Search results for "Chemical analysis"
showing 10 items of 324 documents
o-Phthalaldehyde–N-acetylcysteine polyamine derivatives: formation and stability in solution and in C18 supports
2001
A comparative study of different derivatization procedures has been performed in order to improve the stability of the reaction products o-phthalaldehyde-N-acetylcysteine (OPA-NAC) polyamines. Procedures such as solution derivatization, solution derivatization followed by retention on a packing support, derivatization on different packing supports and on-column derivatization, have been optimized and compared. The degradation rate constant (k) of the derivative was dependent on the procedure used and on the analyte. For the spermine (the most unstable isoindol tested) k was 8 +/- 2 x 10(-2) min(-1) in solution versus 7.7 +/- 1.1 x 10(-4) min(-1) on the (C18) solid support. The results obtai…
Micellar liquid chromatography determination of rivaroxaban in plasma and urine. Validation and theoretical aspects.
2019
A Micellar Chromatographic method to determine rivaroxaban in plasma and urine has been developed. The samples were dissolved in the mobile phase (SDS 0.05 M – 1-propanol 12.5%, phosphate buffered at pH 7) and 20 μL directly injected, avoiding the extraction and purification steps. Using a C18 column and running under isocratic mode at 1 mL/min, analyte was eluted without interference from the matrix in <6.0 min. The detection absorbance wavelength was set to 250 nm. The procedure was validated by Food and Drug Administration guidelines in terms of: system suitability, calibration range (0.05–5 mg/L), linearity, sensitivity, robustness, carry-over effect, specificity, accuracy (−11.1 to 4.2…
Development of the H-point standard additions method for analyte determinations in unknown matrix
1993
Abstract The development of the H-point standard additions method is proposed in order to obtain the unbiased analyte concentration when the matrix of the sample is completely unknown. A spectral region where the interferent behaviour can be considered linear at three wavelengths must be chosen. The method uses the analytical signal data at these three wavelengths, usually situated in the maxima region of the analyte. Two procedures are proposed in order to know and to locate this behaviour for the unknown interferent. Several binary and ternary mixtures of phenol, 4-chlorophenol and 4-chloro-3-methylphenol as representative examples have been assayed, with accurate (less than 3% relative e…
A mathematical model based on the limit dilution method to obtain linear calibration curves which eliminate the matrix effect in quantitative analysi…
1995
Abstract We propose a mathematical model from an analytical application viewpoint inspired in the limit dilution method. The theoretical development of the model and its results are given. The model shows that there is a linear relation between the inverse of fluorescence intensity and the inverse of the dilution factor; each analytic system (sample, diluent and analyte) is characterised by a general linear function which is easily obtained. The analytical applications arising from this linearity are of great importance in X-ray fluorescence analysis. The following immediate applications are proposed: direct procurement of the total correction factor Y/H, rapid calculation of the fluorescen…
Quantitative electron probe microanalysis of metallic oxide mixtures applying an empirical calibration technique
1997
Abstract An analytical procedure is proposed for the independent quantitative chemical analysis of each element in the presence of other elements in the matrix of a sample by Energy Dispersive Electron Probe Microanalysis. For this purpose, an empirical calibration technique (which we shall call here the JABO method), which studies the variation of the X-ray intensities in terms of the analyte concentration in a chemical system with a complex matrix, is established. The methodology consists of the modification of the unknown sample by addition of a diluent, an internal standard and the analyte itself (dilution-addition method). A mathematical model is proposed to calculate the K parameters …
Towards an automatic lab-on-valve-ion mobility spectrometric system for detection of cocaine abuse.
2017
A lab-on-valve miniaturized system integrating on-line disposable micro-solid phase extraction has been interfaced with ion mobility spectrometry for the accurate and sensitive determination of cocaine and ecgonine methyl ester in oral fluids. The method is based on the automatic loading of 500μL of oral fluid along with the retention of target analytes and matrix clean-up by mixed-mode cationic/reversed-phase solid phase beads, followed by elution with 100μL of 2-propanol containing (3% v/v) ammonia, which are online injected into the IMS. The sorptive particles are automatically discarded after every individual assay inasmuch as the sorptive capacity of the sorbent material is proven to b…
Determination of amphetamines in hair by integrating sample disruption, clean-up and solid phase derivatization
2016
The utility of matrix solid phase dispersion (MSPD) for the direct analysis of amphetamines in hair samples has been evaluated, using liquid chromatography (LC) with fluorescence detection and precolumn derivatization. The proposed approach is based on the employment of MSPD for matrix disruption and clean-up, followed by the derivatization of the analytes onto the dispersant-sample blend. The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. Different conditions for MSPD, analyte purification and solid phase derivatization have been tested, using amphetamine (AMP), methamphetamine (MET), ephedrine (EPE) and 3,4-methylenedioxymethamphetamine (MDMA)…
Science based calibration for the extraction of 'analyte-specific' HPLC-DAD chromatograms in environmental analysis
2010
Multivariate science based calibration (SBC) has been applied to the resolution of overlapped peaks in liquid chromatography with diode array detection (LC-DAD). Complex river water samples spiked with 11 pharmaceutical substances resulted in poorly resolved chromatograms containing additional peaks from interfering matrix compounds and a change in the background absorbance due to the mobile phase gradient. Applying the present multivariate approach it was possible to resolve all 11 analytes from overlapping peaks, obtaining linear calibration lines (R2 > 0.96). Recovery percentages on spiked samples ranged between 74.6 and 113.5%, which are quite satisfactory taking into account the low co…
Assessment of oxidative damage to proteins and DNA in urine of newborn infants by a validated UPLC-MS/MS approach
2014
The assessment of oxidative stress is highly relevant in clinical Perinatology as it is associated to adverse outcomes in newborn infants. This study summarizes results from the validation of an Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (UPLC-MS/MS) method for the simultaneous quantification of the urinary concentrations of a set of endogenous biomarkers, capable to provide a valid snapshot of the oxidative stress status applicable in human clinical trials, especially in the field of Perinatology. The set of analytes included are phenylalanine (Phe), para-tyrosine (p-Tyr), ortho-tyrosine (o-Tyr), meta-tyrosine (m-Tyr), 3-NO2-tyrosine (3NO(2)-Tyr), 3-Cl-tyrosine (3Cl-T…
The H-point and generalized H-point standard additions methods for flow injection procedures.
1997
This paper establishes the fundamentals of the H-point standard additions method (HPSAM) and generalized H-point standard additions method (GHPSAM) in the flow injection technique. Two kinds of analytical signals can be employed, FIA peaks and spectra. Different analytical problems have been studied: determinations of one analyte in the presence or absence of matrix effect when different blank features are present, and determination of two analytes in the presence of blank bias error affecting the development of one of them. The determination of chloride with mercury thiocyanate which presents a matrix effect, and the determinations of calcium and/or magnesium with arsenazo III are examined…