-1218
本文用顶空收集法和蒸馏-萃取法提取富集了松口蘑子实体和菌丝体中的香成分,经色谱/质谱联机分析,在子实体中测得64种香成分,并首次在菌丝体中测得36种香成分。菌丝体中有28种组分与子实体香成分相同。为深入研究和开发珍贵的松口蘑提供了科学依据。该提取方法充分有效;该分析方法简便,灵敏度高,可做为分析天然产物香成分时参考。  相似文献   

8.
络合吸附波极谱法测定稀土钢中微量稀土   总被引:2,自引:0,他引:2  
研究了在pH9.2-pH9.5的NH30Na2B4O7介质中,稀土与百里香酚酞的络合物极谱波,波高与镧量在4.0×10^-7-3.6×10^-6mol/L范围内成线性关系。方法已用于稀土钢中微量稀土的测定。  相似文献   

9.
用N2吹扫-冷凝方法分离、收集珍酒、茅台酒的前香。收集液经过感官评定,确认为珍酒、茅台酒的前香。用气相色谱/质谱联用方法研究它们的化学组成。鉴定了12种化合物,并测定了它们的相对含量。  相似文献   

10.
用N2吹扫-冷凝方法分离、收集珍酒、茅台酒的前香。收集液经过感官评定,确认为珍酒、茅台酒的前香。用气相色谱/质谱联用方法研究它们的化学组成。鉴定了12种化合物,并测定了它们的相对含量。  相似文献   

11.
佛手挥发油的化学成分   总被引:25,自引:0,他引:25  
用色谱-质谱-计算机联用法对佛手挥发油的化学成分和相对含量进行了系统分析,得到67种组分,鉴定出31个组分,主要组分是柠檬烯(48.4%)、1-甲基-2-(1-甲乙基)-苯(30.8%)。  相似文献   

12.
石宇  王珊娣  陈庆云 《有机化学》1986,6(4):305-308
聚全氟烷基三嗪(1)具有耐高温、耐氧化和耐酸等特性,可作为气相色谱固定液。它不仅可以分离有机氟化合物如含氟磺酰氟、磺酸酯等,而且也适用于同时含有氯、溴、碘的有机氟化合物。  相似文献   

13.
Titanate sol–gel layers imprinted with midchain carbonic acids have proven highly useful for detecting engine oil degradation processes owing to selective incorporation of oxidised base oil components. Synthesising the material from TiCl4 in CCl4 and precipitating with water leads to imprinted TiO2 nanoparticles with a diameter of 200–300 nm. Replacing the water by a 1 M ammonium hydroxide solution reduces the average particle size to 50–100 nm with retention of the interaction capabilities. Experiments with the latter solution revealed that the 100-nm particles take up substantially more analyte, indicating a size-dependent phenomenon. As the number of interaction sites within each material is the same, this cannot be a consequence of thermodynamics but must be one of accessibility. The sensor characteristic of water-precipitated particles towards engine oil degradation products shows substantially increased sensitivity and dynamic range compared with the corresponding thin films. Coating quartz crystal microbalances with such nanoparticle materials leads to engine oil degradation sensors owing to incorporation of acidic base oil oxidation products. Interaction studies over a large range of layer thicknesses revealed that both the absolute signal and the steepness of the correlation between the sensor signal and the layer height is 2 times higher for the particles. Figure Generation of molecularly imprinted sol–gel nanoparticles  相似文献   

14.
用正己烷溶解达川和万县产的两种红橘油,将样品皂化和甲酯化后,以毛细管柱DB-WAX作为分离柱,用气相色谱-质谱法测定其中的脂肪酸组成,两种红橘油的主要脂肪酸成分有明显的差别,两者的不饱和脂肪酸相对含量分别为92.1%及76.7%。  相似文献   

15.
柴油烃族组成分布的GC-MS测定   总被引:6,自引:0,他引:6       下载免费PDF全文
应用GC-MS测定柴油烃族组成按沸点的分布,通过柱色 谱分离后的柴油饱和烃和芳烃组分分别进入气相色谱-质谱联用仪分析,采集其每一扫描的质谱图后,按ASTM-D2425方法计算其每一扫描的烃族组成,因为每一扫描与保留时间对应,所以可将两部分烃族组成加和后应用ASTM-D2887方法计算柴油烃族组成按沸点的分布规律;实验结果表明,该法与ASTM-D2887和ASTM-D2425的实验结果吻合,并能给出有关柴油烃族组成的详尽分布规律。  相似文献   

16.
臭椿籽挥发油的化学成分分析   总被引:4,自引:0,他引:4  
采用水蒸气蒸馏法对甘肃天水产的臭椿籽挥发油进行提取,挥发油得率约为2.1%(w);用气相色谱-质谱联用技术对挥发性成分进行了分析,鉴定了43个化合物,占挥发油相对含量的96.3%;主要成分为脂肪酸及酯、脂肪烃及甾族化合物,其中含量较高的有亚油酸、油酸、蓖麻酸和蓖麻酸甲酯。  相似文献   

17.
白果中脂肪酸的GC-MS分析   总被引:7,自引:1,他引:6  
将萃取所得白果油进行皂化、甲酯化后 ,进行GC-MS定性及相对含量分析 ,取得了满意的结果。实验检出30种脂肪酸 ,其中亚油酸和油酸占71.8%,不饱和脂肪酸占87.86%。  相似文献   

18.
In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment, the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach for oil spill identification in soils. Figure PCA score plots illustrate clear discrimination of types of crude oil in polluted soil samples (e.g. results are shown for vertisol)  相似文献   

19.
The properties of a scarcely studied twin-tailed surfactant, sodium dioctylphosphinate (SDOP), as emulsifier were studied. The SDOP hidrophile–lipophile balance (HLB) value was measured and the Davies HLB group number of the sodium phosphinate group was computed. The surfactant promotes the formation of water in petroleum ether emulsions. The emulsion was characterized by the employment of several techniques such as centrifuge test and turbidimetry and density measurements. The maximum stability was obtained by the surfactant concentration of 0.3 mol dm−3 with 14 g of water emulsified in 12.41 g oil/g surfactant was emulsified. Conductivity information was used to study the temperature effect on the emulsion droplets and the energy of the droplet clustering during percolation. The enthalpy of adsorption at the oil/water interface was positive at all surfactant concentrations ([S]); its absolute value showed a maximum of [S]=0.1 mol dm−3 and subsequent decreased was attributed to a change in the droplet interface, which would provide the necessary energy for the adsorption of SDOP molecules. The determination of droplet clustering thermodynamic parameters during percolation showed that droplet clusters were formed spontaneously and the process driving force was a negative enthalpy contribution.  相似文献   

20.
琼脂微载体的制备及肝细胞附着生长情况的研究   总被引:2,自引:0,他引:2  
以琼脂为原料,通过悬浮方法成球制备琼脂微载体,直径100~800μm.利用氨基化修饰琼脂微载体,比较大鼠肝细胞在其上的生长情况,并对培养的肝细胞的形态及葡萄糖、白蛋白的代谢情况进行了测定.  相似文献   

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