Search results for "Chemical analysis."
showing 10 items of 308 documents
Application of solid-phase microextraction combined with derivatization to the determination of amphetamines by liquid chromatography
2004
This work evaluates the utility of solid-phase microextraction (SPME) in the analysis of amphetamines by liquid chromatography (LC) after chemical derivatization of the analytes. Two approaches have been tested and compared, SPME followed by on-fiber derivatization of the extracted amphetamines, and solution derivatization followed by SPME of the derivatives formed. Both methods have been applied to measure amphetamine (AP), methamphetamine (MA), and 3,4-methylenedioxymethamphetamine (MDMA), using the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) and carbowax-templated resin (CW-TR)-coated fibers. Data on the application of the proposed methods for the analysis of different kin…
In-tube solid phase microextraction coupled to miniaturized liquid chromatography for both, noble metal nanoparticle assessment and sensitive plasmon…
2021
Abstract Colorimetric localized surface plasmon resonance (LSPR) as analytical response is applied for a wide number of chemical sensors and biosensors. However, the dependence of different factors, such as size distribution of nanoparticles (NPs), shape, dielectric environment, inter-particle distance and matrix, among others, can provide non-reliable results by UV–vis spectrometry in complex matrices if NP assessment is not carried out, particularly at low levels of analyte concentrations. Miniaturized liquid chromatography, capillary (CapLC) and nano (NanoLC), coupled on line with in-tube solid phase microextraction (IT-SPME) is proposed for the first time for both, controlling suitabili…
Control of matrix interferences by multiple linear regression models in the determination of arsenic and lead concentrations in fly ashes by inductiv…
2010
A multiple linear regression technique was used to evaluate and correct the matrix interferences in the determination of As and Pb concentrations in fly ashes by inductively coupled plasma optical emission spectrometry. The direct determination of As and Pb in SRM 1633b by ICP-OES failed to obtain the certified concentrations, except in a couple of cases. However, it proved possible to use the multiple linear regression (MLR) technique to correct the determined concentrations to a satisfactory level. This method of correction is based on the multiple regression line obtained from the analysis of 19 synthetic mixtures of matrix and analyte elements (Al, As, Ca, Fe, Pb, and Si) at five concen…
Identification and determination of synthetic cannabinoids in herbal products by dry film attenuated total reflectance-infrared spectroscopy.
2017
A new procedure has been developed for the identification and quantitative determination of synthetic cannabinoids in illicit herbal preparations. The methodology is based on the use of attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) measurement of sample extracts with 2-propanol drying 5µL of the extracts onto the ATR crystal. The qualitative identification was carried out on the 2-propanol extract after identification of the herbal matrix, followed by its subtraction and using a cut-off criterion of 75%. Quantitative determination was made by univariate calibration using the absorbance of the band located at 1520cm-1 of the spectrum. Four different cannabin…
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…