Search results for "Spectrometry"
showing 10 items of 3206 documents
DNA fluorescence induced by polymethine cation pyrvinium binding
1991
Pyrvinium is a polymethine cation which shows interesting fluorescence emission and DNA binding properties. In diluted aqueous solution, pyrvinium pamoate induced a bright yellow fluorescence in kinetoplast DNA from Trypanosoma cruzi epimastigotes as well as in chicken erythrocyte nuclei under a wide range of excitations. No fading was observed after mounting in suitable media. Spectroscopic studies on pyrvinium solutions revealed bathochromic and hypochromic shifts in the absorption spectrum of its complex with DNA. A striking enhancement of pyrvinium fluorescence was found in solvents of high viscosity or after binding to DNA. Experimental results and the chemical structure of pyrvinium a…
FIA-fluorimetric determination of adrenaline in pharmaceutical formulations by oxidation with molecular oxygen
1998
The fluorimetric determination of adrenaline is carried out in a continuous-flow assembly and by means of the molecular dissolved oxygen. The sample solution merges with an NaOH stream, then the resulting mixture is heated at 73 °C and led to the flow-cell of the fluorimeter. The flow-assembly is very simple and the procedure is quick (107 samples h−1) reproducible (R.S.D. 0.6%), selective and suitable to be applied to determination of adrenaline in formulations. Calibrations graph are linear over the ranges 0.05–15 and 20–40 mgl−1.
Gas assisted mechanical expression (GAME) for the selective recovery of lipophilic and hydrophilic compounds from olive kernel
2017
Abstract This work is devoted to valorize olive kernel; a by-product produced during olive oil extraction process. For this purpose, aqueous liquid solid extraction (LSE), mechanical expression (ME), supercritical CO2 (SC-CO2) and gas assisted mechanical expression (GAME), processes were compared when applied separately or consequently (ME + GAME), in terms of total phenolic compound (TPC) and oil recovery yields. Results showed that although the high extraction yields of TPC using LSE (61.4 ± 1.3%), the extraction process is economically not viable. However, it was demonstrated that applying ME (1 h at 30 MPa) followed by GAME (1 h at 30 MPa ME and 10 MPa SC-CO2 pressures) allowed recoveri…
Screening and authentication of herbal formulations based on microextraction-assisted voltammetry of microparticles
2015
A simple solid state electrochemical methodology for screening and authentication of herbal formulations is described. The proposed method is based on the recording of the voltammetric response, in contact with aqueous buffers, of microparticulate films of antioxidant compounds resulting from micro-extraction of dried herbal samples with ethanol or acetone. The obtained voltammetric responses led us to differentiate between diverse active components upon application of bivariate and multivariate chemometric techniques. Resolution of herbal preparations containing two or more components is possible when well-separated voltammetric signals are recorded. In favorable cases, such characteristic…
Desulfurization processes of thiosemicarbazonecopper(ii) derivatives in acidic and basic aqueous media
2013
This work provides structural evidence for different desulfurization processes in aqueous solutions of [CuL]+ derivatives (HL = pyridine-2-carbaldehyde thiosemicarbazone). Structural resolution has been achieved for the [{CuL(SH)}2] (1), [CuLCl]2[Cu(pic)2] (pic− = picolinato, pyridine-2-carboxilato) (2) and [Cu(HL)(NCS)](NO3) (4) compounds, together with a derivative of 4 with formula [Cu(HL)(NCS)][Cu(HL)(NCS)0.72(NO3)0.28](NO3)2 (5), whose HS−, pic− and NCS− ligands come from thiosemicarbazone breakage. The behaviour of the [CuL]+ species in basic aqueous solutions or water under reflux has been compared with that exhibited by iron(III), cobalt(III), zinc(II) and lead(II) derivatives of th…
Reaction pathways of glucose oxidation by ozone under acidic conditions.
2009
The ozonation of d-glucose-1-(13)C, 2-(13)C, and 6-(13)C was carried out at pH 2.5 in a semi-batch reactor at room temperature. The products present in the liquid phase were analyzed by GC-MS, HPAEC-PAD, and (13)C NMR spectroscopy. Common oxidation products of glucose have also been submitted to identical ozonation conditions. For the first time, a pentaric acid was identified and its formation quantitatively correlated to the loss of C-6 of glucose in the form of carbon dioxide. Potential mechanisms for the formation of this pentaric acid are discussed. The well-accepted pathway involving the anomeric position in glucose, gluconic acid, arabinose, and carbon dioxide is reinvestigated. The …
Identification of Bioactive Compounds in Polar and Nonpolar Extracts of Araujia sericifera
2017
Abstract Araujia sericifera is a native perennial, climbing laticiferous shrub from South America that is currently naturalized in many other countries. Previous data describe promising properties for A. sericifera, but no systematic study of its bioactive compounds and possible medicinal applications has been conducted to date. In the present study, aerial parts of A. sericifera (leaves, stems, and fruits) were explored by combining GC-MS and NMR spectroscopy analysis for both nonpolar (hexane) and polar (methanol) extracts. The hexanic extracts contained high amounts of pentacyclic triterpenes including two new metabolites, 3-tigloyl germanicol (18) and 3-tigloyl lupeol (19). The methanol…
PHYSICO-CHEMICAL CHARACTERIZATION OF THE ACQUALADRONE ROSTRUM
2011
The archaeological discovery of the Acqualadrone rostrum (an offensive naval weapon mounted on the prow at the waterline), off the Italian coast near Messina in 2008, has led to the need for scientific research in order to plan the conservation treatment of this artefact. The discovery is exceptional because of the presence of a wooden section from the original ship. This paper describes the physico-chemical characterization of a metallic and two wooden samples by inductively coupled plasma – optical emission spectroscopy, inductively coupled plasma – mass spectrometry, Fourier transform infrared spectroscopy, 13 C{ 1 H} cross-polarization magic angle spinning NMR spectroscopy, energy-dispe…
SINGLE-PEAK RESOLUTION CRITERIA FOR OPTIMIZATION OF MOBILE PHASE COMPOSITION IN LIQUID CHROMATOGRAPHY
2001
Three criteria that evaluate the single peak resolution (peak purity) in chromatography, the free height fraction, free area fraction, and valley ratio, are examined. The main advantages of these criteria against other criteria based on peak pair separation, are that the measurements are not affected by the identity of neighboring peaks and are normalized, which make them very intuitive. The methodology is illustrated through the isocratic separation of mixtures of several sulphonamides (sulphacetamide, sulphadiazine, sulphadimethoxine, sulphaguanidine, sulphamerazine, sulphamethazine, sulphamethoxazole, sulphamethizole, sulphamonomethoxine, sulphanilamide, sulphapyridine, sulphaquinoxaline…
Study of the performance of a resolution criterion to characterise complex chromatograms with unknowns or without standards
2017
The search for best conditions in liquid chromatography is routinely carried out with information provided by chemical standards. However, sometimes there are samples with insufficient knowledge about their chemical composition. In other cases, identities of the components are known, but there are no standards available, and in other cases the identities of peaks in chromatograms taken under different conditions are ambiguous. Most resolution criteria used to measure separation performance cannot be applied to these samples. In this work, a global resolution function valid for all situations was developed based on automatic measurements of peak prominences (area fraction exceeding the line …