A new method for the quantitative analysis of organochlorine pesticides and polychlorinated biphenyls

A simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub-ppb level. A micro gas-phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation-extraction, and capillary gas chromatographic analysis is carried out in less than four hours.     

The inhomogeneous electron liquid in some bioinorganic assemblies studied by density functional methods

The review starts with a discussion of some recent advances related to the foundations of density functional theory (DFT). Some emphasis is placed on methods which should have special relevance to bioinorganic assemblies. In particular, the inhomogeneous electron liquid in the ground state of such systems is a specific focal point. After a brief summary concerning the possible variational validity of some popular energy functionals, the future value of the important Dirac idempotent density matrix is emphasised, both from first principles and semiempirically by making use of X-ray diffraction experiments. The review concludes with two topical examples of bioinorganic assemblies. The first concerns our own work on an anticancer drug based on a Ru complex, while as a second example a recent DFT study of a molecular biosensor by K. Salazar-Salinas, L.A. Jauregui, C. Kubli-Garfias, J.M. Seminario [J. Chem. Phys. 130, 105101 (2009)] involving an Fe complex is briefly summarised.     

多波段微量TNT成像探测的数值分析和实验研究

建立了CO2激光器辐照微量爆炸物温升分布三维模型,对激光辐照过程和冷却过程中8~14μm和3~5μm波段内的目标表面辐射温度变化特性分别进行分析.利用设计的探测系统对目标进行初步探测,用8~14μm和3~5μm热像设备对目标进行观察分析.研究表明:在10.6μm激光照射过程中,8~14μm波段内沾有TNT目标的辐射温度分别由TNT、基底在8~14μm波段的发射率和对激光辐照的反射率共同决定;在3~5μm内目标辐射温度主要由TNT、基底在3~5μm波段的自身发射率决定.在探测过程中,8~14μm波段内沾染TNT区域的辐射温度明显高于周围区域,而在3~5μm波段内,目标表面辐射温度整体下降,并且沾染区域的辐射温度变得低于周围.     

Optimization of Verapamil Drug Analysis by Excitation-Emission Fluorescence in Combination with Second-order Multivariate Calibration

Excitation emission fluorescence matrices (EEMs) of Verapamil drug were obtained by direct and by derivatization fluorescence spectroscopy. The fluorescence excitation and emission wavelengths were displaced to longer wavelengths and the fluorescence intensity was enhanced upon derivation with respect to the native fluorescence of the drug. The complete EEM of the native fluorescence of the drug and of the derivatization product were rapidly acquired by using a charged-coupled device detector (CCD), which is advantageous in terms of speed in the analysis, with respect to the use of a conventional photomultiplier detector. The EEMs were analyzed by several second-order multivariate calibration methods exploiting the second order advantage. The three-dimensional decomposition methods used, based in different assumptions about the trilinearity of the three way data structure under analysis, were parallel factor analysis (PARAFAC), bilinear least squares (BLLS), parallel factor analysis 2 (PARAFAC2) and multivariate curve resolution—alternating least squares (MCR-ALS). The determination was performed by using the standard addition approach. The figures of merit of the PARAFAC and BLLS methods were calculated, obtaining a lower limit of detection with the derivatization procedure, when compared with the direct measurement of the fluorescence of the drug. In Verapamil drug the best estimations were found with the BLLS and the MCR-ALS models. In the quantification of Verapamil in a pharmaceutical formulation the best estimation, when compared with the result obtained by the US Pharmacopeia high performance liquid chromatography approach, was obtained by direct fluorescence spectroscopy with MCR-ALS and by derivatization fluorescence spectroscopy with the PARAFAC2 model.     

