Handbook Of Solid Phase Microextraction Pdf To Jpg
The relatively new technique of solid phase microextraction (SPME) is an important tool to prepare samples both in the lab and on-site. SPME is a 'e;green'e; technology because it eliminates organic solvents from analytical laboratory and can be used in environmental, food and fragrance, and forensic and drug analysis.
This handbook offers a thorough background of the theory and practical implementation of SPME. SPME protocols are presented outlining each stage of the method and providing useful tips and potential pitfalls. In addition, devices and fiber coatings, automated SPME systems, SPME method development, and In Vivo applications are discussed.
This handbook is essential for its discussion of the latest SPME developments as well as its in depth information on the history, theory, and practical application of the method. Practical application of Solid Phase Microextraction methods including detailed stepsProvides history of extraction methods to better understand the processSuitable for all levels, from beginning student to experienced practitioner.
Hiroyuki Kataoka, in, 2017 1.3.3 Solid-Phase MicroextractionSPME 20, 21, 32, 33, 41, 47, 67, 68, 129–148 is an effective sample preparation technique for integrating several operations such as sample collection, extraction, analyte enrichment, and isolation from sample matrices, and has been used to extract analytes from gaseous, liquid, and solid samples. SPME technology is a nonexhaustive technique based on the partition equilibrium of analytes between the sample matrix and the extraction phase. The SPME process consists of two basic steps: (1) partitioning of analytes between the extraction phase and the sample matrix, and (2) subsequent desorption of concentrated extracts into an analytical instrument. Because sampling, extraction, preconcentration, and sample introduction into an analytical instrument can be performed in a single step, SPME methods provide quantitative or semiquantitative data results. SPME can be roughly classified as static in-vessel and dynamic in-flow microextraction. Available configurations for SPME devices are illustrated in Fig.
SPME usually involves fibers and capillary tubes coated with an appropriate stationary phase. Fiber SPME ( Fig. 1.9A) is the most widely used technique, in which the analyte in the sample is directly extracted onto an outer fiber coatings by absorption or adsorption.
Alternative static in-vessel microextraction techniques include stir bar sorptive extraction (SBSE) ( Fig. 1.9B), and TFME ( Fig. In-tube SPME is an efficient dynamic in-flow microextraction technique that uses a capillary column as an extraction device ( Fig.
1.9D), with sample analytes extracted directly onto an inner capillary coatings. Other methods include syringe SPME such as solid-phase dynamic extraction (SPDE) ( Fig. 1.9E-a) and microextraction in a packed syringe (MEPS) ( Fig. 1.9E-b), and in-tip SPME ( Fig. These SPME techniques can be performed manually or automatically and are easily coupled to chromatographic systems. Florin Marcel Musteata, Dajana Vuckovic, in, 2012Solid-phase microextraction (SPME) approaches have been widely used for invasive and non-invasive in vivo studies.
The target analytes investigated to date include environmental pollutants, pharmaceuticals, pheromones and metabolites, and the studies show the versatility and capability of this technique. The feasibility and applicability of in vivo SPME techniques depend on the development and commercialisation of devices and extraction phases suitable for different types of applications.
Handbook Of Solid Phase Microextraction Pdf To Jpg Online
Proper design of SPME devices and accessorial systems can make the techniques more convenient and more applicable. The development of biocompatible extraction phases improved the sensitivity, selectivity and compatibility of in vivo SPME techniques. The development of SPME calibration methods in recent years has enabled accurate quantification even in situations when equilibrium cannot be reached and/or experimental conditions cannot be controlled or replicated for calibration purposes. SPME is an effective sample preparation method for global metabolomic studies of biofluids and tissues. Tissue metabolomics is particularly interesting for the study of damaged tissues such as tumours in search of novel biomarkers because the concentration of such biomarkers is expected to be higher in such tissue than in surrounding areas. For this type of studies, in vivo SPME presents a less invasive sampling method over the traditional methods, which require invasive biopsy followed by solvent extraction.
SPME also provides improved spatial resolution sampling, which is important when dealing with such heterogeneous specimens, and spatially resolved fibres using separated portions of coatings can play an important role in this type of application. Pawliszyn, in, 2000Solid-phase microextraction (SPME), developed by Pawliszyn and co-workers in 1990, is a new sample preparation technique using a fused-silica fibre that is coated on the outside with an appropriate stationary phase.
The analyte in the sample is directly extracted onto the fibre coating. The method saves preparation time, solvent purchase and disposal costs, and can improve the detection limits. It has been used routinely in combination with gas chromatography (GC) and GC/mass spectrometry (GC/MS), and successfully applied to a wide variety of compounds, especially for the extraction of volatile and semi-volatile organic pollutants from water samples. SPME was also introduced for direct coupling with high performance liquid chromatography (HPLC) and LC/MS in order to analyse weakly volatile or thermally labile compounds not amenable to GC or GC/MS. The SPME/HPLC interface, equipped with a special desorption chamber, is utilized for solvent desorption prior to HPLC analysis, instead of thermal desorption in the injection port of the GC. Moreover, a new SPME/HPLC system known as in-tube SPME, was recently developed using an open-tubular fused-silica capillary column as the SPME device in place of the SPME fibre.
In-tube SPME is suitable for automation, and automated sample handling procedures not only shorten the total analysis time, but also usually provide better accuracy and precision relative to manual techniques. Nilsson, in, 2000Solid-phase microextraction (SPME) is a technique for the extraction of organic compounds from gaseous, aqueous and solid matrices such as many environmental samples. It is rapid and simple, which makes it ideal for automation and in situ measurements, and no harmful solvents are used.
