Janusz Pawliszyn

Applications of solid-phase microextraction in food analysis.

Food analysis is important for the evaluation of the nutritional value and quality of fresh and processed products, and for monitoring food additives and other toxic contaminants. Sample preparation, such as extraction, concentration and isolation of analytes, greatly influences the reliable and accurate analysis of food. Solid-phase microextraction (SPME) is a new sample preparation technique using a fused-silica fiber that is coated on the outside with an appropriate stationary phase. Analyte in the sample is directly extracted to the fiber coating. The SPME technique can be used routinely in combination with gas chromatography (GC), GC-mass spectrometry (GC-MS), high-performance liquid chromatography (HPLC) or LC-MS. Furthermore, another SPME technique known as in-tube SPME has also been developed for combination with LC or LC-MS using an open tubular fused-silica capillary column as an SPME device instead of SPME fiber. These methods using SPME techniques save preparation time, solvent purchase and disposal costs, and can improve the detection limits. This review summarizes the SPME techniques for coupling with various analytical instruments and the applications of these techniques to food analysis.

Evolution of solid-phase microextraction technology

The main objective of this contribution is to describe the development of the concepts, techniques and devices associated with solid-phase microextraction, as a response to the evolution of understanding of the fundamental principles behind this technique. The discussion begins with an historical perspective on the very early work conduced almost a decade ago. As new fundamental understanding about the functioning of the technology developed, new ways of constructing and using the SPME devices evolved.

Applications of solid phase microextraction

Foreword Contents Contributors Glossary Calibration and quantitation by SPME Quantitative aspects of SPME Quantitation by SPME before reaching a partition equilibrium Coatings and interfaces SPME coupled to capillary electrophoresis Selectivity in SPME Properties of commericial SPME coatings Sol-gel technology for thermally stable coatings in SPME Solid versusliquids coatings Physiochemical applications Application of SPME to study sorption phenomena on dissolved humic organic matter The use of SPME to measure free concentrations and phospholipid/water and protein/water partition coefficients Estimation of hydrophobicity of organic compounds Environmental applications Air sampling with SPME The application of sPME in water analysis The application of SPME to pestivide residue analysis Inter-laboratory validation of SPME for the quantitative analysis of aqueous samples SPME for the determination of organochlorine pestivides in natural waters Determination of sulfur-containing compounds in wastewater Analysis of creosote and oil in aqueous contaminations by SPME Direct analysis of solids using sPME Analysis of solid samples by hot water extraction -SPME Field analysis by SPME Organometallic speciation by combining aqueous phase derivatization with SPME-GC-FPD-MS Metal speciation by SPME-CGC-ICPMS The application of SPME-LC-MS to the determination of contaminants in complex environmental matrices SPME-HPLC of environmental pollutants Analysis of industrial pollutants in environmental samples Food, flavour, fragrance and pheromone applications Analysis of food and plant volatiles Application of SPME to measure volatile metabolites produced by staphylococcus carnosus and staphylococcus xylosus Application of SPME methods for the determination of volatile wine aroma compounds in view of the varietal characterization Analysis of vodkas and white rums by SPMS-GC-MS Analysis of food volatiles using SPME Analysis of volatile contaminants in foods Determination of pesticides in foods by automated SPMS-GC-MS SPME in the study of chemical communication in social wasps Pharmaceutical, clinical and forensic applications Propyl chloroformate derivatisation and SPME-GC for screening Of amines in urine Isolation of drugs and poisons in biological fluids by SPME On-fiber derivatization for analysis of steroids by SPME and GC-MS SPME-Quadrupole ion trap mass spectrometry for the determination of drugs of abuse in biological matrices Analysis of drugs in biological fluids using SPME SPME-Microcolumm LC: Application to toxicological drug analysis Optimization of drug analysis by SPME Applications of SPME for the biomonitoring of human exposure to toxic substances Applications of SPME in criminal investigations Reaction monitoring SPME-GC-MS detection analysis of maillard reaction products SPME investigation of intermediates produced during biodegradation of contaminated materials Related techniques Infrared spectroscopic detection for SPME SPME in Near-IR Fiber-optic Evanescent Field Absorption Spectroscopy: A Method for Rapid, Remote In situ Monitoring of Nonpolar Organic Compounds in Water Author Index

Microextraction of drugs.

This review will attempt to provide an overview as well as a theoretical and practical understanding of the use of microextraction technologies for drug analysis. The majority of the published reports to date focus on the use of fibre solid-phase microextraction and so the review is significantly focused on this technology. Other areas of microextraction such as single drop and solvent film microextraction are also described. Where there are insufficient examples in the literature to illustrate important concepts, examples of non-drug analyses are presented. The review is intended for readers new to the field of microextraction or its use in drug extraction, but also provides an overview of the most recent advances in the field which may be of interest to more experienced users. Particular emphasis is placed on the effect various sample matrices have on extraction characteristics.

Rapid determination of polyaromatic hydrocarbons and polychlorinated biphenyls in water using solid-phase microextraction and GC/MS.

