| 2 | Potential of capillary electrophoresis mass spectrometry for the characterization and monitoring of amine-derivatized naphthenic acids from oil sands process-affected water显示文摘Capillary electrophoresis coupled to mass spectrometry(CE–MS) was used for the analysis of naphthenic acid fraction compounds(NAFCs) of oil sands process-affected water(OSPW). A standard mixture of amine-derivatized naphthenic acids is injected directly onto the CE column and analyzed by CE–MS in less than 15 min. Time of flight MS analysis(TOFMS), optimized for high molecular weight ions, showed NAFCs between 250 and 800 m/z. With a quadrupole mass analyzer, only low-molecular weight NAFCs(between 100 and 450 m/z) are visible under our experimental conditions. Derivatization of NAFCs consisted of two-step amidation reactions mediated by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide(EDC), or mediated by a mixture of EDC and N-hydroxysuccinimide, in dimethyl sulfoxide, dichloromethane or ethyl acetate. The optimum background electrolyte composition was determined to be 30%(V/V) methanol in water and 2%(V/V) formic acid. NAFCs extracted from OSPW in the Athabasca oil sands region were used to demonstrate the feasibility of CE–MS for the analysis of NAFCs in environmental samples, showing that the labeled naphthenic acids are in the mass range of 350 to 1500 m/z. | Matthew S.MacLennan Cai Tie Kevin Kovalchik Kerry M.Peru Xinxiang Zhang John V.Headley David D.Y.Chen | 2016 | Journal of Environmental Sciences2016，28，11： | 2 |
| 3 | 毛细管电泳结合电喷雾质谱分析人类癌基因c-myb四链体核酸与活性天然产物的相互作用显示文摘药物与靶点间的作用关系直接影响到药理和药效。药物-靶点结合能力、结合计量关系等信息是药物研发过程中必需的表征数据。人类癌基因c-myb在结直肠癌等多种癌症组织中存在过度表达,目前已成为结直肠癌、白血病等癌症疾病潜在的治疗靶点。位于癌基因c-myb启动子区的一段富含鸟嘌呤(G)的DNA序列,通过阳离子的诱导可自发折叠形成分子内G-四链体,而小分子的特异性识别可以稳定该G-四链体,进而调节基因的转录和表达过程。该文采用压力辅助毛细管电泳前沿分析(PACE-FA)结合电喷雾质谱(ESI-MS)研究人类癌基因c-myb启动子G-四链体(G4)与天然产物分子间的相互作用。PACE-FA法在毛细管电泳前沿分析(CE-FA)过程中施加一个与分析物迁移同向的压力,在保证结果准确度的前提下,能够大大加快分析速度。同时结合ESI-MS,可快速解析结合分子与靶点的亲合力和化学计量关系。首先,利用ESI-MS快速筛选出3种有亲合力的天然产物,亲合力大小依次为:土荆皮乙酸>丁溴东莨菪碱>荷叶碱。考虑到溶液相中存在特异性与非特异性结合,接着用PACE-FA法准确分析溶液相中结合的特异性和结合常数。结果发现:丁溴东莨菪碱能够特异性结合靶点G4 DNA,结合比为1∶1,结合常数为1.18×10^5 L/mol;荷叶碱属于非特异性结合,而土荆皮乙酸并未与靶点G4 DNA形成复合物。该组合方法不仅分析速度快,而且能够提高亲和分析的准确度和特异性,有望应用于靶向药物先导结构的发现和作用机制评价。 | 王双双 杨云鹤 凡珊珊 李卉卉 David D.Y.CHEN | 2020 | 色谱2020，38，9： | 1 |
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