Search results for "Extraction"
showing 10 items of 2072 documents
Simultaneous determination of third-generation synthetic cannabinoids in oral fluids using cyclodextrin-silica porous sorbents
2022
Abstract A microporous material made of cyclodextrin units covalently immobilized into a silica network has found an innovative bioanalytical application in the sample clean-up and simultaneous isolation of three synthetic cannabinoids (ADB-CHMICA, MMB-CHMICA, and MDMB-CHMCZCA) from human oral fluid through solid-phase extraction. The subsequent quantitation is carried out using liquid chromatography coupled to fluorescence detection. The optimized experimental procedure gives recoveries ranging from 76% to 96% in oral fluid samples spiked with the studied cannabinoids at the µg L-1 level. High selectivity is obtained through the extraction procedure due to the presence of cyclodextrin in t…
The PAH composition of surface sediments from Stagnone coastal lagoon, Marsala (Italy)
2006
Abstract This paper examines the presence, distribution, nature and sources of 22 Aromatic Hydrocarbons (PAHs), which are important environmentally and toxicologically, in sediments from the Stagnone coastal lagoon at Marsala (Italy). Analysis was performed by gas chromatography/mass spectrometry (GC/MS) with selected ion monitoring (SIM). The total concentration of polycyclic aromatic hydrocarbons ranged from 72 to 18381 μg/kg of dry matrix. The relative standard deviation (RSD) of the replicates on the concentrations of individual compounds ranged from 5% to 20%. The accuracy of method was estimated by analyzing “blank” samples added of known quantities of analytes and the recover percent…
Comparative study of the determination of trimethylamine in water and air by combining liquid chromatography and solid-phase microextraction with on-…
2005
This work describes a new approach for the determination of trimethylamine (TMA) in water and air by liquid chromatography (LC). The assay is based on the employment of a solid-phase microextraction (SPME) fiber for sampling and for derivatization of the analyte with the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC). The fiber, with a Carbowax-templated resin -50mum coating, was first immersed into a solution of the reagent. Once loaded with the reagent, the fiber was immersed into the water samples or exposed to the air samples in order to extract and to derivatize the analyte. Finally, the fiber was placed into a HPLC-SPME interface to desorb and transfer the TMA-FMOC derivat…
Non-chromatographic speciation of toxic arsenic in fish
2004
Abstract A rapid, sensitive and economic method has been developed for the direct determination of toxic species of arsenic present in fish and mussel samples. As(III), As(V), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were determined by hydride generation–atomic fluorescence spectrometry using a series of proportional equations without the need of a chromatographic previous separation. The method is based on the extraction of arsenic species from fish through sonication with HNO3 3 mol l−1 and 0.1% (m/v) Triton and washing of the solid phase with 0.1% (m/v) EDTA, followed by direct measurement of the corresponding hydrides in four different experimental conditions. The li…
A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos.
2005
Abstract A FTIR methodology has been developed for the simultaneous determination of Cypermethrin and Chlorpyrifos in pesticide commercially available formulations. The method involves the extraction of both active principles with CHCl3 and direct measurement of the peak area values between 1747 and 1737 cm−1 corrected with a baseline defined at 2000 cm−1 for Cypermethrin and peak height values established at 1549 cm−1 corrected using a baseline situated at 1650 cm−1 for Chlorpyrifos. The limits of detection achieved were of the order of 0.7 and 0.4% (w/w), and the relative standard deviation 0.4 and 0.2% for Cypermethrin and Chlorpyrifos, respectively. The developed procedure provided stat…
Spectrophotometric determination of carbaryl by on-line elution after its preconcentration onto polyurethane foam.
2000
Abstract An analytical methodology has been developed for the UV-spectrophotometric determination of carbaryl in waters after its preconcentration onto a polyether type polyurethane foam followed by on-line elution. The aforementioned strategy offers an easy way for in-field sampling and to improve the analytical sensitivity. Several chemical and flow variables (mass of sorbent, sample flow rate, sample volume and carrier flow rate) were studied to ensure the best performance of the system. Recovery studies, carried out on natural water samples spiked with known amounts of carbaryl at concentration levels between 250 and 500 μg l−1, provided recovery percentages between 94 and 105%. A detec…
Thermal lens spectrometric determination of cerium with oxine
1991
Abstract The spectrophotometric and photothermal (TLS) procedures for cerium determination using 8-hydroxyquinoline (oxine), after extraction into chloroform, are compared. Photothermal measurements are made using a coaxial pump/probe thermal lens spectrometer. The use of high-purity reagents at low concentrations permits a decrease in the TLS blank signal and noise, leading to a limit of detection of 9 × 10−9 M (cerium extract concentration), 40-fold lower than the spectrophotometric value. The dynamic range extended up to 6 × 10−7 M and the relative standard deviation for 5 × 10−7 M cerium was 3.9%.
Eficacia analgésica del diclofenaco sódico vs. ibuprofeno después de la extracción quirúrgica de un tercer molar inferior incluido
2004
-Objetivo: En este estudio evaluamos la eficacia analgésica del diclofenaco sódico en comparación con el ibuprofeno, después de la extracción quirúrgica de un tercer molar inferior incluido. -Diseño de estudio: Los pacientes que participaron en el estudio fueron distribuidos de forma aleatoria en dos grupos. Uno fue el grupo ibuprofeno y el otro el grupo diclofenaco. La intervención practicada fue la extracción quirúrgica de un tercer molar inferior cuya dificultad fue determinada en función del grado de inclusión en todos los pacientes. Las variables registradas fueron la intensidad del dolor y la necesidad de medicación de rescate durante un periodo de una semana. Los registros se realiza…
A method for the determination of dimethylamine in air by collection on solid support sorbent with subsequent derivatization and spectrophotometric a…
2005
A new method for dimethylamine determination in air is reported. The proposed assay is based on the employment of C18-packed solid phase extraction cartridges for sampling. The retained amine is then derivatized inside the cartridges with the reagent 1,2-naphthoquinone-4-sulfonate. By observing the coloured area of the cartridge, a semiquantitative estimation of the amine can be made. It was also possible to distinguish between primary and secondary amines by visual inspection. Quantitative tests entailed desorption from the cartridges of the derivatives formed, and measurement of the absorbance of the collected extracts. The selected conditions were applied to quantify dimethylamine up to …
Derivatization of amines in solid-phase extraction supports with 9-fluorenylmethyl chloroformate for liquid chromatography
1997
Abstract A new method based on reaction in solid-phase extraction cartridges with 9-fluorenylmethyl chloroformate is described for improved derivatization of amines prior to liquid chromatography. The effects of the reaction conditions, the kinetics of the reaction and the kind of packing material on the derivatization have been evaluated. The reliability of the described approach has been tested by derivatizing propylamine, diethylamine, diethanolamine, glycine, glutamic acid, p-aminobenzoic acid and β-phenylethylamine. Reaction yields compared with those of the analogous solution derivatizations were in the 44–169% range, and satisfactory linearity was achieved at concentrations of the am…