Solid-phase microextraction (SPME) was investigated as a solvent-free alternative method for the extraction and analysis of nonpolar semivolatile analytes. Analytes were extracted into a polymeric phase immobilized onto a fusedsilica fiber. The fiber was then inserted directly into the injector of a gas chromatograph, and the analytes were thermally desorbed. This new technique allows sampling directly from the source (lake, drinking fountain, etc.) and, therefore, eliminates the loss of analytes through adsorption onto container walls and saves transport costs

Nondestructive Sampling of Living Systems Using in Vivo Solid-Phase Microextraction

Nondestructive Sampling of Living Systems Using in Vivo Solid-Phase Microextraction Gangfeng Ouyang,* Dajana Vuckovic, and Janusz Pawliszyn* MOEKeyLaboratory of Aquatic Product Safety/KLGHEI of Environment andEnergyChemistry, School ofChemistry andChemical Engineering, Sun Yat-sen University, Guangzhou 510275, China Department of Chemistry, University of Waterloo, Waterloo, Ontario N2L 3G1, Canada

Recent developments in solid-phase microextraction

AbstractThe main objective of this review is to describe the recent developments in solid-phase microextraction technology in food, environmental and bioanalytical chemistry applications. We briefly introduce the historical perspective on the very early work associated with the development of theoretical principles of SPME, but particular emphasis is placed on the more recent developments in the area of automation, high-throughput analysis, SPME method optimization approaches and construction of new SPME devices and their applications. The area of SPME automation for both GC and LC applications is particularly addressed in this review, as the most recent developments in this field have allowed the use of this technology for high-throughput applications. The development of new autosamplers with SPME compatibility and new-generation metal fibre assemblies has enhanced sample throughput for SPME-GC applications, the latter being attributed to the possibility of using the same fibre for several hundred extraction/injection cycles. For LC applications, high-throughput analysis (>1,000 samples per day) can be achieved for the first time with a multi-SPME autosampler which uses multi-well plate technology and allows SPME sample preparation of up to 96 samples in parallel. The development and evolution of new SPME devices such as needle trap, thin-film microextraction and cold-fibre headspace SPME have offered significant improvements in performance characteristics compared with the conventional fibre-SPME arrangement. FigurePhoto of a high-throughput multi-fibre SPME PAS autosampler

Solid-phase microextraction of nitrogen-containing herbicides

Abstract A solid-phase microextraction (SPME) method, coupled with GC-MS, GC-NPD and GC-FID has been developed for the analysis of 22 nitrogen-containing herbicides in water. A polar(acly(acrylate) coated fiber was used to extract the analytes directly from the samples over the concentration range 0.1 to 1000 ng/ml. Limits of detection with each of the detectors were determined to be in the ng/l, to sub ng/l levels. Some applications of the method have been demonstrated for soil samples and wine samples with GC-MS and the latter was quantified by standard addition.

Preparation and applications of polypyrrole films in solid-phase microextraction.

Polypyrrole (PPY) and poly-N-phenylpyrrole (PPPY) films were prepared and applied for solid-phase microextraction (SPME). The extraction properties of the new films to volatile organic compounds were examined using an SPME device coupled with GC-flame ionization detection. A PPY-coated capillary was applied for in-tube SPME to evaluate its extraction efficiency towards less volatile compounds and ionic species. The porous surface structures of the films, revealed by scanning electron microscopy, provided high surface areas and allowed for high extraction efficiency. Compared with commercial SPME stationary phases, the new phases showed better selectivity and sensitivity toward polar, aromatic, basic and anionic compounds, due to their inherent multifunctional properties. In addition, PPY and PPPY films showed different selectivity to various groups of compounds studied, indicating that the selectivity of the films could be modified by introducing a new functional group (phenyl in PPPY) into the polymer. For in-tube SPME, the PPY-coated capillary showed superior extraction efficiency to commercial capillaries for a variety of compounds, demonstrating its potential applications for a wide range of analytes when coupled with HPLC. The sensitivity and selectivity of the films for SPME could be tuned by changing the film thickness. These results are in line with both the theoretical expectations and the results obtained by other methods, which indicate not only that PPY films can be used as new stationary phases for SPME. but also that SPME method may provide an alternative tool for studying materials like polypyrrole.

Analysis of environmental air samples by solid-phase microextraction and gas chromatography/ion trap mass spectrometry.

A simple and efficient method for extraction and concentration of volatile organic compounds (VOCs) in air using solid-phase microextraction (SPME) has been developed. The analytes are extracted directly from the air and desorbed into a gas chromatograph for separation and quantification. This method requires minimal sample preparation time and, therefore, is suitable for on-site air monitoring. Analytes can be detected at the part per trillion (ppt) to sub part per billion (ppb) concentration levels with an ion trap mass spectrometer. The precision of the method was determined to be 1.5-6% relative standard deviation (RSD). Temperature and humidity effects were studied experimentally, and the method was compared with an EPA-validated method for selected VOCs. The SPME technique may be suitable for both spot sampling and integral exposure overtime sampling. Integrated sampling has been successfully applied to the identification and quantification of toxic volatile organic compounds in environmental air samples.