Direct immersion solid-phase microextraction has been optimized and applied to the simultaneous determination of the neutral and basic pharmaceuticals: caffeine, carbamazepine, clomipramine, chlorprothixene and clotrimazole at low concentrations in municipal wastewater. Two absorption type stationary phases: polydimethylsiloxane (PDMS) and polyacrylate (PA) have been found to be most effective for extraction of target analytes. The separation and detection were carried out by gas chromatograph coupled with mass spectrometer working in the selected ion monitoring mode. The method was validated for linearity, detection and quantitation limits, selectivity and precision. The average correlation coefficient of the calibration curves was 0.9933. The LOD values in influent and effluent wastewater were in the range of 10–145 ng L?1 and 4–111 ng L?1, respectively, which were a bit higher than those in the deionized water due to matrix effect. The high values of distribution coefficient (Kfs) in PDMS/water and PA/water systems (log Kfs between 3.05 and 4.23) indicates the very high applicability of these stationary phases for determination of carbamazepine, clomipramine, chlorprothixene and clotrimazole in water samples.
The polycrystalline Ho4Ni11In20 was obtained by arc-melting of the elements. The subsequent high temperature procedure was used for single crystal growth. Crystal structure of the compound was investigated by X-ray single crystal method: U4Ni11Ga20 type, C 2/m, a = 22.4528(17), b = 4.2947(3), c = 16.5587(13) Å, β = 124.591(5)°, R1 = 0.0276, wR2 = 0.0493 for 1989 independent reflections with [I>2σ(I)].The structure is composed of three-dimensional network from Ni and In atoms in which Ho atoms fill distorted pentagonal channels. Open image in new window相似文献
An one-pot approach was developed for the synthesis of substituted 5,7-dihydro-1,6-naphthyridines and 5,6,7,8-tetrahydroquinolines with moderate to good yields. This pathway is a modified two-step synthesis of Kröhnke pyridine and involves a four-component tandem reaction of N-phenacylpyridinium bromide, aromatic aldehydes, substituted or nitrogen-containing cyclic ketones and a nitrogen source. This multi-component reaction is performed using microwave irradiation heating of the reaction substrates under an environment of NH4OAc/HOAc.
In addition to the commonly observed single molecule fluorescence intensity fluctuations due to molecular reorientation dynamics, a perylene bisimide-calixarene compound (1) shows additional on-off fluctuations due to its ability to undergo intramolecular excited state electron transfer (PET). This quenching process is turned on rather sharply when a film of poly(vinylacetate) containing 1 is heated above its glass transition temperature (Tg), which indicates that the electron transfer process depends on the availability of sufficient free volume. Spatial heterogeneities cause different individual molecules to reach the electron transfer regime at different temperatures, but these heterogeneities also fluctuate in time: in the matrix above Tg molecules that are mostly nonfluorescent due to PET can become fluorescent again on timescales of seconds to minutes.The two different mechanisms for intensity fluctuation, rotation and PET, thus far only observed in compound 1, make it a unique probe for the dynamics of supercooled liquids.
In this study, microwave assisted a hydrodistillation process (MWHD) of essential oils from lavender (Lavandula angustifolia Miller) was investigated. In order to examine any potential differences in essential oil extraction, the lavender flowers underwent enzymatic pretreatment.A 23 factorial design of experiments, combined with statistical methods of data analysis were used to optimize enzymatic pretreatment and to evaluate the influence of major variables (enzyme concentration, temperature and pH) on the performance of the microwave assisted extraction.Under optimal conditions, an extraction yield of 24 mg oil g?1 substrate was achieved (an increase by approximately 25% in comparison with the classic extraction conditions of conventional hydrodistillation).The main compounds of the essential oils obtained were analyzed and identified by gas chromatography coupled to mass spectrometry (GC-MS). Analyzing the data obtained indicated that the content of main compounds (linalool and linalyl acetate ? 73%) was greater than that obtained by conventional extraction (67%).
Biocatalysts with microorganisms immobilized on solid carriers could provide the solution for development of continuous industrial processes for ethanol obtaining by fermentation of sugars. In this study, modified polyacrylamide hydrogels and marrow stem sunflower are used as supports for Saccharomyces cerevisiae yeast immobilization. The obtained structures are used for fermentation of molasses in batch systems. The free yeast cells are used as reference. The modification of polyacrilamide matrix with (2-hydroxyethyl)methacrylate has a positive effect on structure pore uniformity and fermentation performance. The mechanical properties of the obtained biocatalysts are compared. The novel natural matrix has net superior compression strength.