The principle of SPME is equilibration of the analytes between an organic polymeric phase coated on to a fused-silica fibre and the sample matrix. The parameters of importance for the equilibration process are described below and various environmental applications are discussed. Traditionally, SPME has been combined with analysis by gas chromatography (GC), and mainly aqueous samples have been analysed. This combination has proved to be sensitive, accurate and precise for the quantitative analysis of volatile organic compounds and different classes of pesticides. Solid samples can also be analysed by SPME in spite of the stronger matrix effects, and recently SPME has been coupled with liquid chromatography (LC) for the analysis of polar pesticides.
Gangfeng Ouyang, in, 2012The solid phase microextraction (SPME) technique has been widely used for the analysis of environmental pollutants in air, water, soil and sediment samples, using on-site or off-site analytical approaches. It has been proven very useful for the analysis of a variety of chemicals in the environment, including volatile organic contaminants (VOCs), SVOCs, pesticides, herbicides, organometallic compounds and amines. Headspace–solid phase microextraction (HS–SPME), direct injection–solid phase microextraction (DI–SPME), membrane-protected SPME and in-tube SPME have been used for the analysis of a wide range of environmental matrices, including air, water, soil and sediment samples.
Off-site analysis of environmental samples is now performed in a fully automated fashion using autosamplers or robots. On-site sampling and analysis of environmental samples with SPME is facilitated by development of sampling devices and calibration methods for both grab sampling and long-term monitoring. The development of new SPME calibration methods has accelerated the applications of SPME for on-site sampling and analysis. On-site analysis requires portable and solvent-free sample preparation approaches that work well with micro-instruments. The main remaining challenge is the development of certified methods that would facilitate broader application in high-throughput environmental laboratory applications of this green extraction technology. Janusz Pawliszyn, in, 2012 3.5.5 SPME–Nanospray MS InterfaceSPME was also successfully interfaced to mass spectrometry via electronanospray tips.
99 For the in situ extraction of peptides from the tryptic digests, trypsin was immobilised both on steel wires and on the inside wall of a vial. The devices were incubated together with the RAM–SPME devices and a protein (casein) solution. After the protein digestion, the resulting peptides were analysed by SPME–nanospray MS.
The vial approach provided the best results; up to eight peptides could be identified, which corresponds to a sequence coverage of 58%. The limit of detection of SPME–nanospray MS for the extraction of peptides from an aqueous solution was about 50 fmol/mL. The results demonstrate that the direct coupling of SPME to nanospray can reduce analysis time and is an attractive alternative to conventional approaches like Zip-Tip purification. Gangfeng Ouyang, in, 2012 Publisher SummarySolid-phase microextraction (SPME) is a solvent-free sample preparation technique that integrates sampling, isolation, and concentration.
Its simplicity of use, relatively short sample processing time, and fiber reusability have made SPME an attractive choice for many analytical applications. SPME has been widely applied to the sampling and analysis of environmental, food, aromatic, metallic, forensic, and pharmaceutical samples. Calibration is a process relating the measured analytical signal to the concentration of analyte in the sample matrix. Several methods have been used for the calibration of SPME.
In addition to traditional calibration methods (i.e., external standard, internal standard, and standard addition), the existing SPME calibration methods include equilibrium extraction, exhaustive extraction, and diffusion-based calibration. In this chapter, details and characteristics of these calibration methods will be discussed. SPME calibration technique suitability depends on the application, the number of samples to be analyzed, and the availability of a mass spectrometry instrument in the laboratory. The development of SPME calibration methods is based on an understanding of fundamental principles governing the mass transfer of analytes in multiphase systems.
Theories have been developed to understand the principal processes involved in SPME by applying the basic fundamentals of thermodynamics and mass transfer kinetics. Quantification using calibration curves does not require extensive sample preparation, but the sampling procedure and chromatographic conditions must remain constant for both the sample and the standard solutions, and if there are matrix effects, a blank sample matrix is necessary. Andrews, in, 2000 Future DevelopmentsSPME is currently poised to become one of the major sample preparation methods for aqueous environmental samples in the future. The advantages that it offers, such as ease of use, no solvent and no plugging, make it a potential replacement for many of the liquid–liquid and SPE methods currently used.
The expansion of SPME to the analysis of other analytes which are currently difficult to partition into the fibre coatings is another expected trend. This may be achieved by the development of new fibre coatings or by coupling existing coatings with derivatization or complexation reactions.The future for SPME in the analysis of solids is less certain. Unless more robust SPME methods than those currently described are found, the replacement of Soxhlet extraction by SPME seems unlikely. Additionally, the problem of carryover is a cause for concern with the analysis of higher molecular weight analytes. Currently the cost of SPME fibres does not allow them to be used as single-use devices.
This may, of course, change in the future and single-use fibres are the surest way to ensure that there is no carryover. Kyle, in, 2017 3.3.3 Solid Phase Microextraction (SPME)SPME is a relatively new extraction technique that involves a sorbent-coated rod or fiber that is placed into the sample vial. Compounds from liquid or gaseous samples are adsorbed onto the fiber. Once the extraction is complete, the SPME fiber is inserted into the heated injection port of the GC-MS, where analytes are thermally desorbed from the fiber and enter the analytical column. The fibers are typically composed of a 1–2 cm length of fused silica coated with polar and nonpolar sorbents similar to those available in WCOT GC columns. SPME is most often applied for the extraction and analysis of volatile analytes and pesticides during food and environmental monitoring.
However, SPME has been used in assays for selecting drugs in various biological matrices 16–18.