Coupling with solid-phase microextraction

Hawthorne SB, Grabanski CB, Hageman KJ, Miller DJ. Simple method for estimating polychlorinated biphenyl concentrations on soils and sediments using subcriti-cal water extraction coupled with solid-phase microextraction. J. Chromatogr. A 1998 814 151-160. 

Palmira Arenaz-Laborda, M., Extraction of polycyclic aromatic hydrocarbons from soil using hot water extraction coupled with solid phase microextraction , MSc Dissertation, Northumbria University, Newcastle, UK, 1998. 

Popp, P., C. Bauer, M. Moder, and A. Paschke. 2000. Determination of polycyclic aromatic hydrocarbons in waste water by off-line coupling of solid-phase microextraction with column liquid chromatography. J. Chromatogr. A 897 153-159. 

Aprea, E., Biasioli, F., Carlin, S., Versini, G., Mark, T. and Gasperi, F. (2007) Rapid white truffle headspace analysis by proton transfer reaction-mass spectrometry and comparison with solid-phase microextraction coupled with gas chromatography/mass spectrometry, Rapid Commun. Mass Sp., 21(16), 2564-2572. 

Hageman, K. J., Mazeas, L., Grabanski, C. B., Miller, D. J., and Hawthorne, S. B., Coupled subcritical water extraction with solid-phase microextraction for determining semivolatile organics in environmental solids. Anal. Chem., 68, 3892-3898, 1996. 

It has been coupled with enzyme immunoassay for efficient and fast polyaromatic hydrocarbon (PAH) screening in soil [21]. In a number of studies both static and dynamic superheated water extraction has been coupled to solid-phase microextraction [15, 25, 28, 30, 35, 38], sometimes with other analytical methods also coupled. It has been coupled with gas chromatography-mass spectrometry [31], capillary electrophoresis [31], liquid chromatography-mass spectrometry [32] and liquid chromatography-gas chromatography [41]. Sometimes other chemicals are added to the water used, such as acid [42] or phosphate buffer [43]. Different trapping methods for analytical extraction have been examined [44]. 

Liu, Z. and Pawliszyn, J., Coupling of solid-phase microextraction and capillary isoelectric focusing with laser-induced fluorescence whole column imaging detection for protein analysis. Analytical Chemistry, 77,165, 2005. 

Solid-phase microextraction (SPME) was used for headspace sampling. The FFA were extracted from the headspace with PA, Car/PDMS, and CW/DVB fibers. It was examined whether addition of salt (NaCl) and decreasing the pH by addition of sulphuric acid (H SO ) increased the sensitivity. FFA were analyzed using gas chromatography coupled to mass spectrometry in selected ion monitoring. 

SOLID-PHASE MICROEXTRACTION COUPLED WITH GAS OR LIQUID CHROMATOGRAPHY... 

Principles and Characteristics As mentioned already (Section 3.5.2) solid-phase microextraction involves the use of a micro-fibre which is exposed to the analyte(s) for a prespecified time. GC-MS is an ideal detector after SPME extraction/injection for both qualitative and quantitative analysis. For SPME-GC analysis, the fibre is forced into the chromatography capillary injector, where the entire extraction is desorbed. A high linear flow-rate of the carrier gas along the fibre is essential to ensure complete desorption of the analytes. Because no solvent is injected, and the analytes are rapidly desorbed on to the column, minimum detection limits are improved and resolution is maintained. Online coupling of conventional fibre-based SPME coupled with GC is now becoming routine. Automated SPME takes the sample directly from bottle to gas chromatograph. Split/splitless, on-column and PTV injection are compatible with SPME. SPME can also be used very effectively for sample introduction to fast GC systems, provided that a dedicated injector is used for this purpose [69,70],... 

In the 1990s, Pawliszyn [3] developed a rapid, simple, and solvent-free extraction technique termed solid-phase microextraction. In this technique, a fused-silica fiber is coated with a polymer that allows for fast mass transfer—both in the adsorption and desorption of analytes. SPME coupled with GC/MS has been used to detect explosive residues in seawater and sediments from Hawaii [33]. Various fibers coated with carbowax/divinylbenzene, polydimethylsiloxane/divinylbenzene, and polyacrylate are used. The SPME devices are simply immersed into the water samples. The sediment samples are first sonicated with acetonitrile, evaporated, and reconstituted in water, and then sampled by SPME. The device is then inserted into the injection port of the GC/MS system and the analytes thermally desorbed from the fiber. Various... 

Solid-phase microextraction has also been used for to determine volatile organic compounds in soil [26]. Target compounds were adsorbed directly from a head-space sample above a soil layer onto a fused-silica fibre. Vacuum distillation coupled with gas chromatography-mass spectrometry [27], head-... 

