Search results for "Derivative"
showing 10 items of 1074 documents
Preparation and structural studies on the tBu2Sn(IV) complexes with aromatic mono- and dicarboxylic acids containing hetero {N} donor atom
2004
Nine complexes of 'Bu2Sn(IV)(2+) were obtained in the solid state with ligands containing -COOH group(s) and aromatic (N) donor atom. The binding sites of the ligands were identified by FT-IR spectroscopic measurements. It was found that in most cases the -COO- groups are co-ordinated in monodentate manner. Nevertheless, in some of our complexes, the -COO- group forms bridges between two central {Sn} atoms resulting in the formation of an oligomeric structure, a motif that is characteristic only to the nicotinate compound. These pieces of information and the rationalisation of the experimental Sn-119 Mossbauer nuclear quadrupole splittings, Delta, - according to the point charge model forma…
Multiple Roles of Isocyanides in Palladium-Catalyzed Imidoylative Couplings: A Mechanistic Study
2016
International audience; Kinetic, spectroscopic and computational studies examining a palladium-catalyzed imidoylative coupling highlight the dual role of isocyanides as both substrates and ligands for this class of transformations. The synthesis of secondary amides from aryl halides and water is presented as a case study. The kinetics of the oxidative addition of ArI with RNC-ligated Pd-0 species have been studied and the resulting imidoyl complex [(ArC=NR)Pd(CNR)(2)I] (Ar=4-F-C6H4, R = tBu) has been isolated and characterized by X-ray diffraction. The unprecedented ability of this RNC-ligated imidoyl-Pd complex to undergo reductive elimination at room temperature to give the amide in the p…
Acid-induced rearrangement of epoxygermacra-8,12-olides: synthesis and absolute configuration of guaiane and eudesmane derivatives from artemisiifolin
2010
A study on the acid-induced rearrangement of 4,5-epoxy- and 1,10-epoxygermacra-8,12-olides was carried out. From a 4,5-epoxy derivative, guaianes were obtained, whereas 1,10-epoxy derivatives furnished, depending on the stereochemistry of the C-1/C-10 epoxy ring, trans-5β,10α- or trans-5α,10β-eudesmanolides.
Influence of the differentiation system on the analytical parameters for the spectrophotometric determination of clonazepam in urine
1991
Abstract Electronic and mathematical differentiation of the ultraviolet visible spectra were compared from the study of the analytical parameters of the direct determination of clonazepam in urine samples. Third-order derivative spectra were used. The mathematical differentiation provides higher sensitivity, a lower limit of detection, and better accuracy and precision than the electronic one. The use of a diode array instrument provides lower sensitivity than that found using a conventional spectrometer; however, the limit of detection obtained in both cases is of the same order.
Simultaneous determination of oxybenzone and 2-ethylhexyl 4-methoxycinnamate in sunscreen formulations by flow injection-isodifferential derivative u…
2001
Abstract A flow injection procedure was developed for the simultaneous determination of two UV filters (oxybenzone and 2-ethylhexyl 4-methoxycinnamate) in sunscreen formulations, based on the isodifferential approach. The use of the second derivative spectra allowed a selective determination of the analytes free from matrix interferences and without pretreatment of samples. Standard solutions of the analytes were analyzed by the proposed procedure in order to select the appropriate wavelengths to solve the mixture. After this, the procedure was validated using commercial sunscreen formulations the concentrations of which were determined by an HPLC procedure. The two procedures gave comparab…
Comparative evaluation of liquid chromatography versus gas chromatography using a β-cyclodextrin stationary phase for the determination of BTEX in oc…
2009
An HPLC method for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene in occupational environments was developed and compared with a GC-MS method. Chromatographic analysis using a beta-cyclodextrin stationary phase was performed after active and passive air sampling by adsorption on activated charcoal and pressurized fluid extraction. The analytes were completely separated and quantified using both methods, although GC-MS provided better resolutions and lower detection limits than HPLC. The HPLC method was unsuccessfully applied to the determination of benzene in real samples because its sensitivity was too low. Both methods were applied to the analysis …
Quantification of nortriptyline in plasma by HPLC and fluorescence detection
2009
Abstract A simple, sensitive and specific high-performance liquid chromatography method has been developed for the determination of nortriptyline (NT) in plasma samples. The assay involved derivatization with 9H-fluoren-9-ylmethyl chloroformate (Fmoc-Cl) and isocratic reversed-phase (C 18 ) chromatography with fluorescence detection. The developed method required only 100 μl of plasma sample, deproteinized and derivatized in one step. Calibration curves were lineal over the concentration range of 5–5000 ng/ml. The derivatization reaction was performed at room temperature in 20 min and the obtained NT derivative was stable for at least 48 h at room temperature. The within-day and between-day…
In situ derivatization for double confirmation of 2C–C in oral fluids by ion mobility spectrometry
2017
Ion mobility spectrometry (IMS) is a powerful tool to carry out quick and sensitive detection of illicit activities and has been employed for the determination of the psychedelic drug 2,5-dimethoxy-4 chlorophenethylamine (2C–C) in oral fluid samples. Saliva samples were extracted with chloroform and analysed by IMS reaching a limit of detection (LOD) of 14 μg L−1. Nevertheless, IMS has a scarce resolution and selectivity of the method can be often compromised by the presence of potential interferents with similar molecular weights and drift times. Thus, a rapid and in situ derivatization with acetone, to form the corresponding imine, has been proposed in the present study to confirm the pre…
Direct derivative spectrophotometric determination of carbaryl and carbofuran in water samples
1990
Abstract Derivative absorption spectrophotometry has been applied to the direct determination of carbaryl and carbofuran in water samples. The use of the third derivative for carbaryl and the fourth derivative for carbofuran reduces the matrix effect and the seventh derivative provides, in both cases, accurate results for the determination of these pesticides, even working at low dilution levels of the samples. A limit of detection of 4 ppb and a variation coefficient of 0.1% have been obtained for the determination of carbaryl. Carbofuran can be determined with a limit of detection of 5 ppb and a variation coefficient of 0.02%.
First-order derivative resolution of overlapped PAH peaks with common mass spectra in gas chromatography–mass spectrometry
2007
Abstract First-order derivative of 15 points smoothed chromatograms of mixtures of benzo( b )fluoranthene (BbF) and benzo( k )fluoranthene (BkF) for the m / z 252 ion obtained using two microscans has been proposed as a simple alternative to the resolution of overlapped chromatographic peaks of these two compounds which have identical mass spectra. The procedure provides limits of detection of 12 and 29 ng g −1 for BbF and BkF, respectively and offers the possibility to use the 250 and 248 ions to confirm the identity of these analytes.