Search results for "Extraction"
showing 10 items of 2072 documents
On-line speciation of mercury in fish by cold vapour atomic fluorescence through ultrasound-assisted extraction
2004
A fully mechanized procedure has been developed for the speciation of mercury in fish samples by using cold vapour atomic fluorescence spectrometry (CV-AFS). Sample slurries in an acid mixture in the presence of a surfactant and with traces of K2Cr2O7, were injected into a flow system, sonicated and merged with 1 ml of an oxidant mixture of KBr/KBrO3 heated at 50 °C in a water bath and total Hg determined by CV-AFS. Sonicated sample slurries were also measured, in the absence of KBr/KBrO3, in order to obtain a second series of data which could be employed to establish the concentrations of free Hg(II). Different compositions of the acidic extractant solutions were evaluated by mixing HCl, H…
In-tube solid-phase microextraction and liquid chromatography using a monolithic column for the selective determination of residual ethylenediamine i…
2009
The selective determination of the diamine ethylenediamine (EDA) in the presence of a higher amount of residual dimethylamine in cationic polymers has been developed. The strategy uses both a solution derivatization with a selective agent of primary amines such as o-phthaldialdehyde-N-acetyl-L-cysteine (OPA-NAC) and an in-tube solid-phase microextraction (IT-SPME) coupled to liquid chromatography (LC). A 70 cm long, 0.32 mm internal diameter, and 3 microm thick commercially available capillary column coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane was employed to replace the injection loop of a Rheodyne injection valve. A volume of 1 mL of derivatized sample was passed thro…
A cost-effective method for estimating di(2-ethylhexyl)phthalate in coastal sediments.
2013
This study describes the development of a new method for the analysis of di(2-ethylhexyl)phthalate (DEHP) using 0.1-0.3 g of sediment sample, based on matrix solid phase dispersion (MSPD) using C18 as dispersant phase (0.4 g) and acetonitrile-water as eluting solvent (3.4 mL 1:3.25, v/v). No evaporation step is required. 3 mL of extracts were processed on-line by in-tube solid phase microextraction (IT-SPME) coupled to capillary liquid chromatography (CapLC) and diode array detector (DAD). A short analytical column Zorbax SB C18 (35×0.5 mm, 5 μm) provided suitable results. FTIR-ATR was employed for characterizing sediment samples and MSPD procedure. The total analysis time was less than 20 …
Rapid screening of organophosphorus pesticides in honey and bees by liquid chromatography—Mass spectrometry
2002
Twenty-two organophosphorus pesticide residues were simultaneously determined in honey and honeybee samples by extraction procedures based on solid-phase and liquid chromatography-atmospheric pressure chemical ionization-mass in positive and negative ionization modes. Pesticides in honeybee samples were extracted by matrix solid phase dispersion with C18 silica and subsequently eluted with a mixture of dichloromethane-methanol (85∶15, v/v). The average recoveries from spiked honeybees (0.5–10 μg g−1) ranged from 76% for coumaphos to 100% for omethoate, with relative standard deviations between 3 and 17%. Limits of detection were ≤0.13 μg g−1 and limits of quantification were ≤0.43 μg g−1. H…
Automated on-line in-tube solid-phase microextraction-assisted derivatization coupled to liquid chromatography for quantifying residual dimethylamine…
2008
Abstract A method for the analysis of dimethylamine (DMA) by automated in-tube solid-phase microextraction (IT-SPME)-supported chemical derivatization coupled with high-performance liquid chromatography was developed. Extraction, derivatization and desorption were studied by using a capillary coated with 95% polydimethylsiloxane and 5% polydiphenylsiloxane. Solution derivatization and automated IT-SPME derivatization using 9-fluorenylmethyl chloroformate (FMOC) were compared. The proposed procedure provided adequate linearity, accuracy and precision in the 0.2–2.0 μg/mL concentration interval, and the limit of detection (LOD) was 50 ng/mL. The main advantages of the proposed procedure are: …
Evaluation of a Real-Time PCR Assay for the Detection and Quantification of Group Spores in Food
2010
A procedure based on quantitative real-time PCR was evaluated for the detection and quantification of Bacillus cereus spores. Several methods for DNA isolation, such as various heat treatments and germination solutions, were evaluated on spore suspensions of representative strains of the B. cereus group. Overall, the commercially available DNeasy tissue kit yielded the maximum amount of DNA. The procedure also was used to construct calibration curves for different food matrices, with a wide spore quantification range of 5 log units using serial dilutions of spore suspensions of B. cereus CECT 148T. The detection limit for B. cereus in artificially contaminated liquid egg and reconstituted i…
Determination of pesticides in soil samples by solid phase extraction disks
1993
A systematic study comparing the methodology and analytical results obtained in an investigation of seven pesticide residues (Molinate, Atrazine, Carbofuran, Pirimicarb, Prometryn, Malathion and Tetrachlorvinphos) in soil samples is reported. Solid-phase extraction (SPE) using glass columns and 47 mm disks of octyl and octadecyl-bonded silica was used in the pesticide analysis. The best extraction efficiency and clearest extracts are obtained with C8 disks. The analyses were carried out by capillary gas chromatography with nitrogen and phosphorus detection. Recovery experiments were performed at ppb levels in spiked soil samples. The average recoveries of the compounds were 53–77%. Detectio…
Amphetamine and methamphetamine determination in urine by reversed-phase high-performance liquid chromatography with sodium 1,2-napthoquinone 4-sulfo…
1995
A rapid method is described for the identification and determination of amphetamine and methamphetamine in human urine samples by liquid chromatography with UV-Vis detection. The samples were transferred onto a C18 solid-phase extraction column and chromatographed on a Hypersil ODS RP C18, 5 microns (250 x 4 mm I.D.) with an acetonitrile-water elution gradient containing propylamine. Under these conditions, the amines are eluted with a short retention time. The procedure has been applied to the determination of amphetamine and methamphetamine in the range 0.3-4.0 micrograms/ml in spiked urine samples. The detection limits at 280 nm were 4 and 2 ng/ml for amphetamine and methamphetamine, res…
Determination of caffeine in tea samples by Fourier transform infrared spectrometry
2002
A sustainable and environmentally friendly procedure has been developed for the FTIR determination of caffeine in tea leaf samples. The method is based on the extraction with ammonia and CHCl3 and direct determination of caffeine on the chloroform extracts using peak height absorbance measurements at 1658.5 cm(-1) and external calibration. The method provides a sensitivity of 0.2142 absorbance units mg(-1) mL and a limit of detection of 1 mg L(-1), corresponding to 0.002% m/m caffeine in tea leaves. As compared with a reference procedure, based on UV absorbance measurement at 276 nm after low pressure column chromatography, the developed procedure reduces the consume of CHCl3 by a factor of…
A rapid HPLC assay for zearalenone in laboratory cultures ofFusarium graminearum
1993
A high pressure liquid chromatographic (HPLC) method to determine zearalenone in corn contaminated withFusarium graminearum is described. After extraction with methanol-water and solvent partition, samples were cleaned up by applying the extract to a disposable silica cartridge and by eluting the toxin with a mixture of hexane/dry ethyl ether (5/5). Separation was achieved by a reverse phase μBondapak C18 column followed by fluorescence detection using an excitation wavelength at 274 nm and an emission wavelength at 440 nm. Detection limit was about 5 ng. Recoveries ranging from 85.37 to 100.97%, in standard solutions range 30–0.5 µg/ml, were found.