Sample application solid-phase microextraction

Another relatively new SPE approach originally developed for the analysis of volatile organic compounds in environmental samples is solid-phase microextraction (SPME). This technique has gained acceptance for a wide variety of additional applications for the isolation of organic compounds from aqueous solu-... 

While open tubular (OT) columns are the most popular type, both open tubular and packed columns are treated throughout, and their advantages, disadvantages, and applications are contrasted. In addition, special chapters are devoted to each type of column. Chapter 2 introduces the basic instrumentation and Chapter 7 elaborates on detectors. Other chapters cover stationary phases (Chapter 4), qualitative and quantitative analysis (Chapter 8), programmed temperature (Chapter 9), and troubleshooting (Chapter 11). Chapter 10 briefly covers the important special topics of GC-MS, derivatization, chiral analysis, headspace sampling, and solid phase microextraction (SPME) for GC analysis. 

Several extraction methods for water samples are applicable, such as solvent extraction, SPE using a cartridge and disk and solid-phase microextraction (SPME). 

Applications The potential of a variety of direct solid sampling methods for in-polymer additive analysis by GC has been reviewed and critically evaluated, in particular, static and dynamic headspace, solid-phase microextraction and thermal desorption [33]. It has been reported that many more products were identified after SPME-GC-MS than after DHS-GC-MS [35], Off-line use of an amino SPE cartridge for sample cleanup and enrichment, followed by TLC, has allowed detection of 11 synthetic colours in beverage products at sub-ppm level [36], SFE-TLC was also used for the analysis of a vitamin oil mixture [16]. 

Figure l Photograph of diver collecting water samples during early studies on dissolved explosives in simulated ordnance in waters off San Clemente Island. Water is drawn by a pump over a solid phase microextraction fiber (not seen in photo) where explosives are retained and enriched. The SPME fiber was then presented to an IMS analyzer for the determination of explosives. Full application of these methods was made in Halifax Harbor. Source [72]... 

Oxidation, as is well known, leads not only to the formation of heavy compounds but also of volatile compounds that are responsible for off-flavors. Usually they are evaluated by capillary GC, through several sampling techniques are available (purge and trap, head space solid phase microextraction (SPME)). Rovellini et al. [26] recently proposed the application of HPLC for identifying... 

Due to the various health risks of different element species, there are a multitude of applications for natural water samples in this field (e.g., Cr and Sb speciation or Br and I determination).19 The investigation of heavy metal complexes with humic substances by isotope dilution SEC-ICP-MS has been described, for example, by McSheehy and Mester.20 Copper, zinc and molybdenum were found to form complexes with similar size fractions of humic substances in seepage water samples from soils. Sturgeon s group proposed the use of solid phase microextraction (SPME)... 

Lopez-Avila et al. [107] showed that microwave-assisted extraction of pesticides and polycyclic aromatic hydrocarbons from soil is a viable alternative to Soxhlet extraction and needs a smaller sample volume and extraction time [108,109]. These techniques have also been compared in the case of chlorophenols. Lopez-Avila et al. compared microwave-assisted extraction with electron capture gas chromatography to ELISA for the determination of polychlorinated biphenyls in soils. Both techniques are applicable to field screening and monitoring applications. Microwave-assisted extraction [111, 112] and solid-phase microextraction [113] have been applied to the extraction of pesticides from soil. It was observed by these and other workers [114] that the selectivity of microwave-assisted extraction is highly dependent on the soil composition. 

The following table provides a listing of the major types of sorbents used in sampling, concentrating, odor profiling, and air and water pollution research.16 These materials are useful in a wide variety of research and control applications. Many can be obtained commercially in different sizes, depending on the application involved. The purpose of this table is to aid in the choice of a sorbent for a given analysis. Information that is specific for solid phase microextraction (SPME) is provided elsewhere in this chapter. 

Chen Y. and J. Pawliszyn. 2007. Theory of solid phase microextraction and its application in passive sampling. In R. Greenwood, G.A. Mills, and B. Vrana (eds), Comprehensive Analytical Chemistry, pp. 3-32. Amsterdam Elsevier. 

