Solid phase extraction water partitioning

Water solubility, dissociation constant(s) and n-octanol/water partition coefficients allow one to predict how an analyte may behave on normal-phase (NP), reversed-phase (RP), or ion-exchange solid-phase extraction (SPE) for sample enrichment and cleanup. 

Analytical methods for parent chloroacetanilide herbicides in soil typically involve extraction of the soil with solvent, followed by solid-phase extraction (SPE), and analysis by gas chromatography/electron capture detection (GC/ECD) or gas chromatog-raphy/mass spectrometry (GC/MS). Analytical methods for parent chloroacetanilides in water are similarly based on extraction followed by GC with various detection techniques. Many of the water methods, such as the Environmental Protection Agency (EPA) official methods, are multi-residue methods that include other compound classes in addition to chloroacetanilides. While liquid-liquid partitioning was used initially to extract acetanilides from water samples, SPE using... 

A soil sample (10 g) was extracted by mechanically shaking with methanol-deionized water. This mixture was filtered and a portion was removed for partitioning into toluene-hexane. A phenyl solid-phase extraction (SPE) cartridge was employed... 

When liquid samples such as serum, plasma, milk, or honey are not to be extracted using direct liquid-liquid partitions with organic solvents but through use of solid-phase extraction or matrix solid-phase dispersion techniques, dilution with water (323, 324), phosphate buffer saline (325), or phosphoric acid (326, 327) is often the only sample preparation procedure applied. Milk analysis sometimes requires further pretreatment for fat removal (328). Centrifugation at about 7000g at 4-10 C for 20 min is the usually applied procedure for making the fat floating on top of milk readily eliminated. 

Nakamura, M., Suzuki, T., Amano, K., Yamada, S. (2001) Relation of sorption behavior of agricultural chemicals in solid-phase extraction with their n-octanol/water partition coefficients evaluated by high-performance liquid chromatography (HPLC). Anal. Chim. Acta 428, 219-226. 

In a subsequent study, solvent partitioning and solid-phase extraction techniques were used to produce a partial ly -pur If led extract (15). The first step In the purification scheme Involved partitioning of a highly oonoentrated ethanol 1c extract of house fly ovaries between chloroform and water. Further processing of the chloroform layer (I.e., evaporation, solvent exchange, and filtration through a bed of Porapac Q) eventually produced a methanol 1c extract with a 23-fold Increeee In OH activity over the crude extract. 

Pesticides are extracted from grapes with acetonitrile using a singlephase extraction followed by liquid-liquid partitioning formed by addition of MgS04 and NaCl. Removal of residual water and clean up are performed simultaneously by using dispersive solid-phase extraction. The pesticide extract was analyzed by GC/MS. 

Reversed-phase solid-phase extraction (SPE) involves the partitioning of organic solutes from a polar mobile phase, such as water, into a nonpolar solid phase, such as the C-18 sorbent (Fig. 4.1). Partitioning involves the interaction of the solute within the chains of the stationary phase, which may be a C-18 hydrocarbon, C-8 hydrocarbon, or the polymeric sorbents (such as styrene-divinylbenzene). The word hydrophobic mechanism is commonly... 

Methods for the extraction of pesticides from water exploit the partitioning of analytes between the aqueous phase and a water-immiscible solvent (Liquid-Liquid Extraction [LLE]) or an adsorbent material (Solid-Phase Extraction [SPE]). The SPE technique has been shown to offer several advantages over LLE and it is included in most of recent analytical protocols devoted to analyzing contaminants in water samples. Nevertheless, the LLE technique is still used in many environmental laboratories. 

Solid phase micro extraction (SPME) is a techniques in which a silica fiber coated with a thin film of polymer is brought into contact with an aqueous matrix where the organics in solution partition onto the fiber. The fiber is subsequently placed into the injector of a GC where the heat causes the release of analyte onto the column. This has been applied to endosulfan (a- and (3-) and endosulfan sulfate in water with limits of detection of less than 0.3 pg/L reported (Magdic and Pawliszyn 1996). 

Clarification of extracts can be accomplished with Carrez reagents (44). Purification has been performed by solid phase or partition. Wu et al. (47) absorbed saccharin onto ODS-4 cartridges and then eluted with methanol phosphate buffer. Puttemans et al. (28,50) extracted saccharin from soft drinks and yogurt by ion-pair extraction with tri-n-octylamine and back-extraction to an aqueous phase with perchlorate. Tereda and Sakabe (48) used cetrimide and Sep-Pak Cl8 in the cleanup of saccharin in coffee drink. The column was preconditioned with methanol, water, and 5 mM cetrimide. The sample, diluted in phosphate buffer pH 3.0 containing cetrimide was poured into the cartridge, washed with water, and eluted with acetonitrile water (1 1, v/v). Moriyasu et al. (40) added n-propylammonium bromide to the extract, passed it through a Bond Elut Cl 8 column, and eluted the sweetener with a mixture of methanol-water (4 6, v/v). The eluate was passed through a Bond Elut SAX column and washed with 0.5% phosphoric acid and water, and the sweetener was eluted with 0.3 N hydrochloric acid. 

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