Solid-phase microextraction fiber selection

The following tables provide information on the selection and optimization of solid phase microextraction fibers.1 The reader is also advised to consult the tables for headspace analysis in this chapter. 

D. Djozan and T. Baheri, Preparation and evaluation of solid-phase microextraction fibers based on monolithic molecularly imprinted polymers for selective extraction of diacetyl-morphine and analogous compounds, / Chromatogr. A, 1166 (1-2) 16-23,2007. 

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. 

A new, fast, sensitive, and solventless extraction technique was developed in order to analyze beer carbonyl compounds. The method was based on solid-phase microextraction with on-fiber derivatization. A derivatization agent, 0-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine (PFBOA), was absorbed onto a divinyl benzene/poly(dimethylsiloxane) 65- xm fiber and exposed to the headspace of a vial with a beer sample. Carbonyl compounds selectively reacted with PFBOA, and the oximes formed were desorbed into a gas chromatograph injection port and quantified by mass spectrometry. This method provided very high reproducibility and linearity When it was used for the analysis of aged beers, nine aldehydes were detected 2-methylpropanal, 2-methylbutanal, 3-methylbutanal, pentanal, hexanal, furfural, methional, phenylacetaldehyde, and (E)-2-nonenal. (107 words)... 

Here is a student procedure to measure nicotine in urine. A 1.00-mL sample of biological fluid was placed in a 12-mL vial containing 0.7 g Na2CO , powder. After 5.00 pig of the internal standard 5-aminoquinoline were injected, the vial was capped with a Teflon-coated silicone rubber septum. The vial was heated to 80°C for 20 min and then a solid-phase microextraction needle was passed through the septum and left in the headspace for 5.00 min. The fiber was retracted and inserted into a gas chromatograph. Volatile substances were desorbed from the fiber at 250°C for 9.5 min in the injection port while the column was at 60°C. The column temperature was then raised to 260°C at 25°C/min and eluate was monitored by electron ionization mass spectrometry with selected ion monitoring at m/z 84 for nicotine and m/z 144 for internal standard. Calibration data from replicate... 

R. E. Shirey, SPME fibers and selection for specific applications, in S. A. Scheppers Wercinski, ed., Solid Phase Microextraction A Practical Guide, Marcel Dekker, New York, 1999, pp. 59-110. 

Solid Phase MicroExtraction (SPME) is a solvent-free sample preparation method based on the adsorption of analytes directly from an aqueous sample onto a coated fused-silica fiber. Headspace SPME was used in combination with gas chromatography-mass spectrometry/ selective ion monitoring (GC/MS-SIM) to analyze for TCA in wine. 

Solid-phase microextraction (SPME) is a technique that was first reported by Louch et al. in 1991 (35). This is a sample preparation technique that has been applied to trace analysis methods such as the analysis of flavor components, residual solvents, pesticides, leaching packaging components, or any other volatile organic compounds. It is limited to gas chromatography methods because the sample must be desorbed by thermal means. A fused silica fiber that was previously coated with a liquid polymer film is exposed to an aqueous sample. After adsorption of the analyte onto the coated fiber is allowed to come to equilibrium, the fiber is withdrawn from the sample and placed directly into the heated injection port of a gas chromatograph. The heat causes desorption of the analyte and other components from the fiber and the mixture is quantitatively or qualitatively analyzed by GC. This preparation technique allows for selective and solventless GC injections. Selectivity and time to equilibration can be altered by changing the characteristics of the film coat. 

Thermal desorption from a solid phase microextraction (SPME) fiber has shown considerable potential for selectively introducing semivolatile chemicals into an IMS. ° The SPME approach is a simple design patterned after the early platinum wire introduction thermal desorption system described. With SPME, semivolatile compounds are extracted by either absorption or adsorption onto a nonvolatile polymeric coating or solid sorbent phase that has been coated onto a small fiber. Normally, the adsorption liber is housed in the needle of a syringe to permit puncture of a sample bottle septum and to protect the fiber from contamination during transfer of the fiber from the sample to the IMS instrument. After the analytes are adsorbed onto the SPME fiber, the fiber is retracted into the needle and then injected in a normal syringe technique such that the fiber is extended into the heated region of the IMS and the analytes are desorbed from the fiber into the clean carrier gas of the IMS. 

Solid-phase microextraction is suitable for rapid extraction and preconcentration of compounds of different polarity and volatility from a variety of matrices. The selectivity of SPME depends on the phase coating of the silica fiber. The volume of the coating determines the capacity and the sensitivity of the method. The choice of the appropriate stationary phase should take into account both volatility and polarity of analytes. Using thick coatings, both extraction and... 

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