Solid-phase extraction approach

Zang X. et al., 2005. A novel online solid-phase extraction approach integrated with a monolithic column and tandem mass spectrometry for direct plasma analysis of multiple drugs and metabolites. Rapid Commun Mass Spectrom 19 3259. 

In contrast to the solid-phase extraction approach, only nonpolar Cis-deriva-tized silica has been used as the sorbent in matrix solid-phase dispersion technique. This technique has been successfully applied in the determination of furazolidone in meat (66), milk (181), and swine tissues (180). 

Two approaches have been used to separate the analyte from its matrix in particulate gravimetry. The most common approach is filtration, in which solid particulates are separated from their gas, liquid, or solid matrix. A second approach uses a liquid-phase or solid-phase extraction. 

For the analysis of organic additives in polymeric materials, in most cases, prior extraction will be necessary. Depending on the nature of the additive, many different approaches are employed. These include soxhlet extraction with organic solvent or aqueous media, total sample dissolution followed by selective precipitation of the polymer leaving the additive in solution, assisted extraction using pressurised systems, ultrasonic agitation and the use of supercritical fluids. In trace analysis, solid phase extraction (SPME) from solution or solvent partition may be required to increase the analyte concentration. 

In a related approach from the same laboratory, the perfluorooctylsulfonyl tag was employed in a traceless strategy for the deoxygenation of phenols (Scheme 7.82) [94], These reactions were carried out in a toluene/acetone/water (4 4 1) solvent mixture, utilizing 5 equivalents of formic acid and potassium carbonate/[l,T-bis(diphe-nylphosphino)ferrocene]dichloropalladium(II) [Pd(dppf)Cl2] as the catalytic system. After 20 min of irradiation, the reaction mixture was subjected to fluorous solid-phase extraction (F-S PE) to afford the desired products in high yields. This new traceless fluorous tag has also been employed in the synthesis of pyrimidines and hydantoins. 

The most common (off-line) sample preparation procedures after protein precipitation are solid phase extraction and liquid-liquid extraction. Multiple vendors and available chemistries utilize 96-well plates for solid phase extraction systems and liquid-liquid extraction procedures. Both extraction process can prepare samples for HPLC/MS/MS assay. Jemal et al.110 compared liquid-liquid extraction in a 96-well plate to semi-automated solid phase extraction in a 96-well plate for a carboxylic acid containing analyte in a human plasma matrix and reported that both clean-up procedures worked well. Yang et al.111 112 described two validated methods for compounds in plasma using semi-automated 96-well plate solid phase extraction procedures. Zimmer et al.113 compared solid phase extraction and liquid-liquid extraction to a turbulent flow chromatography clean-up for two test compounds in plasma all three clean-up approaches led to HPLC/MS/MS assays that met GLP requirements. 

Ding J. and Neue U.D., 1999. A new approach to the effective preparation of plasma samples for rapid drug quantitation using online solid phase extraction mass spectrometry. Rapid Commun Mass Spectrom 13 2151. 

Pozo O.J. et al., 2006. Efficient approach for the reliable quantification and confirmation of anitbiotice in water using online solid-phase extraction liquid chromatography/tandem mass spectrometry. J Chromatogr A 1103 83. 

Another example of nitrogen-based ligands can be found in a new family of ligands that were developed in solution through the use of solid-phase extractions (SPE) (Scheme 22) (49). In this approach, a building block strategy was taken in... 

One of the most widely used techniques across all disciplines is solid-phase extraction (SPE). A simple approach to SPE is shown in Fig. 2.3. These columns provide rapid extraction, minimize emulsion problems, and eliminate most sample handling. 

Currently, perhaps the most promising approach based on the use of molecularly imprinted polymers is solid phase extraction (SPE). Traditionally, when complex samples require a clean-up/enrichment step prior to high-resolution analysis,... 

Sample preparation refers to a family of solid/liquid handling techniques to extract or to enrich analytes from sample matrices into the final analyte solution. While SP techniques are well documented, few references address the specific requirements for drug product preparations, which tend to use the simple dilute and shoot approach. More elaborate SP is often needed for complex sample matrices (e.g., lotions and creams). Many newer SP technologies such as solid-phase extraction... 

Postigo C, de Alda MIL, Barcelo D et al (2010) Analysis and occurrence of selected medium to highly polar pesticides in groundwater of Catalonia (NE Spain) an approach based on on-line solid phase extraction-liquid chromatography-electrospray-tandem mass spectrometry detection. J Hydrol 383 83-92... 

Jenkins et al. developed a capillary electrophoresis system for the measurement of iohexol as a marker of the glomerular filtration rate (GFR) with a run time of 5.25 min and a coefficient of variation (CV) of 4.3% at 80 mg L" [121]. The GFR, calculated from the plasma clearance, had a reproducibility of 5.47 %. A similar approach (liquid chromatography-mass spectrometry with positive electrospray ionization after enrichment by solid phase extraction) was applied by Putschew et al. for the determination of iodinated contrast agents in treatment plant effluents and surface waters [118]. 

For analyzing amphenicol residues in liquid samples such as milk, a pretreatment centrifugation step for fat removal is usually required (21, 22). Dilution of milk samples with water prior to solid-phase extraction cleanup is also often needed (23, 24). Semisolid samples such as muscle, kidney and liver, require, however, more intensive sample pretreatment. The most popular approach for tissue break-up is through use of a mincing and/or a homogenizing apparatus. 

Solid-phase extraction seems to be more suitable for multiresidue cleanup. This procedure has become the method of choice for isolation and/or cleanup of -lactam antibiotics from biological matrices, because it requires low solvent consumption, it is generally less time-consuming and labor-intensive, and offers a variety of alternative approaches that allow better extraction of the more hydrophilic -lactam antibiotics such as ampicillin. It is usually performed using reversed-phase Ci8 (69-71, 80-83, 90, 92-94, 99, 107, 112-116, 121-125) or Cg (103), anion-exchange (95, 124), and polar diol (95) or alumina (101, 113) sorbents. In recent applications, some workers demonstrated the potential of online solid-phase extraction in the determination of monobasic penicillins in bovine muscle tissues using a reversed-phase Cis 5 m cartridge and an automated... 

Cleanup of macrolides and lincosamides from coextracted material can also be accomplished with solid-phase extraction columns. Nonpolar sorbents such as XAD-2 resin (148) or reversed-phase sorbents (133, 134, 137, 141, 142) are usually employed in solid-phase extraction. In the latter case, ion-pairing with pentanesulfonic acid can also be applied for enhancing retention onto the hydro-phobic Ci8 material (154). However, these sorbents are not always effective for efficient cleanup of liver and kidney extracts. The basic character of macrolides and lincosamides suggests that cation-exchange sorbents such as aromatic-sulfonic acid (145,147), or polar sorbents such as silica (144,152,153), aminopropyl (139), or diol (149-151), can be powerful alternative approaches for isolation and/or cleanup of these compounds. 

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