含噻吩杂环Schiff碱及其配合物的合成与发光性质

在热乙醇中合成了2-乙酰基噻吩缩异烟酰肼及其与Cd(II)、Cu(II)和Zn(II)形成的三种配合物;利用元素分析、摩尔电导测定,以及红外光谱、紫外光谱和热分析确定了合成产物的组成和结构,并测定了配合物的组成及发光性质.结果表明,酰肼的配位方式的不同导致配合物呈现不同的发光性质.     

Synthesis and Antitumor Activity of 4-tert-Butyl-5-benzyl-2-benzyliminothiazoles

A series of novel Schiff bases including 4-tert-butyl-5-benzyl-2-benzyliminothiazoles was synthesized by reacting the aromatic aldehydes with the corresponding 2-aminothiazoles.The antitumor bioassay revealed that compounds 2n and 2m exhibited potent cytotoxicity against human cervix cancer（HeLa） cell line with IC50 values of 0.001 and 0.007 mmol/L,respectively.The preliminary structure-activity relationship（SAR） investigations and the apoptosis evaluation suggest that 4-tert-butyl-5-benzyl-2-benzyliminothiazoles may be a satisfactory backbone for antitumor activity,and compound 2n can serve as an attractive candidate for the development of novel apoptosis in anticancer treatment.     

Synthesis,Crystal Structure and Copper Complex of 1,3-Alternate p-tert-Butylthiacalix[4]arene 2-picolyl Schiff Base

A p-tert-butylthiacalix[4]arene-based polydentated ligand with four Schiff base units on 1,3-alternate position at lower rim has been prepared in three steps,which coordinated to copper ion to form a novel dicopper complex.The structures of the polydentated thiacalixarene ligand and copper complex were fully characterized by spectroscopy and X-ray single crystal diffraction method.     

Method development for compositional analysis of low molecular weight poly(vinyl acetate) by matrix-assisted/laser desorption-mass spectrometry and its application to analysis of chewing gum

The influence of the sample preparation parameters (the choice of the solvent and of the matrix:analyte ratio) was investigated and optimal conditions were established for MALDI mass spectrometry analysis of the pristine low molecular weight polyvinyl acetate (PVAc). It was demonstrated that comparison of polymer’s and solvent’s Hansen solubility parameters could be used as a guide when choosing the solvent for MALDI sample preparation. The highest intensity PVAc signals were obtained when ethyl acetate was used as a solvent along with the lowest matrix–analyte ratio (2,5-dihydroxybenzoic acid was used as a matrix in all experiments). The structure of the PVAc was established with high accuracy using the matrix-assisted laser desorption/ionization-Fourier transform mass spectrometry (MALDI-FTMS) analysis. It was demonstrated that PVAc undergoes unimolecular decomposition by losing acetic acid molecules from its backbone under the conditions of FTMS measurements. Number and weight average molecular weights as well as polydispersity indices were determined with both MALDI-TOF and MALDI-FTMS methods. The sample preparation protocol developed was applied to the analysis of a chewing gum and the molecular weight and structure of the polyvinyl acetate present in the sample were established. Thus, it was shown that optimized MALDI mass spectrometry could be used successfully for characterization of polyvinyl acetate in commercially available chewing gum.     

Trace analysis of uranyl ion (UO2) in aqueous solution by fluorescence turn-on detection via aggregation induced emission enhancement effect

A sensitive fluorescence turn-on method for trace amounts of uranyl ion (UO₂²⁺) in solution has been developed in this study, based on aggregation induced emission enhancement (AIEE) characteristics of 4-pethoxycarboxyl salicylaldehyde azine (PCSA) induced by complex interaction between UO₂²⁺ and PCSA. Under optimized conditions, a fluorescence enhancement at 540 nm could be observed, which was linearly related to the concentration of UO₂²⁺ in the range of 1–25 ppb (part per billion). Analytical data showed that a detection limit of 0.2 ppb was achieved with the relative standard deviation (R.S.D.) 1.3% (n = 5). The proposed method was successfully utilized in quantifying UO₂²⁺ in fuel processing wastewaters.     

Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma,enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization, significantly reduces the matrix effects and provides a great analytical tool for the isolation of small molecules from human plasma.     

Synthesis and spectrophotometric studies of water-soluble amino[bis(ethanesulfonate)] azobenzene pH indicators

Three azobenzene pH indicators with amino[bis(ethanesulfonate)] substituents were synthesized and studied by UV–visible absorption spectroscopy in aqueous solution. The indicators exhibit brilliant and distinct colour changes with transitions between pH 1 and 4. Significant changes were observed in the UV–visible spectra on titration with acid with pK_a values ranging from 2.2 to 2.8. The indicators demonstrate individual changes in colour as a function of pH. These novel pH indicators complement the existing library of azobenzene indicator dyes and may be useful for environmental situations with high proton concentrations.     

ZnO nanoparticles: a green efficient catalyst for the room temperature synthesis of biologically active 2-aryl-1,3-benzothiazole and 1,3-benzoxazole derivatives

A facile synthetic protocol for the synthesis of 2-aryl-1,3-benzothiazoles and 1,3-benzoxazoles has been demonstrated using ZnO nanoparticles as a mild and efficient heterogeneous catalyst. The reactions using ZnO nanoparticles were very fast (<8 min) and provided excellent yields (>90%) of the products. The catalyst was recycled and reused up to eight times without significant loss of catalytic activity. The potential application of 2-(4-hydroxyphenyl)-1,3-benzothiazole as new acid–base indicator has also been demonstrated in this Letter.     

Inhibitory study of some novel Schiff base derivatives on Staphylococcus aureus by microcalorimetry

The effect of a series of novel Schiff base compounds on Staphylococcus aureus was studied by microcalorimetric method at 37 °C The results showed that all of the organic compounds had the capacity to inhibit the growth of S. aureus in different extent. And the extent and duration of the inhibitory effect on the growth of S. aureus, judged from the rate constant (k), varied with the different structure of the Schiff base compounds. According to the power-time curves, the multiplication rate constant and inhibition ratio were calculated. The growth rate constant of S. aureus (in log phase) in the presence of Schiff base compounds decreased with the increasing of the concentrations of these compounds regularly. The experimental results revealed that the hydrophilicity of Schiff bases had a great influence on their antibacterial activity. Of these Schiff bases, the greater their hydrophilicity, the higher their antibacterial activity. The antibacterial structure-activity relationship (SAR) of Schiff base derivatives was also briefly discussed.