Search results for "Spectroscopy"
showing 10 items of 10293 documents
Multi-technique approach for qualitative and quantitative characterization of furazidin degradation kinetics under alkaline conditions
2016
Degradation of drug furazidin was studied under different conditions of environmental pH (11-13) and temperature (30-60°C). The novel approach of hybrid hard- and soft-multivariate curve resolution-alternating least squares (HS-MCR-ALS) method was applied to UV-vis spectral data to determine a valid kinetic model and kinetic parameters of the degradation process. The system was found to be comprised of three main species and best characterized by two consecutive first-order reactions. Furazidin degradation rate was found to be highly dependent on the applied environmental conditions, showing more prominent differences between both degradation steps towards higher pH and temperature. Complim…
The application of phospholipid removal columns and ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry for quantificati…
2016
In this study a robust and sensitive method based on a proposed sample purification procedure, using zirconia-coated Phree™ columns and analysis by ultra-high performance liquid chromatography with triple quadrupole tandem mass spectrometry are presented for the assessment of multi-class antibiotics in farmed fish species. The sample preparation procedure benefited from combined precipitation of proteins and selective removal of phospholipids by Phree™ columns, resulting in a high sensitivity of the method (LOQ 0.3-9mgkg(-1)). The in-house validation results (precision, repeatability, decision limit CCα, detection capability CCβ, etc.) indicate that the elaborated method is fully suitable f…
Comparison of several methods used for the determination of cephalosporins. Analysis of cephalexin in pharmaceutical samples
2002
The precision of UV absorbance of intact and acid degraded cephalosporins, ninhydrin, high performance liquid chromatography and iodometric methods used for analysis of cefoxitin, cefotaxime, cephazolin and cephalexin were compared. To obtain the calibration graphs the analytical signal used were: absorbance, first derivative absorbance, second derivative absorbance and H-point Standard Additions Method by using absorbance values at two selected wavelengths as analytical signal. These methods and calibration graphs were also used for the determination of cephalexin in pharmaceutical samples.
Furosemide assay in pharmaceuticals by Micellar liquid chromatography: study of the stability of the drug.
2000
A simplified high-performance liquid chromatographic procedure is described for the determination of furosemide (4-chloro-N-furfuryl-5-sulphamoylanthranillic acid), which makes use of UV detection, a C18, reversed-phase column, and micellar mobile phases of sodium dodecyl sulphate (SDS) and 1-propanol at pH 3 buffered with phosphate system. The most adequate experimental conditions to handle furosemide solutions in the analytical laboratory are studied. The mixture of furosemide and its degradation products which are formed upon light exposition was resolved with a mobile phase of 0.04 M SDS-2% propanol. Separation of furosemide from its common impurities and the hydrolytic product, 4-chlor…
Determination of pharmaceutical residues in wastewater using high performance liquid chromatography coupled to quadrupole-Orbitrap mass spectrometry
2016
Abstract A multi-class method for the determination of 24 emerging pharmaceutical residues has been developed and validated. The method is based on solid-phase extraction of wastewater samples using Strata-X cartridges followed by high performance liquid chromatography coupled to hybrid quadrupole − Orbitrap high resolution mass spectrometry (HPLC-Q-Orbitrap-HRMS). A single-laboratory validation procedure showed satisfactory analytical performance. The analysis of 21 samples collected at the wastewater treatment plant in Riga revealed the occurrence of 20 compounds of different therapeutic classes. The highest concentration was found for the central nervous system stimulator caffeine − up t…
In situ generation of Co(II) by use of a solid-phase reactor in an FIA assembly for the spectrophotometric determination of penicillamine
2005
[EN] A flow injection analysis (FIA) manifold for the determination of penicillamine in pharmaceutical preparations is proposed. The manifold includes a solid-phase reactor for the in situ production of the derivatizing reagent, Co(II) ion, which forms a coloured complex with penicillamine in an alkaline medium. The reactor is prepared by natural immobilization of cobalt carbonate on a polymer matrix, which endows it with a high mechanical and microbiological stability. The cobalt released by passage of a 5 x 10(-4) Mol l(-1) sulphuric acid stream at a flow-rate of 2.3 ml min(-1) is merged with a volume of 314 mu l of sample containing penicillamine in ammonium-ammonia buffer at pH 9.5 to m…
Chiral separation of oxprenolol by affinity electrokinetic chromatography-partial filling technique using human serum albumin as chiral selector
2005
The intrinsic characteristics of capillary electrophoresis have made this technique a powerful tool in the chiral separation field. The present paper deals with the enantiomeric separation of oxprenolol enantiomers by affinity electrokinetic chromatography-partial filling technique using human serum albumin (HSA) as chiral selector. Several experimental conditions and variables affecting the separation such as pH, HSA concentration and plug length, background electrolyte concentration, temperature and voltage were studied. Baseline separation of oxprenolol enantiomers was obtained in less than 8 min under the following selected conditions: electrophoretic buffer composed of 50 mM Tris-(hydr…
Studies of Reversible Hydrogen Binding in Nano- Sized Materials
2015
Experimental review of materials suitable for reversible hydrogen binding in nanoporous and nanosized structures of materials, based on natural zeolite (clinoptilolite) and graphene (exfoliated electrochemically from raw graphite), were analyzed. Characterization of materials with SEM, XRD, EDS and Raman spectroscopy methods and aspects of synthesis of a nanostructured zeolite and a few-layer graphite material was done in this work. It was established from gas analyzer results that hydrogen mass fraction in natural zeolite ranged from 1.1 % to 1.4 %, but in the few-layer graphite material − from 0.39 % to 0.46 %.
Photocatalytic coalescence of functionalized gold nanoparticles.
2009
A novel strategy for the synthesis of chromophore-functionalized AuNPs with a narrow size distribution is reported. It consists of increasing the size of preprepared NPs by means of a fast (second scale) and clean (light and an organic photocatalyst) method. The results agree with thiolate ligand liberation from the NP surface promoted by photogenerated radicals. This lets gold cores come together and finally coalesce.
Prediction of soil texture distributions using VNIR-SWIR reflectance spectroscopy
2013
Abstract Reflectance spectroscopy provides an alternate method to non-destructively characterize key soil properties. Different approaches, including chemometrics techniques or specific absorption features, have been proposed to estimate soil properties from visible and near-infrared (VNIR, 400-1200 nm) and shortwave infrared (SWIR, 1200-2500 nm) reflectance domains. The main goal of this study was to test the performance of two distinct methods for soil texture estimation by VNIR-SWIR reflectance measurements: i) the Continuum Removal (CR) technique that was used to correlate specific spectral absorption features with clay, silt and sand content, and ii) the Partial Least-Squares Regressio…