Recent developments in solid-phase microextraction (original) (raw)
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Developments in liquid-phase microextraction
TrAC Trends in Analytical Chemistry, 2003
The development of faster, simpler, inexpensive and more environmentally friendly sample-preparation techniques is an important issue in chemical analysis. Recent research trends involve miniaturisation of the traditional liquid-liquid extraction (LLE) principle by greatly reducing the acceptor-to-donor phase ratio. One of the emerging techniques in this area is liquid-phase microextraction (LPME), where a hollow fibre impregnated with an organic solvent is used to accommodate or protect microvolumes of acceptor solution. This novel methodology proved to be an extremely simple, low-cost and virtually solvent-free sample-preparation technique, which provided a high degree of selectivity and enrichment by additionally eliminating the possibility of carry-over between runs. This article presents the different modes and hollow-fibre configurations of LPME, followed by an up-to-date summary of its applications. The most important parameters and practical considerations for method optimisation are also discussed. The article concludes with a comparison of this novel method with solid-phase microextraction (SPME) and singledrop microextraction (SDME). #
Protocol for solid-phase microextraction method development
Nature protocols, 2010
Solid-phase microextraction (SPME) is a sample preparation method developed to solve some of the analytical challenges of sample preparation as well as sample introduction and integration of different analytical steps into one system. Since its development, the utilization of SPME has addressed the need to facilitate rapid sample preparation and integrate sampling, extraction, concentration and sample introduction to an analytical instrument into one solvent-free step. This achievement resulted in fast adoption of the technique in many fields of analytical chemistry and successful hyphenation to continuously developing sophisticated separation and detection systems. However, the facilitation of high-quality analytical methods in combination with SPME requires optimization of the parameters that affect the extraction efficiency of this sample preparation method. Therefore, the objective of the current protocol is to provide a detailed sequence of SPME optimization steps that can be a...
Developments in hollow fiber based liquid-phase microextraction: principles and applications
Microchimica Acta, 2012
Hollow fiber liquid-phase microextraction (HF-LPME) offers an efficient alternative to classical techniques for sample preparation and preconcentration. Features include high selectivity, good enrichment factors, and improved possibilities for automation. HP-LPME relies on the extraction of target analytes from aqueous samples into a supported liquid membrane (SLM) sustained in the pores of the wall of a porous hollow fiber, and then into an acceptor phase (that can be aqueous or organic) in the lumen of the hollow fiber. After extraction, the acceptor solution is directly subjected to a chemical analysis. HP-LPME can be performed in either the 2-or 3-phases mode. In the 2-phase mode, the organic solvent is present both in the porous wall and inside the lumen of the hollow fiber. In the 3-phase mode, the acceptor phase can be aqueous and this results in a conventional 3-phase system compatible with HPLC or capillary electrophoresis. Alternatively, the acceptor solution is organic and this represents a 3-phase extraction system with two immiscible organic solvents that is compatible with all common analytical instruments. In HP-LPME methods based on the use of SLMs, the mass transfer occurs by passive diffusion, and high extraction yields as well as efficient extraction kinetics are obtained by applying a pH gradient. In addition, active transport can be performed by using carrier or applying an electrical potential across the SLM. Due to high analyte preconcentration, excellent sample clean-up, and low consumption of organic solvent, HF-LPME has a large application potential in areas such as drug analysis and environmental monitoring. This review focuses on the fundamentals of extraction principles, technical implementations, and future trends in HF-LPME.
Solid‐phase microextraction: a powerful sample preparation tool prior to mass spectrometric analysis
Journal of mass spectrometry, 2004
Sample preparation is an essential step in analysis, greatly influencing the reliability and accuracy of resulted the time and cost of analysis. Solid-Phase Microextraction (SPME) is a very simple and efficient, solventless sample preparation method, invented by Pawliszyn in 1989. SPME has been widely used in different fields of analytical chemistry since its first applications to environmental and food analysis and is ideally suited for coupling with mass spectrometry (MS). All steps of the conventional liquid-liquid extraction (LLE) such as extraction, concentration, (derivatization) and transfer to the chromatograph are integrated into one step and one device, considerably simplifying the sample preparation procedure. It uses a fused-silica fibre that is coated on the outside with an appropriate stationary phase. The analytes in the sample are directly extracted to the fibre coating. The SPME technique can be routinely used in combination with gas chromatography, high-performance liquid chromatography and capillary electrophoresis and places no restriction on MS. SPME reduces the time necessary for sample preparation, decreases purchase and disposal costs of solvents and can improve detection limits. The SPME technique is ideally suited for MS applications, combining a simple and efficient sample preparation with versatile and sensitive detection. This review summarizes analytical characteristics and variants of the SPME technique and its applications in combination with MS.
