Use of modifiers in on-line and off-line supercritical fluid extraction

For many applications using supercritical fluid extraction (SFE), modifiers may be required.This paper will present some findings regarding the use of various modifiers including methanol, hexane, acetone, chloroform, dichloromethane, toluene, and tributylphosphate, in on-line and off-line SFE with cryogenic adsorbent trapping. The specific applications involved the extractions of petroleum hydrocarbons and pesticides from naturally incurred soils.     

Thermal behavior of some N,N-dimethylbiguanide derivatives displaying antimicrobial activity

N,N-Dimethylbiguanide derivatives (HDMBG)X, where X=CH₃COO (1), Cl (2) and NO₃ (3) respectively, exhibit in vitro antimicrobial activity on representative bacterial and fungal strains. The presence of N,N-dimethylbiguanidium ion for all derivatives was evidenced by IR and ¹H NMR spectra. Thermal analysis gave information on their decomposition steps and also on the accompanying thermodynamic effects. According to TG and DTG curves processes as melting, oxidative degradation as well as oxidative condensation of –C=N– units occur. The different nature of the anions results different melting points. Paracyanide formation at various condensation degrees was observed.     

Analysis of Mammalian Cell Cytoplasm with Electrophoresis in Nanometer Inner Diameter Capillaries

Capillary electrophoresis in 770 nanometer inner diameter capillaries coupled to electrochemical detection with an etched electrode matching an etched capillary (etched electrochemical detection) has been used with ultrasmall sampling to inject subcellular samples from intact single mammalian cells. Separations of cytoplasmic samples taken from rat pheochromocytoma cells have been achieved. As little as 8% of the total volume of a single cell has been sampled and analyzed. Dopamine has been identified and quantified in these PC12 cells using this technique. The average cytoplasmic level of dopamine in rat pheochromocytoma cells has been determined to be 240 ± 60 μM. The use of electrophoresis in 770 nanometer inner diameter capillaries with electrochemical detection to monitor cytoplasmic neurotransmitters at the single cell level can provide information about complex cellular functions such as neurotransmitter storage and synthesis.     

Fused s-triazino heterocycles. XIII. 1,3,7,10,11c-Pentaazabenz[de]-anthracene and 1,3,7,10,11,13,13d-heptaazabenz[de]cyclopenta[H]-anthracene,two new ring systems

The synthesis of the title compounds 5a-c and 6a-c is described using, 2,6-diaminopyridine as starting material. The key intermediates are 2-t-butyl-4-cyano-5(2-dimethylaminoethenyl)-1,3,6,9b-tetraazaphenalene 4 and 10-amino-2-t-butyl-10,11-dihydro-11-imino-1,3,7,10,11c-pentaazabenz[de]anthracene 5c .     

Synthesis,thermal, spectral,antimicrobial and cytotoxicity profile of the Schiff bases bearing pyrazolone moiety and their Cu(II) complexes

Journal of Thermal Analysis and Calorimetry - A series of Schiff bases resulted in the [1?+?1] condensation of 8-alkyl-2-hydroxy-tricyclo[7.3.1.02.7]-tridecan-13-one with the...     

Simultaneous Determination of Some Analgesic Drugs Using Mixed Mode Stationary Phase

A new HPLC method based on a mixed mode stationary phase Hypersil Duet C18/SAX was developed and applied for the simultaneous determination of acetaminophen, acetylsalicylic acid and codeine. Parameters, such as the composition of the mobile phase, the nature of the organic modifier, the buffer type and the flow rate were investigated to optimize the separation. The results obtained show that the new HPLC method is rapid, highly efficient and selective. The studied compounds are separated in 10 min, by means of a mobile phase containing phosphate buffer (pH 7.50) and methanol (65:35 v v⁻¹). The retention mechanisms of each analyte were investigated using both the linear solvent strength theory and stoichiometric displacement model. The method was fully validated and showed good linearity for each compound for a concentration ranging between 2.0 and 40 μg mL⁻¹. The limits of detection and quantification were determined and they are lower than 0.1 μg mL⁻¹. The precision (RSD) of the method does not exceed 2 % for all studied compounds. The method was successfully applied for the assay of acetaminophen, acetylsalicylic acid and codeine in pharmaceutical formulations.

     

Novel fluorescence nanostructured materials obtained by entrapment of an ornamental bush extract in hybrid silica glass

Synthesis of some novel fluorescence nanomaterials loaded with photoactive polyphenols originated from plants with a high spectrum of biological activity, by replacing synthetic chemicals, may open new opportunities for optical and bio-medical applications. This paper presents the synthesis, characterization and fluorescence properties of a new class of materials based on host hybrid matrices obtained through templated sol–gel route, by hydrolysis and co-condensation of tetraorthoethylsilicate with octaisobutyltetracyclo [7.3.3.1^5,11] octasiloxane-endo-3,7-diol. The aim of paper is focused on the evaluation of the behavior of the fluorescence properties of ornamental bush extract at immobilization in a templated silica matrix and in a silica-silsesquioxane network, using as templates a neutral, non-toxic and biodegradable surfactant from poly(ethyleneglycol) class and a high biocompatible non-surfactant from glucidic class. The proofs of ornamental bush extract entrapment by physical interactions in silica based networks were provided by FT-IR and UV–VIS spectroscopy. The changes of polymer network due to the hydrogen bond interactions between residual Si–OH groups and functional groups of organic molecules from extract were evidenced by shifts of specific vibrations. In UV–VIS-NIR domain, the chromophore groups from ornamental bush extract were also evidenced by similar small shifts. As a result of ornamental bush extract entrapment, in all the immobilized samples the fluorescence intensity was more than 10 times amplified in samples templated with poly(ethylenglycol) surfactant) and of about 5 times in samples with glucidic template due to the physical adsorption of polyphenolic molecules from extract, excellent synergistic optical properties of SiO₂ and silsesquioxane compound and also due to a favorable conformational arrangement. The size of synthesized polymeric materials, estimated by dynamic light scattering technique showed main diameters less then 1.4 μm, namely 1,060 and 211 nm—for samples with d-glucose template and 1,330 and 531 nm—for samples with poly(ethyleneglycol) template, respectively, with a narrow size distribution and a polidispersity varying between 0.022 and 0.426. These results are in good accordance with TEM images that evidenced the presence of some polymeric aggregates which contain the vegetal extract immobilized inside hybrid SiO₂-Sq polymeric network of about hundred nanometers size. This study bring new contributions to the development of the sol–gel procedure by entrapment of a complex vegetable mixture in polymeric matrices as integral component of silica and hybrid silica-silsesquioxane networks which leads to a significant enhancement of the functional properties of the final material, thus diversifying the potential applications of organic doped sol–gel glasses.