吡咯甲亚胺镍/铜/锌配合物的合成、荧光性质及镍、铜配合物的晶体结构

合成并表征了3个配合物NiL (1),Cu₂L₂ (2)和Zn₂L₂ (3)(H₂L=1,2-双(3,5-二甲基-4-乙氧羰基-吡咯-2-基)苯).单晶衍射结果表明在配合物1中,脱质子配体用4个氮原子与金属NiⅡ配位,中心金属离子为扭曲的平面正方形配位构型.而双核配合物2拥有双螺旋结构,每个配体桥联2个具有平面正方形配位构型的铜中心.推测配合物3和2的结构类似.此外还研究了配体和配合物的荧光性质.     

Three New Anthraquinones from Polygonum cillinerve

Three new anthraquinones, emodin-8-β-D-（2＂-O-coumarate）glucoside 1, emodin-8-β-D-（6＇-O-acetyl）glucoside 2 and physicon-8-β-D-（6＇-O-acetyl）glucoside 3, were isolated from the roots of Polygonum cillinerve and their structures were established by spectroscopic methods. The biological activity indicated that compound 1 had the scavenging activity on 1,1-diphenyl-2-picrylhydrazyl （DPPH） radicals （the IC50 = 8.5 μmol/L）, and compound 1-3 showed no activities against HL-60 and BCJC-823 cells by MTT method in vitro.     

凹凸棒土应用于水样中铜和铅测定的研究

本文以凹凸棒土为固相萃取剂,与火焰原子吸收光谱(FAAS)法联用,富集并检测样品中的痕量金属离子。研究了凹凸棒土对痕量Cu(Ⅱ)和Pb(Ⅱ)的吸附作用,考察了吸附时间、凹凸棒土加入量等影响其吸附和解吸的主要因素、并考察了静态饱和吸附容量,及共存离子的影响。结果表明,当pH 6.0、凹凸棒土用量为0.25 g时,凹凸棒土对Cu(Ⅱ)和Pb(Ⅱ)的吸附率达到90.3%和92.1%;用20 mL 0.1 mol.L-1的HNO3可将吸附在凹凸棒土上的Cu(Ⅱ)和Pb(Ⅱ)定量洗脱。凹凸棒土对Cu(Ⅱ)和Pb(Ⅱ)的静态饱和吸附容量分别为15.8 mg.g-1、23.7 mg.g-1;本法对Cu(Ⅱ)和Pb(Ⅱ)的检出限分别为2.80μg.L-1、0.25μg.L-1;相对标准偏差分别为1.9%和2.1%(Cu(Ⅱ)、Pb(Ⅱ):0.40μg.mL-1,n=5)。在优化的实验条件下,实测了水样中Cu(Ⅱ)和Pb(Ⅱ)的含量,加标回收率均在96%～105%之间,结果令人满意。     

Convenient Synthesis of 3,5‐Biscarbamoyl‐pyridine Derivatives

An efficient and convenient method for synthesis of 3,5‐bis‐carbamoyl‐2,6‐dimethylpyridine derivatives was achieved in good to excellent yields by reaction of anilines with 3,5‐bis(3′,5′‐dimethyl‐1′‐pyrazolyl‐carbonyl)‐2,6‐dimethylpyridine, in which pyrazoles served as leaving groups. The structures of products were confirmed by spectra data and microanalysis.     

An ionic liquid-based sorbent for solid phase extraction of trace iron(Ш) from biological and natural water samples

A new ionic liquid modified silica gel sorbent was prepared from the reaction of active silica gel with N-3-(-3-triethoxysilylepropyl)-3-methylimidazolium chloride ([(TESP)MIm]Cl). This sorbent was exploited as solid phase extractant for separation and preconcentration of metal ions prior to their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). It was found that it can selectively adsorb Fe(Ш). Identification of the surface modification was performed on the basis of FT-IR. Experimental conditions for effective adsorption of trace Fe(Ш) were optimised using both batch and column procedures. At pH 3, Fe(Ш) could be quantitatively adsorbed and completely eluted by using 2?mL of 0.1?mol?L^?1 of HCl. 150?mL of sample solution was adopted as the maximum sample volume and a high enrichment factor of 75 was obtained. Most common coexisting ions did not interfere with the separation and preconcentration of Fe(Ш) at optimal conditions. The maximum static adsorption capacity of the sorbent was 37.0?mg?g^?1. The detection limit of the present method was 0.48?µg?L^?1, and the relative standard deviation (R. S. D.) was lower than 1.7%. The method was successfully applied to the preconcentration of trace Fe(Ш) in biological and natural water samples with satisfactory results.     

