Extraction, solid phase using silica-based adsorbent

A cleanup procedure is usually carried out to remove co-extracted matrix components that may interfere in the chromatographic analysis or be detrimental to the analytical instrument. The cleanup procedure is dependent on the nature of the analyte, the type of sample to be analyzed, and the selectivity and sensitivity of the analytical instrument used in the analysis. Preliminary purification of the sample extracts prior to chromatographic separation involves liquid-liquid partitioning and/or solid-phase extraction (SPE) using charcoal/Celite, Elorisil, carbon black, silica, or aminopropyl-silica based adsorbents or gel permeation chromatography (GPC). 

Solid phase extraction. With the availability of pre-prepared cartridges of silica-based adsorbents, the use of solid phase extraction has increased in the last few years although the technique has been in use for many years for the isolation of many biochemicals, e.g. amino acids, catecholamines. In essence it is a version of chromatography conditions for the selective adsorption of the analytes (column, solvent, pH, etc.) are chosen, the sample is applied to a column, washed and the analytes selectively eluted with appropriate solvents. Since the columns are disposable there is no need to worry about protein contamination or infection. The adsorbents available cover an even wider range than HPLC materials since they are not required to withstand high back pressures. It is possible... 

In addition to electrophoresis-based collection of DNA in microchannels (see Section 7.7.3), adsorbents have been used to collect and purify DNA. In these cases, microchannels are generally used because of the small quantity of material requiring collection. Using solid phase extraction, sorbent particles of nano- and micro-silica and micro-sized octadecylsilica were immobilized using sol-gel chemistry to hU the microchannels of the microfluidic device [194]. DNA as well as several organic compoimds were evaluated for adsorption and desorption. They showed excellent adsorption, but poor recovery because they were difficult to extract. 

Some techniques that combine the properties of extraction and cleanup are supercritical fluid extraction (SEE) and matrix solid-phase dispersion (MSPD). Supercritical fluids, i.e., at a temperature and pressure in excess of their critical point, have unique properties for selective extraction of analytes from a sample. Solid samples are mixed with an inert dispersant, such as hydromatrix, and the mixture packed into the cell of the SEE apparatus. The sample is extracted with supercritical CO2, with or without addition of organic modifier, and the extracted analytes may be collected inline or offline on suitable adsorbents (Figure 3). Further cleanup of the sample extract may be performed using SPE. MSPD is based on intimate mixing of animal tissue sample with a bonded silica, such as Cig, and packing of the blended material into a column from which interferences can be eluted by washing with solvents and the analytes eluted using a selective solvent. 

Gas chromatography, coupled with flame-ionisation, electron capture (for halogenated species) and mass spectrometric detectors, is the most popular tool for determination of SVOCs in melted snow samples [44]. A prerequisite is the efficient separation of the analytes from the aqueous matrix, which can be accomplished using filtration onto quartz fibre filters and sohd phase extraction [88]. Solid phase micro-extraction, which utilises equihbrium-based adsorption of analytes onto a polymer fibre bundle, has also been proposed and tested in laboratory studies [13, 89]. Both methods allow for an efficient transfer into the injection port of a gas chromatograph without water contamination. Directly coupled inlet sampler with GC-EID instrumentation has also been used [90]. The air sample was pre-concentrated using adsorbents (Carbotrap B, Carbosieve), followed by heating and collection on a cryofocuser (a fused silica capillary tube packed with... 

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