The phase behavior of the carbon dioxide + cycloalkane mixtures usually receives low attention, though these systems are important for many industries, e.g. the carbon capture and storage. In this paper calculations results for the carbon dioxide + cyclopentane binary system are presented, based on SRK and PR cubic equations of state with classical van der Waals mixing rules. A single set of binary parameters for each model was proposed to predict the global phase behavior of the system in a wide range of pressure and temperature. Albeit the thermodynamic models used are simple, they are able to represent fairly well the phase behavior of the system analyzed in this paper.
The aim of this research was to investigate the chemical composition of Coreopsis tinctoria Nutt. fruits extract, to highlight the potential of ultrasound assisted extraction in the fast preparation of extracts rich in polyphenols using different solvents (55%, 78% and 96% hydrous ethanol) and to evaluate the antioxidant potential of formulated extracts. LC-MS/MS was used to characterize the ethanolic extract from Coreopsis tinctoria Nutt. dried fruits. The extract contains different flavonoids (marein, flavanomarein, quercetagetin-7-O-glucoside, okanin aurone, leptosidin, luteolin, apigenin) and phenolic acids (chlorogenic acid, caffeic acid). Several parameters that could affect extraction efficiency were evaluated. Finally, this study focused on determination of plant extracts total phenolic content and their antioxidant capacity. The experimental results allowed the selection of the optimum operating parameters leading to the highest total polyphenolic content, expressed as gallic acid equivalents, and avoiding the degradation of phenolic compounds (ethanol 55%; extraction temperature 323.15 K, extraction time 30 min, liquid/solid ratio 20/1). A good relationship between total phenolic content and antioxidant capacity was obtained.
In the present study, we propose a method for the evaluation of different classes of xenobiotic organic compounds enclosed in the municipal landfill leachate using comprehensive two-dimensional gas chromatography coupled with quadrupole mass spectrometry (GCxGC-qMS). Here we show that, due to high peak capacity of comprehensive two-dimensional gas chromatography, in a single run it is possible to separate compounds with different physical-chemical properties (such as aliphatic and aromatic compounds, polyaromatic hydrocarbons, phenols, phthalates, aldehydes, ketones, nitrogen containing compounds, organo-phosphoric flame retardants etc.), compounds which have proved to be endocrine disruptors, compounds that are persistent, bioaccumulative and toxic, carcinogenic, mutagenic, teratogenic, reprotoxic or harmful for the environment. Even though a solvent extraction method has been optimised, the extraction step still remains the main problem for a comprehensive characterization of all classes of organic toxicants enclosed in the municipal landfill leachate.
Four novel thiourea derivatives containing a thiazole moiety were synthesized and characterized by IR, 1H and 13C NMR, mass spectrometry and elemental analysis. The crystal structure of 1a was determined from single crystal X-ray diffraction data. It crystallizes in monoclinic space group P21/n with unit cell dimensions a = 11.7752(6) Å, b= 3.8677(2) Å, c= 27.4126(13) Å and β = 92.734(5) Å. There is a strong intramolecular hydrogen bond of the type N-H?O, with H?O distance of 2.5869(19) Å. The mass fragmentation pattern has also been discussed. The antifungal activity of the synthesized compounds was studied by broth micro-dilution method and poisoned food technique. The compounds 1b and 1c possessed a broad spectrum of antifungal activity.
Specular reflection infrared microspectroscopy was used for chemical imaging of cross-sectioned urinary stones to determine their chemical composition and morphology simultaneously. Absorption spectral bands were recovered from reflection spectra by Kramers-Kronig transform. FUse of far-infrared radiation provides high-contrast images and allows more precise constituent distribution determinations than mid-infrared because band asymmetry after the transform caused by diffuse reflection is less in the far-infrared.
