Search results for "Microextraction"
showing 10 items of 144 documents
Off-line solid-phase microextraction and capillary electrophoresis mass spectrometry to determine acidic pesticides in fruits.
2003
A method based on solid-phase microextraction (SPME) and capillary electrophoresis/mass spectrometry (CE/ MS) is described for determining simultaneously five acidic pesticides (o-phenylphenol, ioxynil, haloxyfop, acifluorfen, picloram) in fruits. The CE device is coupled to an electrospray interface by a commercial sheath-flow adapter. Emphasis is placed on fulfillment of the speed and sensitivity requirements. The best separation is achieved using 32 mM ammonium formate/acid formic buffer at pH 3.1, with a working voltage of 25 kV. The MS detection of the five pesticides was performed in negative ionization mode. Full-scan spectra with base peaks corresponding to [M-H]- were obtained exce…
Determination of N-nitrosodiethanolamine in cosmetic products by reversed-phase dispersive liquid-liquid microextraction followed by liquid chromatog…
2016
A new analytical method for the determination of N-nitrosodiethanolamine (NDELA), a very harmful compound not allowed in cosmetic products, is presented. The method is based on a new approach of dispersive liquid-liquid microextraction (DLLME) useful for extraction of highly polar compounds, called reversed-phase DLLME (RP-DLLME), followed by liquid chromatography-ultraviolet/visible (LC-UV/Vis) determination. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the optimized conditions, a mixture of 750µL of acetone (disperser solvent) and 125µL of water (extraction solvent) was rapidly injected into 5mL of toluene sample solution. The e…
A headspace solid-phase microextraction method of use in monitoring hexanal and pentane during storage: Application to liquid infant foods and powder…
2006
The determination of two secondary lipid oxidation compounds (hexanal and pentane) in liquid infant foods using a headspace solid-phase microextraction gas chromatographic (HS-SPME-GC) method has been developed and validated. The HS-SPME analytical conditions (fibre position, equilibration and sampling times) were selected. The analytical parameters of the method (linearity: hexanal from 2.48 to 84.78 ng/g, pentane from 6.21 to 79.55 ng/g; precision: hexanal 2.87%, pentane 2.343.46%; recovery: hexanal 106.60%, pentane 95.39%; detection limit: hexanal 3.63 ng and pentane 4.2 ng) demonstrate the usefulness of the method. Once optimized, the method was applied to liquid infant foods based on m…
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 …
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: …
Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS.
2010
Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1 ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative stan…
Matrix effects on solid-phase microextraction of organophosphorus pesticides from water
1997
Abstract This study develops a method for solid-phase microextraction (SPME) of eight organophosphorus pesticides, diazinon, fenthion, fenitrothion (sumithion), methyl-parathion, parathion, methyl-trithion, ethion and triazophos, from water. Determination is carried out by gas chromatography with nitrogen-phosphorus detection. To perform the SPME, poly(dimethylsiloxane) and polyacrylate fibers were initially compared on the basis of their absorption capacities for the selected pesticides, and polyacrylate was selected to accomplish the rest of assays. The main factors affecting the SPME process such as memory effect, stirring rate, extraction temperature and absorption-time profile were stu…
Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography …
2020
The degradation kinetics and residual levels of the sulfonylurea herbicide tribenuron-methyl (TBM) in different environmental waters were studied using in tube-solid phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nanoLC) and UV diode array detection (DAD). This approach combines the high extraction efficiency of IT-SPME using polymeric coatings reinforced with metal oxide nanoparticles and the high sensitivity attainable by nanoLC, making possible the determination of TBM at low ppb levels (limit of detection, 0.25 ppb) without altering the sample matrix. The present study demonstrated that the preservation of the sample properties is essential to ensure accu…
Determination of organophosphorus pesticides in honeybees after solid-phase microextraction.
2001
A method based on solid-phase microextraction (SPME) followed by gas chromatography with nitrogen-phosphorus detection was developed for the purpose of determining 18 organophosphorus pesticide residues in honeybee samples (Apis mellifera). The extraction capacities of polyacrylate and poly(dimethylsiloxane) fibers were compared. The main factors affecting the SPME process, such as the absorption time profile, salt, and temperature, were optimized. The method involved honeybee sample homogenization, elution with an acetone:water solution (1:1) and dilution in water prior to fiber extraction. Moreover, the matrix effect on the extraction was evaluated. In samples spiked at the 0.2 mg kg(-1) …