用C60键合硅胶固定相液相色谱分离杯芳烃及杯芳冠醚类化合物

以自合成的C60 键合硅胶液相色谱固定相 ,分别选用3种不同选择性的流动相体系 :异丙醇 -环己烷 ,氯仿 -环己烷和二氯甲烷 -环己烷 ,考察了流动相组成对杯芳烃及杯芳冠醚化合物保留行为和分离选择性的影响。在一定的流动相条件下溶质能得到较好分离。     

Synthesis, structures, and spectral properties of biomimetic azomethine metal chelates with chromophores CuN2S2, CuN2O2, and CuN2Se2. Crystal structure of bis[4-(benzyl)aldimino-3-methyl-1-phenyl-5-pyrazolothiolato]copper(II)

Copper(II) chelates of composition CuL₂ were synthesized based on 4-aminomethylene derivatives of 5-thiopyrazoles (LH). The complexes were studied by UV, IR, ESR, and EXAFS spectroscopy, magnetochemistry, and X-ray diffraction analysis. The coordination polyhedra in the complexes are pseudotetrahedra or octahedra of the types CuN₂S₂ or CuN₄S₂, respectively, which are distorted due to the Jahn—Teller effect. The UV and ESR spectra of copper chelates with a six-coordinate metallocycle formed by the N and S atoms of the azomethine ligand and the nitrogen atom of the quinoline substituent (R) of the C=N−R fragment are most similar to the spectra observed for metals involved in the active centers of natural metalloenzymes (“blue” copper proteins). Published inIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 1891–1896, November, 2000.     

光活性[1]1-联萘酚(BINOL)的不对称合成

由于 1 ,1 -联萘酚 ( BINOL)可作为手性配体或手性催化剂的前体 ,在不对称合成反应中具有广泛的应用 [1,2 ] ,所以如何得到光学纯的 BINOL的研究吸引了许多化学家的注意 .制备光学活性的 BINOL的方法较多 ,但一般效果较好的是用拆分的方法[3,4] .通过 2 -萘酚不对称氧化偶联直接得到 BINOL的方法也有许多报道 [5 ,6 ] ,但结果都不理想 .近来 ,Kocovsky等 [7]用鹰爪金碱作为手性诱导试剂 ,在Cu Cl2 存在下 ,2 -萘酚偶联得 BINOL,其 ee值为 1 0 0 % ,但产率只有 1 4% ,且由于鹰爪金碱价格昂贵 ,限制了该法的应用 .在此基础上 ,我…     

锆镁磷脂膜色谱固定相的制备及其在评价药物-膜相互作用中的应用

基于锆基质与磷脂之间强烈的路易斯酸碱作用,制备了锆镁磷脂膜色谱固定相,并使用红外光谱、X射线光电子能谱对该色谱固定相进行了表征;使用与体内环境类似的生理缓冲液体系为流动相,评价了该模拟生物膜色谱固定相预测药物膜渗透性的能力,结果表明药物在锆镁磷脂膜色谱中的保留(log Kmbm)与表观渗透率(log Papp)在预测药物的膜渗透性、跨膜吸收等方面具有非常好的相关性,相关系数为0.970,斜率接近1。通过理论推导,引入了直观、方便的热力学指标吉布斯自由能差值（Δ(ΔG°)）对药物-膜之间的相互作用强弱进行了评价。     

脱叔丁基杯[8]芳烃键合固定相的制备及其液相色谱性能

杯芳烃(Cahixarenes)是一类由苯酚单元经亚甲基相连而成的大环化合物,与β-环糊精类似,它能与多种溶质形成主客体包容配合物,并通过超分子作用识别离子和中性分子等客体,利用杯芳烃的分子识别作用可提高色谱分离性能,Glennon等制备了酯化杯[4,6]芳烃键合固定相,     

光声喇曼光谱的理论分析

对光声喇曼光谱(PARS)作了系统的理论分析,分别导出固体和液体介质中的光声喇曼光谱的信号表达式,并进行了数值估算。 关键词：     

Solvent and concentration effects on the properties of electrospun poly(ethylene terephthalate) nanofiber mats

This study describes the preparation and characterization of nanofibrous mats obtained by electrospinning poly(ethylene terephthalate) (PET) solutions in trifluoroacetic acid/dichloromethane (TFA/DCM). Special attention was paid to the effect of polymer concentration and solvent properties on the morphology, structure, and mechanical and thermal properties of the electrospun nonwovens. The results show that the spinnable concentration of PET solution in TFA/DCM solvents is above 10 wt %. Mats have nanofibrous morphology with fibers having an average diameter in the range of 200–700 nm (depending on polymer concentration and solvent composition) and an interconnected pore structure. Higher solution concentration favors the formation of uniform fibers without beads and with higher diameter. Morphology and fiber assembly changed with the solvent properties. Solvent mixtures rich in TFA, i.e., those with higher dielectric constant and lower surface tension, originated fibers with small diameter. However, due to the lower volatility, those solvent mixtures also produced more branched and crosslinking fibers, with less morphologic uniformity. Mechanical properties (Young's modulus, ultimate strength, and elongation at break) and thermal properties (glass transition, crystallization, and melting) have been studied for the PET electrospun nanomats and compared with those of the original polymer. Solvent effect on fiber crystallinity was not significant, but a complex effect was observed on the mechanical properties of the electrospun mats, as a consequence of the different structural organization of the fibers within the mat network. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 460–471, 2008     

Luminescent complexes with ligands containing C=N bond

Data on luminescent complexes with azomethine ligands are generalized and systematized. The synthesis and luminescent properties of complexes with acyclic and cyclic azomethines are considered.