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31.
Application of chromatography technology in the separation of active alkaloids from Hypecoum leptocarpum and their inhibitory effect on fatty acid synthase 下载免费PDF全文
Qiulong Zhang Guangxiang Luan Tao Ma Na Hu Yourui Suo Xiaoyan Wang Xiaofeng Ma Chenxu Ding 《Journal of separation science》2015,38(23):4063-4070
A method that involved the combination of pH‐zone‐refining counter‐current chromatography and semipreparative reversed‐phase liquid chromatography has been established for the preparative separation of alkaloids from Hypecoum leptocarpum. From 1.2 g of crude sample, 31 mg N‐feruloyltyramine, 27 mg oxohydrastinine, 47 mg hydroprotopine, 25 mg leptopidine, and 18 mg hypecocarpine have been obtained. The structure of the new compound, hypecocarpine, is confirmed based on the analysis of spectroscopic data, including NMR, UV, and IR spectroscopy and positive electrospray ionization mass spectrometry. The known chemical structures were characterized on the basis of 1H and 13C NMR spectroscopy. The purities of the five alkaloids are all over 92.7% as determined by high‐performance liquid chromatography. The alkaloids’ cytotoxicity in breast cancer cells is assessed by using a Cell Counting Kit assay and their inhibitory effect on fatty acid synthase expression is assessed by a Western blot assay. These results suggest that leptopidine could suppress growth and induce cytotoxicity in breast cancer cells and that the cytotoxicity of leptopidine may be related to its inhibitory effect on fatty acid synthase expression. 相似文献
32.
Efficient Counter Electrode Manufactured from Ag2S Nanocrystal Ink for Dye‐Sensitized Solar Cells 下载免费PDF全文
Qingquan He Shoushuang Huang Dr. Jiantao Zai Nianqi Tang Bo Li Prof. Qiquan Qiao Prof. Xuefeng Qian 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(43):15153-15157
It is generally believed that silver or silver‐based compounds are not suitable counter electrode (CE) materials for dye‐sensitized solar cells (DSSCs) due to the corrosion of the I?/I3? redox couple in electrolytes. However, Ag2S has potential applications in DSSCs for catalyzing I3? reduction reactions because of its high carrier concentration and tiny solubility product constant. In the present work, CE manufactured from Ag2S nanocrystals ink exhibited efficient electrocatalytic activity in the reduction of I3? to I? in DSSCs. The DSSC consisting of Ag2S CE displayed a higher power conversion efficiency of 8.40 % than that of Pt CE (8.11 %). Moreover, the devices also showed the characteristics of fast activity onset, high multiple start/stop capability and good irradiated stability. The simple composition, easy preparation, stable chemical property, and good catalytic performance make the developed Ag2S CE as a promising alternative to Pt CE in DSSCs. 相似文献
33.
《Journal of mass spectrometry : JMS》2017,52(3):144-151
To improve our understanding of the electrospray ionization (ESI) process, we have subjected equimolar mixtures of salts A+X− (A+ = Li+, NBu4+; X− = Br−, ClO4−, BF4−, BPh4−) in different solvents (CH3CN, tetrahydrofuran, CH3OH, H2O) to negative‐ion mode ESI and analyzed the relative ESI activity of the different anionic model analytes. The ESI activity of the large and hydrophobic BPh4− ion greatly exceeds that of the smaller and more hydrophilic anions Br−, ClO4− and BF4−, which we ascribe to its higher surface activity. Moreover, the ESI activity of the anions is modulated by the action of the counter‐ions and their different tendency toward ion pairing. The tendency toward ion pairing can be reduced by the addition of the chelating ligands 12‐crown‐4 and 2.2.1 cryptand and is, although to a smaller degree, further influenced by the variation of the solvent. Complementary electrical conductivity measurements afford additional information on the interactions of the ionic constituents of the sample solutions. Copyright © 2017 John Wiley & Sons, Ltd. 相似文献
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通过简单的原位化学合成法结合离子交换法制备了Cu修饰氮掺杂碳(Cu-N-C)和Fe/Cu修饰氮掺杂碳纳米管(Fe/Cu-N-C/CNT),并系统评估了2种催化剂作为染料敏化太阳能电池(dye-sensitized solar cells,DSSCs)对电极在I3-/I-体系中的电化学特性和光伏性能。采用X射线衍射(XRD)、拉曼(Raman)、X射线光电子能谱(XPS)和场发射扫描电镜(FESEM)对合成的催化剂进行组分和形貌表征。结果表明:纳米管状的Fe/Cu-N-C/CNT的石墨化程度比纳米颗粒状的Cu-N-C更高,更有利于I3-还原反应中电荷的传输。光伏性能测试结果表明:基于Fe/Cu-N-C/CNT对电极的DSSCs的光电能量转换效率(power conversion efficiency,PCE)达到7.55%,高于相同测试条件下Cu-N-C(6.99%)和Pt(6.76%)对电极的PCE。50圈连续循环伏安测试结果表明:Fe/Cu-N-C/CNT催化剂具有比Cu-N-C更好的电化学稳定性。 相似文献
35.