New potentially biologically active compounds derived from 2-mercapto-benzoxazole were synthesized and coupled on polymeric support of poly (maleic anhydride-alt-vinyl acetate) for the preparation of polymer-drug conjugates with controlled drug release. All compounds were characterized by elemental and spectroscopy (FT-IR, 1H-NMR) analysis. The toxicological tests recommend the products for further laboratory screening. 相似文献
The single crystal X-ray structures and the spectroscopic properties of complexes of monensic acid (C36H62O11·H2O) with toxic metal ions of Cd(II) and Hg(II) are discussed. The cadmium(II) complex (1) is of composition [Cd(C36H61O11)2(H2O)2] and crystallizes in the monoclinic system (space group P2(1), Z = 2) with a = 12.4090(8), b = 24.7688(16), c = 14.4358(11) Å, β = 91.979(7)°. Two ligand monoanions are bound in a bidentate coordination mode to Cd(II) via the carboxylate and the primary hydroxyl oxygens occupying the equatorial plane of the complex. The axial positions of the inner coordination sphere of Cd(II) are filled by two water molecules additionally engaged in intramolecular hydrogen bonds. The Hg(II) complex (2), [Hg(C36H60O11)(H2O)], crystallizes in the orthorhombic system (space group P2(1)2(1)2(1), Z = 4) with a = 12.7316(2), b = 16.4379(3), c = 18.7184(4) Å. The monensic acid reacts with Hg(II) in a tetradentate coordination manner via both oxygen atoms of the carboxylate function and oxygens of two hydroxyl groups. The twofold negative charge of the ligand is achieved by deprotonation of carboxylic and secondary hydroxyl groups located at the opposite ends of the molecule. Hg(II) is surrounded by five oxygen atoms in a distorted square pyramidal molecular geometry.
After oxidation of tannins (Tannins 1–3) extracted from grape seeds, Tanoxil compounds with increased solubility and enhanced antioxidant activities were synthesized. In this research, ABTS+· assay and a chemiluminescence method were used for antioxidant measurement of hydrophilic compounds (Tanoxils 1–3).
It was observed that the antioxidant activity (AA, %) is very similar for the three samples, while at the same time AA is quite high (93.16%–96.48%). The percentage of inhibition by ABTS+· is higher for Tanoxil 2 (96.4%) as compared to Tannin 2 compound (14.34%). Moreover, the total content (TCF) of carboxyl and phenolic groups was investigated. TCF values, determined for Tanoxil products, revealed a double (Tanoxil 1) or triple (Tanoxil 2) increase as compared to the value of the TCF of Tannin 1. Tanoxil products represent an interest for future research as they have a high AA (96.4%) and the content of acidic groups is significant (TCF, 0.191 meq g?1).
Bacterial cellulose (BC), a natural polymer with unique physical and mechanical properties, has several applications in the biomedical field, including drug loading and controlled drug delivery. For this study, a Box-Behnken experimental design was employed as a statistical tool to optimize the release of a model drug, amoxicillin, from BC membranes. Independent variables studied were the concentration of the drug (X1), the concentration of glycerol (X2) and the concentration of a permeation enhancer (X3). From the variables studied, drug concentration had the highest effect on drug release. Among the other independent variables, th linear and quadratic X2 terms, the linear X3 term and the interaction term X2X3 were found to affect the release of amoxicillin from bacterial cellulose membranes.
Common waste glasses (window, bottle glass or tableware) with fly ash form a glass matrix for chromium waste immobilization. Soluble chromium from residual waters was adsorbed on fly ash; the resulting solid contained 23.7% Cr6+. The three glass wastes, chromium-containing fly ash, and borax were used to make glasses in weight ratios waste glass: borax: fly ash of 1: 1: 1 and 1.5: 0.5: 1. The hydrolytic stability ranged from 18.46 to 28.13 µg g?1 soluble Na2O, qualifying them in the HGB1 class. The chemical stability, characterized by the dissolution rate, was 0.011–0.077 µg cm?2 h?1, depending on the glass composition and the aggressive medium pH. The chromium leachability is influnced by the glass composition and the pH of the leaching solution, ranging between 0–0.015% of the total chromium. Chromium waste vitrification is a viabile solution with multiple economic advantages.
The rearrangement of easily accessible Cookson’s diketone with chlorosulfonic acid in chloroform followed by the acidic hydrolysis gave 6-chloro-7-hydroxy-dichloropentacyclo[6.3.0.02,6.03,10.05,9]undecane-4-one, whose syn-stereochemistry was assigned through the X-ray crystal structure analysis. This key structure was used for the stereoselective synthesis of the D3-trishomocubane derivatives as well as for the preparation of potential drugs bearing hydroxy- and amino-functional groups. A new multigram preparative synthesis of D3-trishomocubane was developed. 相似文献
Magnetic fluid applications require stability under demanding conditions. Complete magnetic fluids and their component surfactants and dispersing oils were irradiated. Their subsequent thermal oxidation was characterized by chemiluminescence and DSC. Except for polyisobutylsuccinic anhydride, irradiation sensitized the components toward oxidation. The components were ranked by stability. Complete fluids were more stable than would be predicted from their components suggesting that they may be used for nuclear applications.