Excerpt 4C is taken from an article in Analytical Chemistry. Headspace solid-phase microextraction (HSSPME) is coupled with GC to quantify polychlorinated biphenyls (RGBs) in milk. The RGBs are volatilized out of the liquid phase (milk) into the gas phase (headspace) and concentrated on an SPME fiber. The concentrated RGBs on the fiber are then injected into the GG. 

The fabrication of imprinted monolithic solid-phase microextraction fibres has been developed for the selective extraction and preconcentration of diacetylmorphine and its structural analogues, triazines, bisphenol A, anaesthetics, and antibiotics followed by GC or HPLC analysis [156,163,179,196,197]. In addition, the on-line coupling of the imprinted monolith as a preconcentration column with a conventional analytical column has been proposed for the enrichment and cleanup of environmental and food samples [163]. However, at present, the capacity of the imprinted fibres and thus the degree of recovery of analytes are very variable and obviously need some improvement. For example, the recoveries of triazines after SPME with an imprinted monolith prepared by in situ polymerisation of MAA as... 

Aresta A, Palmisano F, Vatinno R, Zambonin CG (2006) Ochratoxin A Determination in Beer by Solid-Phase Microextraction Coupled to Liquid Chromatography with Florescence Detection A Fast and Sensitive Method for Assessment of Noncompliance to Legal Limits. J Agric Food Chem 54 1594... 

McCooeye, M. A., Mester, Z., Ells, B., Barnett, D. A., Purves, R. W., and Guevremont, R. (2002). Quantitation of amphetamine, methamphetamine, and their methylenedioxy derivatives in urine by solid-phase microextraction coupled with electrospray ionization-high-field asymmetric waveform ion mobility spectrometry-mass spectrometry. Anal. Chem. 74 3071-3075. 

Yang and Her [ 193] have described a rapid method for the determination of down to 200 ppt of semi-volatile compounds such as 1-chloronaphthalene, nitrobenzene and 2-chlorotoluene in soils by coupling solid-phase microextraction with attenuated total reflectance Fourier transform infrared spectroscopy. 

Wennrich et al. [167] investigated the capabilities of coupling accelerated solvent extraction with water as the extraction solvent and solid-phase microextraction to determine chlorophenols in polluted soils. Subcritical water extraction was performed using a commercially available accelerated solvent extractor. This system solves the problem of the analytes partitioning back to the soil matrix, which can occur in straightforward subcritical water extraction because in the Wennrich et al. method [167] the aqueous phase and the soil are separated under the extraction conditions. 

Moens, L., DeSmaele, T., Dams, R., VandenBroeck, R and Sandra, P. (1997) Sensitive, simultaneous determination of organomercury, -lead, and -tin compounds with headspace solid phase microextraction capillary gas chromatography combined with inductively coupled plasma mass spectrometry. Anal. Chem., 69, 1604—1611. 

Bagheri, H. and A. Salemi. 2004. Coupling of a concentric in-two-tube solid phase microextraction technique with HPLC-fluorescence detection for the ultratrace determination of polycyclic hydrocarbons in water samples. Chromatographia 59 501-505. 

Queiroz ME, Oliveira EB, Breton F et al (2007) Immunoaffinity in-tube solid phase microextraction coupled with liquid chromatography-mass spectrometry for analysis of fluoxetine in serum samples. J Chromatogr A 1174 72-77... 

Nishida M, Yashiki M, Namera A, Kimura K (2006) Single hair analysis of methamphetamine and amphetamine by solid phase microextraction coupled with in matrix derivatization. J ChromatogrB Analyt TechnolBiomedLifeSci 842(2) 106-110. doi S 1570-0232(06)00580-0 [pii] 10.1016/j. j chromb.2006.07.039... 

J. C. Wu, Z. Mester, J. Pawliszyn, Speciation of organoarsenic compounds by polypyrrole-coated capillary in tube solid phase microextraction coupled with liquid chromatography/electrospray ionisation mass spectrometry, Anal. Chim. Acta, 424 (2000), 211-222. 

Several analytical approaches are employed to quantify sulphur volatiles in wine among them, the headspace procedure, such as the Purge and Trap, and solid-phase microextraction methods, combined with GC coupled to different detectors, was shown to be quite effective (Mestres et al., 2000 Rauhut et al., 1998). Recent papers suggest that the HS-SPME technique, with an improved choice of fiber coating phases, would be one of the more promising approaches for the concurrent measurement of compounds with different boiling points (Mestres et al., 2002 Fang and Qian, 2005). 

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