Anisotropic Nanoparticles with Controllable Morphologies from Non‐Cross‐Linked Seeded Emulsion Polymerization

A simple and elegant approach to fabricate anisotropic P(VC‐co‐AAEM)/PS nanoparticles with controllable morphologies via emulsifier‐free seeded emulsion polymerization is presented. Non‐cross‐linked P(VC‐co‐AAEM) seeds with hydrophilic surface are first synthesized through copolymerization of vinyl chloride (VC) and acetoacetoxyethyl methacrylate (AAEM), which are used to prepare P(VC‐co‐AAEM)/PS NPs with multiple bulges by SEP of styrene. Electron microscopy observation indicates that the content of AAEM in seeds is crucial to control the phase separation and morphology of the composite NPs. Moreover, the thermodynamic immiscibility between PVC and PS is the driving force for the formation of PS bulges onto the P(VC‐co‐AAEM) seeds. The resultant anisotropic NPs with non‐cross‐linked feature may promisingly serve as compatibilizers for further polymer processing.

     

How Graphene Oxide Quenches Fluorescence of Rhodamine 6G

We investigate the fluorescence quenching of Rhodamine 6G (R6G), a well known laser dye with a high fluorescence quantum yield, by as-synthesized graphene oxide (GO) in aqueous solution, which is found to be rather efficient. By means of steady-state and time-resolved fluorescence spectroscopy combined with detailed analysis about the linear absorption variation for this R6G-GO system, the pertinent quenching mechanism has been elucidated to be a combination of dynamic and static quenching. Possible ground-state complexes between R6G and GO during the static quenching have also been suggested. Furthermore, the direction of photoinduced electron transfer between R6G and GO has been discussed.     

Intramolecular Aldol Condensation ofα- Oxo Ketene Dibenzylthioacetals: A Facile Route to Substituted Thiophenes

As a kind of intermediates, a-oxo ketene dithioacetals I are important in organicsynthesis"'. In our recent studies, we found that the difference of dialkythio group canbestow various properties on these kinds of compounds"'. To exploit the reactivityadjusted by the dialkythio groups in l, a-oxo ketene dibenzylthioacetals 2 were chosenand studied. Some interesting new results were obtained in these experiments. Here wereport the new results.When studying the reaction of a-oxo ketene dibenzylt…     

咪唑基手性硫醚衍生物的合成与表征

硫及氮、磷、氧等原子能够与大多数过渡金属络合形成多齿的螯合物.手性的硫醚钯络合物常用于不对称碳碳键的形成、不对称的Diels-Alder、Hetero-Diels-Alder环加成、Heck反应以及羰基的加成反应中,很多手性配合物都表现出良好的手性诱导效果.     

基于纳米金比色检测NOS1AP基因单碱基突变

基于单、双链DNA与纳米金颗粒间的不同静电作用, 建立了一种基于颜色反应检测NOS1AP基因单碱基突变的方法. 根据NOS1AP基因的单碱基多态位点设计检测探针、互补靶序列及带有单碱基突变序列寡核苷酸DNA. 室温下, 检测探针分别与互补序列、单碱基突变序列在缓冲液中进行杂交, 再分别加入纳米金溶液以及NaCl溶液. 用肉眼可以观察到纳米金溶液在两种不同杂交溶液中产生明显不同的颜色变化. 这种变化可通过紫外-可见分光光度计测定纳米金溶液的紫外吸收峰值的变化来证实. 实验结果表明, 纳米金溶液在一定浓度NaCl存在的条件下, 对互补双链NOS1AP DNA及单碱基突变NOS1AP DNA呈现出不同的颜色反应及紫外吸收光谱的改变. 此方法可望用于相关疾病的医学诊断及单碱基突变的检测.