Search results for "sample preparation"
showing 10 items of 343 documents
Microwave-assisted extraction of OCPs, PCBs and PAHs concentrated by semi-permeable membrane devices (SPMDs)
2005
Abstract Microwave-assisted extraction (MAE) has been evaluated as an alternative to dialysis for extraction of some water-borne hydrophobic contaminants sampled by semi-permeable membrane devices (SPMDs). Seven organochlorine pesticides (OCPs), 11 polychlorinated biphenyls (PCBs) and 13 polycyclic aromatic hydrocarbons (PAHs) were accumulated in SPMDs at nanogram levels and extracted with three 3-min irradiation cycles with 33 mL of a solvent mixture hexane–water (10:1,v/v) in each cycle. The developed MAE method gave for all analytes investigated statistically comparable extraction yields with those found by dialysis carried out with a total volume of 250 mL hexane for 48 h at room temper…
Headspace-Liquid Phase Microextraction for Attenuated Total Reflection Infrared Determination of Volatile Organic Compounds at Trace Levels
2010
A combination of headspace (HS) sampling and liquid phase microextraction (LPME) has been successfully developed to solve sensitivity problems in attenuated total reflection (ATR) infrared determination of volatile organic compounds (VOCs). The HS sampling facilitates the selective extraction of the target volatile analytes from the sample matrix, while the liquid phase microextraction allows their preconcentration prior to infrared analysis. The direct determination of extracted analytes in the acceptor solvent provides high preconcentration factors of the order of 200 with a reduced consumption of organic solvents and a minimum generation of wastes, being thus the developed methodology a …
Selective solid phase extraction of a drug lead compound using molecularly imprinted polymers prepared by the target analogue approach
2002
Molecularly imprinted polymers have been evaluated at the sample clean-up stage in the analysis of a drug lead compound. In order to circumvent quantification problems related to bleeding of the template, a structurally related analogue of the latter was used. This was selected based on criteria related to interaction site location, solubility, availability and stability of the analogue. Selection of suitable polymerisation conditions was then made using a small batch format (ca. 50 mg) and rapid assessment of binding in the equilibrium mode. It was found that the amount of template could be greatly reduced compared to the conventional protocol, requiring only 5 μmol of template per gram of…
Inductively coupled plasma atomic emission spectrometric determination of arsenic in mussel products
1993
A precise, accurate procedure is proposed for the determination of arsenic in mussel products by inductively coupled plasma atomic emission spectrometry. Organic matter is destroyed by dry ashing. Experimental conditions for the determination of arsenic were selected and an interference study was carried out. The methodology developed has a detection limit of 0.1 μg g−1, a relative standard deviation of 3%, and a recovery percentage of 98±2%. The accuracy of the method was checked by analysis of a certified sample of NIST oyster tissue (certified 14.0±1.2 μg g−1; found 14.1±1.1 μg g−1). The proposed procedure was used to analyze real samples of mussel products.
In-tube solid-phase microextraction coupled by in valve mode to capillary LC-DAD: Improving detectability to multiresidue organic pollutants analysis…
2009
Abstract A simple and fast capillary chromatographic method has been developed to identify and quantify organic pollutants at sub-ppb levels in real water samples. The major groups of pesticides (organic halogens, organic phosphorous, and organic nitrogen compounds), some hydrocarbons (polycyclic aromatic hydrocarbons), phthalates and some phenols such as phenol and bisphenol A (endocrine disruptors) were included in this study. The procedure was based on coupling, in-tube solid-phase microextraction (IT-SPME) by using a conventional GC capillary column (95% methyl–5% phenyl substituted backbone, 80 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve to capillary liquid chromatog…
Indirect analysis of urea herbicides from environmental water using solid-phase microextraction.
2000
We described here a solid-phase microextraction procedure used to extract six urea pesticides-- chlorsulfuron, fluometuron, isoproturon, linuron, metobromuron and monuron--from environmental samples. Two polydimethylsiloxanes and a polyacrylate fiber (PA) are compared. The extraction time, pH control, addition of NaCl to the water and the influence of organic matter such as humic acid on extraction efficiency were examined to achieve a sensitive method. Determination was carried out by gas chromatography with nitrogen-phosphorus detection. The proposed method requires the extraction of 2 ml of sample (pH 4, 14.3%, w/v, NaCl) for 60 min with the PA fiber. The limits of detection range from 0…
CHEMICAL ANALYSIS FOR SPECIFIC COMPONENTS | Micronutrients and Other Minor Meat Components
2014
The chemical analysis of the many micronutrients (minerals and vitamins) and other components such as cholesterol and enzymes in meat and meat products are addressed in this article. The sample preparation and main methods for the determination of these components are reviewed and described as well as their respective major advantages and disadvantages.
Modern trends in solid phase extraction: New sorbent media
2016
Abstract Based on the recently published literature, this review provides an update of the most important features and application of formats and devices employed in solid phase extraction (SPE). Special attention was paid on new trapping media proposed in SPE prior the chromatography analysis, based on the use of nanostructured materials, including carbon nanomaterials, electrospun nanofibers, dendrimes and magnetic nanoparticles, molecular recognition sorbents, as aptamers, immunosorbents, molecular imprinted polymers, ion imprinting polymers, metal-organic frameworks and restricted access materials. Discussions on the present limitations as well as expected future trends of the new trapp…
Vibrational spectroscopy in soil and sediment analysis
2014
The literature concerning the use of vibrational spectroscopy for soil and sediment analysis, published in the last years, has been revised in order to provide a picture of the strengths and weaknesses of these direct techniques to characterize soil composition and properties. Many soil components as water, organic matter, like humic substances, and minerals, can be determined together with physicochemical parameters as pH, conductivity or redox potential. The main strategies to obtain sample spectra and to extract, as many as possible, useful information were evaluated, taking into account the progress on chemometrics and discussing the whole analytical process, from sampling to sample pre…
Carbohydrates from Chemical Pulps: Characterization by Capillary Zone Electrophoresis
2006
Capillary zone electrophoresis (CZE) is one of the novel separation techniques, being applicable, for example, to virtually all important biomass-derived monosaccharides. However, in spite of this fact the utilization of this technique in the pulp and paper industry is currently rather limited. In this chapter practical guidance and some application examples are given to show how carbohydrate material (polysaccharides, oligosaccharides, and neutral and acidic monosaccharides) in pulps and spent liquors can be analyzed by CZE. Emphasis is placed on sample preparation and separation conditions including comparison with other separation methods, such as gas chromatography (GC) and high-perform…