Estimation of binding constants between ristocetin and teicoplanin and peptides using on-column ligand derivatization coupled to affinity capillary electrophoresis

This work utilizes on-column ligand synthesis and affinity capillary electrophoresis (ACE) to determine binding constants (K_b) of 9-flourenylmethyloxy carbonyl (Fmoc)-amino acid derivatives to the glycopeptide antibiotics ristocetin (Rist) and teicoplanin (Teic). In this technique, two separate plugs of sample are injected on to the capillary column and electrophoresed. The initial sample plug contains a d-Ala-d-Ala terminus peptide and either one or two non-interacting standard(s). The second plug contains a Fmoc-amino acid-N-hydroxysuccinimide (NHS) ester. The electrophoresis is then carried out with an increasing concentration of Rist or Teic in the running buffer. Upon electrophoresis the initial d-Ala-d-Ala peptide reacts with the Fmoc-amino acid yielding a new Fmoc-amino acid-d-Ala-d-Ala peptide derivative. Continued electrophoresis results in the binding of Rist or Teic to the Fmoc-amino acid-d-Ala-d-Ala peptide derivatives. Analysis of the change in the relative migration time ratio (RMTR) or electrophoretic mobility () of the Fmoc-amino acid-d-Ala-d-Ala peptide derivatives relative to the non-interacting standards, as a function of the concentration of Rist and Teic, yields a value for K_b. These findings demonstrate the advantage of coupling on-column ligand synthesis to ACE for estimating binding parameters between antibiotics and ligands.Abbreviations Rist Ristocetin - Teic Teicoplanin - ACE Affinity capillary electrophoresis - RMTR Relative migration time ratio     

Chemical composition and antimicrobial activity of the essential oils of Ferula latisecta and Mozaffariania insignis from Iran

The hydrodistilled oils from the aerial parts of Ferula latisecta and Mozaffariania insignis, which is endemic to Iran, were analyzed by GC and GC/MS. (Z)-Ocimenone (32.4%), (E)-ocimenone (20.3%), and cis-pinocarvone (11.4%) were the main components among the 22 constituents characterized in the oil of F. latisecta, representing 87.7% of the total components detected. Twenty-five compounds were identified in the oil of M. insignis, representing 99.0% of the total oil, with octyl acetate (41.1%), β-pinene (30.3%), and α-pinene (23.9%) as the main constituents. The essential oils were examined for their potential antimicrobial activities. Published in Khimiya Prirodnykh Soedinenii, No. 6, pp. 561–563, November–December, 2006.     

Nitrogen doped nano porous graphene as a sorbent for separation and preconcentration trace amounts of Pb,Cd and Cr by Ultrasonic assisted in‐syringe dispersive micro solid phase extraction

Nitrogen doped nano porous graphene was used as an efficient sorbent in solid‐phase extraction process for simultaneous separation and pre‐concentration of metal ions lead (II), cadmium(II), and chromium(III)) in biological samples. Ultrasonic assisted in‐syringe dispersive micro solid phase extraction coupled with micro sampling atomic absorption spectrometry was utilized for the determination of metal ions. Nitrogen doped nano porous graphene was synthesized as a nano sorbent by chemical vapour deposition method. Methane and aniline were used as carbon and nitrogen sources. The characterization of sorbent was performed by field emission scanning electron microscope, transmission electron microscopy, atomic force microscope, fourier transform infrared, chemical element analysis and raman analysis. Effective parameters on the extraction efficiency such as pH, sorbent dosage, eluent volume and eluent concentration were optimized by central composite design and desirability function. Experimental results indicate that the optimal conditions for this extraction were pH = 6.4, 1.42 mg of sorbent, 100 μL of eluent, and 0.84 mol L^‐1 of eluent concentration. The detection limits are as low as 1.5, 0.3 and 0.9 μg L^‐1 for lead, cadmium, and chromium, respectively. The intra‐day precisions were 3.6, 4.38 and 2.94 and Inter‐day precision were 4.83, 5.26 and 4.52 for lead, cadmium, and chromium, respectively. Method performance was investigated by determination of mentioned heavy metals in complicated biological matrixes such as human plasma, urine and saliva samples with good recoveries.     

A hyperbranched polyamidoamine dendrimer grafted onto magnetized graphene oxide as a sorbent for the extraction of synthetic dyes from foodstuff

Microchimica Acta - Graphene oxide nanosheets were modified with magnetite nanoparticles, and a hyperbranched polyamidoamine dendrimer was then covalently attached to their surface. The resulting...     

Low Temperature Preparation of 3D Solid and Hollow ZnS Nanosphere Self-Assembled from Nanoparticles by Varying Sulfur Source

In this work, we report a facile hydrothermal method for the preparation of three dimensional hollow ZnS nanostructures, using Zinc bis(salicyle aldehitato), Zn(Sal)₂, thioacetamide (TAA) and thioglycolic acid (TGA) as Zn²⁺, sulfur source and capping agent, respectively. The ZnS solid and hollow sphere was produced from the self-assembly of nanoparticles with diameters of 11 ± 2 nm with TGA and TGA, TAA, respectively. Furthermore, with changing zinc precursor from Zn(Sal)₂ to zinc acetate [Zn(OAC)₂], ZnS nanorods were obtained. The products were characterized by XRD, SEM, TEM, selected area electron diffraction, and FT-IR spectra. The influence of surfactant (Polyethylene glycol) on the morphology of the products was also investigated. Possible formation mechanism and optical properties of these architectures were also reported.     

2‐hydroxyethylammonium formate ionic liquid grafted magnetic nanoparticle as a novel heterogeneous catalyst for the synthesis of substituted imidazoles

Catalytic one‐pot condensation of benzil, aldehyde and ammonium acetate have been successfully carried out using 2‐hydroxyethylammonium formate (HEAF) grafted on a magnetic nanoparticles as a new heterogeneous catalyst. The as‐prepared catalyst was characterized by FT‐IR, TEM, FESEM, VSM, TGA and XRD. This catalyst indicated significant advantages, such as excellent yields, shorter reaction time, reusability of the catalyst and easy workup process.     

Magnetic‐based picolinaldehyde–melamine copper complex for the one‐pot synthesis of hexahydroquinolines via Hantzsch four‐component reactions

A picolinaldehyde–melamine copper complex was loaded on a magnetic Fe₃O₄ core, so that it contained 0.33 mmol of Cu per gram, and was used as an efficient catalyst. The as‐synthesized catalyst was characterized using various techniques, including Fourier transform infrared spectroscopy, X‐ray diffraction, energy‐dispersive X‐ray spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometry and thermogravimetric analysis. The catalyst was used to activate the raw materials in the synthesis of hexahydroquinoline derivatives in one‐pot four‐component reactions. Low reaction time (minutes versus half an hour), solvent‐free condition and magnetically separable catalyst are some salient features of the developed catalyst. Also, the optimum amount of catalyst and temperature were determined as 0.07 g and 87.6 °C, respectively, which were obtained using response surface methodology and optimization techniques.