Automation of solid-phase microextraction on a 96-well plate format
Journal of Chromatography A, 2007
Studies have been performed assessing the feasibility and characterizing the automation of solid-phase microextraction (SPME) on a multi-well plate format. Four polycyclic aromatic hydrocarbons (PAHs), naphthalene, fluorene, anthracene and fluoranthene, were chosen as test analytes to demonstrate the technique due to their favorable partition coefficients, K fw , between polydimethylsiloxane (PDMS) extraction phases and water. Four different PDMS configurations were investigated regarding their suitability. These included (i) a PDMS membrane; (ii) a multi-fiber device containing lengths of PDMS-coated flexible wire; (iii) a stainless steel pin covered with silicone hollow fiber membrane and (iv) commercial PDMS-coated flexible metal fiber assemblies. Of these configurations, the stainless steel pin covered with silicone tubing was chosen as a robust alternative. An array of 96 SPME devices that can be placed simultaneously into a 96-well plate was constructed to demonstrate the high-throughput potential when performing multiple microextractions in parallel. Different agitation methods were assessed including magnetic stirring, sonication, and orbital shaking at different speeds. Orbital shaking whilst holding the SPME device in a stationary position provided the optimum agitation conditions for liquid SPME. Once the analytes had been extracted, desorption of the analytes into an appropriate solvent was investigated. Liquidphase SPME and solvent desorption on the multi-well plate format is shown to be a viable alternative for automated high-throughput SPME analysis compatible with both gas-and liquid-chromatography platforms.
Overview of Different Modes and Applications of Liquid Phase-Based Microextraction Techniques
Processes
Liquid phase-based microextraction techniques (LPµETs) have attracted great attention from the scientific community since their invention and implementation mainly due to their high efficiency, low solvent and sample amount, enhanced selectivity and precision, and good reproducibility for a wide range of analytes. This review explores the different possibilities and applications of LPμETs including dispersive liquid–liquid microextraction (DLLME) and single-drop microextraction (SDME), highlighting its two main approaches, direct immersion-SDME and headspace-SDME, hollow-fiber liquid-phase microextraction (HF-LPME) in its two- and three-phase device modes using the donor–acceptor interactions, and electro membrane extraction (EME). Currently, these LPμETs are used in very different areas of interest, from the environment to food and beverages, pharmaceutical, clinical, and forensic analysis. Several important potential applications of each technique will be reported, highlighting it...
Separations, 2019
The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published in the last 5 years (2014-2019) thus providing the reader with information about the current state-of-the-art and the future potential directions of the research in pollutant monitoring using SPME. To this end, we revised the studies focused on the investigation of persistent organic pollutants (POPs), pesticides, and emerging pollutants (EPs) including personal care products (PPCPs), in different environmental, food, and bio-clinical matrices. We especially emphasized the role that SPME is having in contaminant surveys following the path that goes from the environment to humans passing through the food web. Besides, this review covers the last technological developments encompassing the use of novel extraction coatings (e.g., metal-organic frameworks, covalent organic frameworks, PDMS-overcoated fiber), geometries (e.g., Arrow-SPME, multiple monolithic fiber-SPME), approaches (e.g., vacuum and cold fiber SPME), and on-site devices. The applications of SPME hyphenated with ambient mass spectrometry have also been described.
Bioapplications of solid phase microextraction
2001
Solid phase microextraction ( S m ) has experienced rapid development in the recent decade. Especi aU y for volatile org anic compounds in environment al sample anaiysis, SPME features the special advantages of cornbining sampling, sample preparation, and sample transfer into a single step. However, due to the complexity of biomatrices and non-volatile and polar nature of the dmg compounds, most dmg analyses by SPME and in-tube SPME are still in their primary analytical optimization stage. Based on the fact that SPME is an equilibrium extraction process, in this thesis, SPME has been successfûlly applied for dmg-protein studies. The theory of protein binding study by headspace SPME was fmt illustrated with selected alkylbenzene compounds binding to bovine serum albumin (BSA) as the model system. Drug binding to human serum albumin (HSA) was subsequentl y studied by direct SPME due to the non-volatile and polar nature of the model h g , diazepam. This method can be easily adapted to ...