An in vitro controlled release study of valproic acid encapsulated in a titania ceramic matrix

Despite the therapeutic efficacy of valproic acid towards numerous diseases, its poor bioavailability and systemic side effects pose significant barriers to long term treatment. In order to take advantage of controlled release implants of valproic acid, the drug was encapsulated into titania ceramic matrices via a sol-gel process. The integrity and structure of valproic acid-containing matrices were characterized through the use of FESEM, TEM, and BET analyses. In vitro controlled release studies and kinetic analyses were performed under ambient conditions (25 °C, atmospheric pressure) and controlled release behaviors were studied using a GC-MS method. Results showed first order dependence in the rate of valproic acid release as a function of drug concentrations in the titania ceramic device. A marked dependence on the surface area and pore size distribution with drug loading was also observed. This research opens new possibilities for the design of novel time-delayed controlled release systems for valproic acid encapsulates.     

ANALYSIS OF MEBENDAZOLE POLYMORPHS BY FOURIER TRANSFORM INFRARED SPECTROMETRY USING CHEMOMETRIC METHODS

A Fourier transform infrared (FT-IR) spectrometric method diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) was developed for the rapid, direct measurement of mebendazole in drugs. Conventional KBr-spectra and DRIFTS-spectra were compared for best determination of active substance in drug formulations. Two chemometric approaches, partial least-squares (PLS2) and principal component regression (PCR+) methods were used in data procesing. The best results were obtained with the PLS2 method.     

Identification of functionally key residues in maltose transporter with an elastic network model-based thermodynamic method

Periplasmic binding protein-dependent maltose transport system (MBP-MalFGK₂) of Escherichia coli, an important member of the Adenosine triphosphate-binding cassette transporter superfamily, is in charge of the transportation of maltoses across cellular membrane. Studies have shown that this transport processes are activated by the binding of maltose and are accompanied by large-scale cooperative movements between different domains which are mediated by a network of important residues related to signal transduction and allosteric regulation. In this paper, the functionally crucial residues and long-range allosteric pathway of the regulation of the system by substrate were identified by utilising a coarse-grained thermodynamic method proposed by our group. The residues whose perturbations markedly change the binding free energy between maltoses and MBP-MalFGK₂ were considered to be key residues. In result, the key residues in 62 clusters distributed in different subdomains were identified successfully, and the results from our calculation are highly consistent with experimental and theoretical observations. Furthermore, we explored the long-range cooperation within the transporter. These studies will help us better understand the physical mechanism of the effects of the maltose on MBP-MalFGK₂ by long-range allosteric modulation.     

Preparation and characterization of biodegradable magnetic carriers by single emulsion-solvent evaporation

This paper describes a single emulsion-solvent evaporation protocol to prepare PEGylated biodegradable/biocompatible magnetic carriers by utilizing hydrophobic magnetite and a mixture of poly(D,L lactide-co-glycolide) (PLGA) and poly(lactic acid-block-polyethylene glycol) (PLA-PEG) (26:1 by mass) polymers. We characterized the magnetic microspheres in terms of morphology, composite microstructure, size and size distribution, and magnetic properties. Results show that the preparation produces magnetic microspheres with a good spherical morphology, small size (mean diameter of 1.2–1.5 μm) by means of large size distributions, and magnetizations up to 20–30 emu/g of microspheres.     

Intra-arterial application of magnetic nanoparticles for targeted thrombolytic therapy: A rat embolic model

Targeted delivery of thrombolytic drug to the site of emboli exhibits potential to greatly reduce hemorrhagic side effect. A rat embolic model with an easy access of a magnet was established for study of the efficacy of magnetic drug targeting. In anesthetized rats, a whole blood clot produced in vitro was injected from the right iliac artery and lodged in the left iliac artery. Intra-arterial infusion of recombinant tissue plasminogen activator (rt-PA) thereafter significantly reversed the iliac flow within 15 min. Placement of an NdFeB magnet above the left iliac artery caused magnetic nanoparticle retention against hemodynamic dragging force in the presence and absence of the clot. Our results suggest the feasibility of this rat embolic model for the study of magnetic targeted delivery of thrombolytic drugs.