We developed a useful and preparative method based on high-speed counter-current chromatography with mass spectrometry (HSCCC/MS) to purify gentamicin C1a, C2/2a and C1 from standard powder. The analytes were purified on the HSCCC model CCC-1000 (multi-layer coil planet centrifuge) with a volatile two-phase solvent system composed of n-butanol/10% aqueous ammonia solution (50:50, v/v) and detected on an LCMS-2020EV quadrupole mass spectrometer fitted with an electrospray ionization (ESI) source system in positive ionization following scan mode (m/z 100-500). The HSCCC/ESI-MS peaks indicated that gentamicin C1a (m/z 450: [M+H](+)), C2/2a (m/z 464: [M+H](+)) and C1 (m/z 478: [M+H](+)) have the peak resolution values of 1.3 and 1.7 from 30 mg of loaded gentamicin powder. The HSCCC yielded 3.9 mg of gentamicin C1a, 12.6 mg of gentamicin C2/2a and 12.0 mg of gentamicin C1. These purified substances were analyzed by LC/MS with scan positive-mode. Based on the LC/MS chromatograms and spectra of the fractions, analytes were estimated to be over 95% pure. These gentamicin isomers of C1a, C2/2a and C1 were evaluated for their antibacterial activities. The overall results indicate that this approach of HSCCC/MS is a powerful technique for the purification of gentamicin components. 相似文献
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38.
在北京正负电子对撞机的J/ψ和Ds能区,选择了辐射巴巴事例,并以此来研究北京谱仪的桶部簇射计数器能量响应特性.在消除了由于电子和辐射光子在桶部簇射计数器中沉积能量区域重叠的影响后,正确地得到了桶部簇射计数器在电子和光子动量小于2GeV以下的能量响应,表明在所研究能区,桶部簇射计数器的能量响应线性很好.对桶部簇射计数器微小的非线性进行修正后,重建的π0不变质量谱得到改善. 相似文献
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Separation of five compounds from leaves of Andrographis paniculata (Burm. f.) Nees by off‐line two‐dimensional high‐speed counter‐current chromatography combined with gradient and recycling elution 下载免费PDF全文
Li Zhang Qi Liu Jingang Yu Hualiang Zeng Shujing Jiang Xiaoqing Chen 《Journal of separation science》2015,38(9):1476-1483
An off‐line two‐dimensional high‐speed counter‐current chromatography method combined with gradient and recycling elution mode was established to isolate terpenoids and flavones from the leaves of Andrographis paniculata (Burm. f.) Nees. By using the solvent systems composed of n‐hexane/ethyl acetate/methanol/water with different volume ratios, five compounds including roseooside, 5,4′‐dihydroxyflavonoid‐7‐O‐β‐d ‐pyranglucuronatebutylester, 7,8‐dimethoxy‐2′‐hydroxy‐5‐O‐β‐d ‐glucopyranosyloxyflavon, 14‐deoxyandrographiside, and andrographolide were successfully isolated. Purities of these isolated compounds were all over 95% as determined by high‐performance liquid chromatography. Their structures were identified by UV, mass spectrometry, and 1H NMR spectroscopy. It has been demonstrated that the combination of off‐line two‐dimensional high‐speed counter‐current chromatography with different elution modes is an efficient technique to isolate compounds from complex natural product extracts. 相似文献