Cholesterol-based hydrogen-bonded liquid crystals

Hydrogen bonding is a powerful tool for assembling molecules and building new liquid crystalline structures. In this study, non-symmetric dimesogens were prepared by intermolecular hydrogen bonding between rationally designed H-bond donor (3-cholesteryloxycarbonylpentanoic acid) and acceptor (4-(pyridine-4-ylmethyleneimino)phenyl 4-alkoxybenzoate) moieties. Their liquid crystalline properties were investigated by differential scanning calorimetry, polarized optical microscopy and X-ray diffraction. Cholesteric and smectic phases were observed. As for the covalently linked dimesogens, several types of smectic periodicities occur for these H-bonded cholesteryl compounds depending on the molecular parameters.     

Designed nanostructured pt film for electrocatalytic activities by underpotential deposition combined chemical replacement techniques

Multiple-deposited Pt overlayer modified Pt nanoparticle (MD-Pt overlayer/PtNPs) films were deliberately constructed on glassy carbon electrodes through alternately multiple underpotential deposition (UPD) of Ag followed redox replacement reaction by Pt (II) cations. The linear and regular growth of the films characterized by cyclic voltammetry was observed. Atomic force spectroscopy (AFM) provides the surface morphology of the nanostructured Pt films. Rotating disk electrode (RDE) voltammetry and rotating ring-disk electrode (RRDE) voltammetry demonstrate that the MD-Pt overlayer/PtNPs films can catalyze an almost four-electron reduction of O(2) to H(2)O in air-saturated 0.1 M H(2)SO(4). Thus-prepared Pt films behave as novel nanostructured electrocatalysts for dioxygen reduction and hydrogen evolution reaction (HER) with enhanced electrocatalytic activities, in terms of both reduction peak potential and peak current, when compared to that of the bulk polycrystalline Pt electrode. Additionally, it is noted that after multiple replacement cycles, the electrocatalytic activities improved remarkably, although the increased amount of Pt is very low in comparison to that of pre-modified PtNPs due to the intrinsic feature of the UPD-redox replacement technique. In other words, the electrocatalytic activities could be improved markedly without using very much Pt by the technique of tailoring the catalytic surface. These features may provide an interesting way to produce Pt catalysts with a reliable catalytic performance as well as a reduction in cost.     

Determination of Dextromethorphan and its Metabolite Dextrorphan in Human Hair by Gas Chromatography–Mass Spectrometry

An analytical method has been developed for determination of dextromethorphan (DMP) and dextrorphan (DRP) in human hair by gas chromatography–mass spectrometry (GC–MS). Hair samples (30 mg) were washed with distilled water and acetone and cut into small fragments (<1 mm) before extraction with methanol. The extracts were evaporated to dryness and then derivatized by use of BSTFA containing 1% TMCS, for preparation of the trimethylsilyl (TMS) derivative of DRP. The extract (1 μL) was then injected into the GC–MS. Recoveries of DMP and DRP at 7.0 and 22.5 ng mg^?1 were in the range 90.6–97.2% with intra-assay and inter-assay precision of less than 5.7% and 4.7%, respectively. LOD and LOQ were, respectively, 0.67 and 2.13 ng mg^?1 for DMP and 0.14 and 0.47 ng mg^?1 for DRP. The responses were linear with correlation coefficients (r > 0.9995) for the drugs studied. The applicability of the method was proven by analysis of authentic hair samples.     

Transfer Hydrogenation of C= C Double Bonds Catalyzed by Ruthenium Amido-Complexes: Scopes, Limitation and Enantioselectivity

The reduction of C = C double bonds is one of the most fundamental synthetic transformations and plays a key role in the manufacturing of a wide variety of bulk and fine chemicals. Hydrogenation of olefinic substrates can be achieved readily with molecular hydrogen in many cases, but transfer hydrogenation methods using suitable donor molecules such as formic acid or alcohols are receiving increasing attention as possible synthetic alternatives because it requires no special equipment and avoids the handling of potentially hazardous gaseous hydrogen.     

铈杂多配离子-水滑石超分子层柱材料ZnAl-Ce(PMoV)2的插层组装、表征及催化性能

以十四酸根阴离子柱撑Zn-Al水滑石Zn0.77Al0.22(OH)2.0.22C13H27COO.0.81 H2O(记为ZnAl-14A)为预撑前体,在水溶液中用离子交换法将以2∶17缺位杂多酸根离子(P2Mo16VO61)11-记为(P Mo V)为配体的稀土杂多配阴离子Ce(P2Mo16VO61)219-(记为Ce(PMoV)2)插层组装到水滑石层板间,合成了一种具有大的层间距(3.37 nm)的超分子插层材料Zn0.77Al0.23(OH)2.0.0105[Ce(P1.9Mo15.7V1.1O61)2].0.011C13H27COO.0.83H2O(记为ZnAl-Ce(PMoV)2)。用ICP,IR,XRD和DTA对产物的组成和结构进行了表征。结果表明,该产物中Ce(PMoV)2配阴离子沿其长轴垂直于层板的方向分布于水滑石层间;产物具有规整的层状结构和热稳定性;产物对乙酸与正丁醇的酯化反应,二甘醇的脱水-环化反应和H2O2氧化环己烷的反应有良好的催化性能,且易于回收重复使用。     

PVC功能膜固相透射光度法测定钯

提出了用PVC功能膜固相透射吸光光度法测定钯的方法。研究发现 ,在pH 3～ 4HOAc NaOAc介质中 ,钯与均匀分布在PVC功能膜上的硫代米氏酮形成疏水性的配合物 ,在自制的固相透射分光光度附件上测定。在 5 2 0nm波长处具有最大吸收 ,钯浓度在 0～ 7.5 μg 10ml范围内 ,A与C有良好的线性关系 ,检出限为 0 .0 15 μg·ml-1,标准偏差为 0 .78%。方法简便、快速、试剂用量少 ,可直接用于矿样中钯的测定     

Study on analysis of153Sm-EDTMP stability in vitro and vivo by HPLC

The behavior of¹⁵³Sm-EDTMP in vitro and vivo is analyzed by the size exclusion HPLC. The experimental results show that EDTMP amounts have an obvious effect on the stability in vitro and uptake of¹⁵³Sm-EDTMP in the liver. HPLC analysis of urine sample indicates that¹⁵³Sm-EDTMP es excreted in the original form. The behavior in vivo of¹⁵³Sm-EDTMP containing 4 μg is similar to that of¹⁵³Sm-EDTMP containing 50 μg EDTMP at 1 h post-injection.     

Hydroxylation of nigranoic acid to 6β-hydroxynigranoic acid by Caryospora carllicarpa YMF1.01026

Microbial transformation of nigranoic acid by Caryospora carllicarpa YMF1.01026 afforded the new derivative 6β-hydro-xynigranoic acid. Its structure was elucidated by spectroscopic methods.