MEPS has so far been applied mainly to the analysis of drugs in biological samples only one application for the extraction of PAHs in water has been published.26 One of the major advantages of the MEPS design is that the packed syringe can be used many times over, for example, more than 400 times for water samples. Moreover, the technique permits a fast handling time in the analysis of PAHs in water, the speed enhancement being 15 and 100 times compared to the literature procedures of solid-phase microextraction (SPME) and stir bar sorptive extraction (SBSE), respectively see Sections 4.2.3 and 4.2.4. 

Lanno, R., T.W. La Point, J.M. Conder, and J.B. Wells. 2005. Application of solid-phase microextraction fibers as biomimetic sampling devices in ecotoxicology, Chapter 28. In G.K. Ostrander (ed.), Techniques in Aquatic Toxicology, Vol. 2, pp. 511-522. Florida Taylor Francis-CRC Press. 

New applications of the SPE Solid-phase microextraction (SPME) for sampling analytes from 102,146-155... 

Lopez-Bianco, M.C., S. Blanco-Cid, B. Cancho-Grande, and J. Simal-Gandara. 2003. Application of single-drop microextraction and comparison with solid-phase microextraction and solid-phase extraction for the determination of a- and [1-endosulfan in water samples by gas chromatography-electron-capture detection. J. Chromatogr. A 984 245-252. 

Applications with Solid-Phase Microextraction (SPME) in Combination with SSID Solid-phase microextraction (SPME) and SSID with GC-ICP-MS were also applied for the determination of Me-Hg in fish tissue. The samples were digested... 

Augusto, E., Valentey, A.L.P. Applications of solid-phase microextraction to chemical analysis of live biological samples. Trends Anal. Chem. 21(428 38) (2002)... 

Preinjection sample preparation is not a chromatographic issue per se. Nevertheless, it is an important consideration in the successful application of a complete analytical process. Nerin et al. reviewed sample treatment techniques applicable to polymer extract analysis, including headspace methods, supercritical fluid extraction, and solid phase microextraction. 

Tsoukali H, Raikos N, Theodoridis G, Psaroulis D. Headspace solid phase microextraction for the gas chromatographic analysis of methyl-parathion in post-mortem human samples. Application in a suicide case by intravenous injection. Forensic Sci Int 2004 143 127-32. 

Natangelo, M.,Tavazzi, S., and Benfenati, E. (2002). Evaluation of solid phase microextraction-gas chromatography in the analysis of some pesticides with different mass spectrometric techniques application to environmental waters and food samples, Anal Lett., 35(2), 327-338. 

Solid phase microextraction (SPME) represents a modem alternative for sample preparation eliminating most of the disadvantages related to water sample preparation, SPME is a new sample enrichment technique that can easily transfer the analytes to the GC inlet. Since the invention of the technique in 1989 by J. Pawliszyn, its applications have dramatically increased. It has been used mainly for environmental water analysis (Pawliszyn, 1997). The basic equipment of SPME is simple. As shown in Fig. 4, a fiised-silica rod is connected to a stainless steel tube that can be withdrawn inside a syringe needle, after sampling, for protection and transfer to GC inlets. 

Abalos, M. and Bayona, J. M., Application of GC coupled to chemical ionisation mass spectrometry following headspace solid-phase microextraction for the determination of free volatile fatty acids in aqueous samples, J. Chromatogr. A, 891, 287-294, 2000. 

Ramesh, A. and Elumalai Ravi, P., Applications of solid-phase microextraction (SPME) in the determination of residues of certain herbicides at trace levels in environmental samples, J. Environ. Monit., 3, 505-508, 2001. 

Wardencki, W. and Namiesnik, J., Studies on the application of solid-phase microextraction for analysis of volatile organic sulfur compounds in gaseous and liquid samples, Chem. Anal. (Warsaw), 44, 485-493, 1999. 

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