1995 McBryde Medal Award Lecture Solid phase microextraction – a unique tool for chemical measurements

Abstract

The paper presents recent advances in solid phase microextraction (SPME). The method utilizes a small fused silica fibre coated with a suitable polymeric stationary phase for analyte extraction from various matrices. The fibre is mounted in a syringe-like holder for protection. SPME has been used for the characterization of polymeric coating properties. Infinite-dilution weight-fraction activity coefficients have been determined for five solutes in two different stationary phases. Their values correlate well with the structure of the analytes and the coating. Other SPME uses include simultaneous determination of 60 pesticides in liquid matrices. A comparison between SPME, liquid extraction, and Soxhlet extraction for the analysis of Atrazine, Simazine, and Metolachlor in well water, as well as Metolachlor in soil samples, produced similar results for all three methods. The solvent-free character of SPME enables its use as sample introduction technique for fast GC analysis. Separations of BTEX in less than 9 s, and of volatile compounds described in EPA method 624 in 2.5 min, are described. SPME has also been used for the analysis of tetraethyllead and Pb(I1) in water. Before the analysis, lead is derivatized with sodium tetraethylborate, and the tetraethyllead formed is extracted from sample headspace. Sub-ppb detection limits have been achieved with FID. Finally, SPME has been coupled to HPLC with the use of a specially designed interface. The combination has been tested on samples of polyaromatic hydrocarbons and surfactants in water. Very good precision of retention times and peak areas has been achieved.

Fibers Coated with Molecularly Imprinted Polymers for Solid-Phase Microextraction

“…The technique, which has proven its usefulness beside the conventional extraction techniques such as liquid−liquid extraction, Soxhlet extraction, and solid-phase extraction, is simple, relatively inexpensive, and compatible with analytical separation systems such as gas chromatography, liquid chromatography, and capillary electrophoresis . Reviews on the theory, practice, and state of the art of SPME have been published. − SPME is based on the partitioning of analytes between the sample and the extraction phase, which is fixed on the surface of a fused-silica fiber. − In our group, direct-immersion SPME has been used for the extraction of drugs from biological samples such as urine and plasma . Sampling conditions were systematically optimized in order to increase the partitioning of analytes toward the coated fiber.…”

Solid Phase Microextraction for Field Sampling

“…Solid phase micro extraction (SPME) fibres have improved in quality over the last few years and are now commonly used for introducing analytes into a gas chromatograph [1,2]. The technique utilises a one cm length of fused silica coated with an adsorbent or absorbent phase.…”

An Improved Interface for Coupling Solid-Phase Microextraction (SPME) to High Performance Liquid Chromatography (HPLC) Applied to the Analysis of Explosives

“…SPME preserves the advantages of SPE while eliminating the disadvantages of plugging and solvent use [3]. Pawliszyn and coworkers have described solid-phase microextraction in detail and demonstrated the technique to be a rapid, simple, and solventfree sample preparation method [3][4][5][6]. SPME has been applied to the analysis of a wide range of volatile and semi-volatile compounds utilizing the effective combination of SPME and primarily GC analysis.…”