Headspace extraction analysis Solid-phase

Headspace extraction, see also Dilution analysis Solid-phase microextraction Hemoglobin... 

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. 

Microwave-assisted desorption coupled to in situ headspace solid-phase microextraction (HS-SPME) was first proposed as a possible alternative pretreatment of samples collected from workplace monitoring. Therefore, pretreatment that takes a short time and uses little or no organic solvents has led to the recent development of a new extraction technique. Solid-phase micro-extraction (SPME) coupled with GC analysis has been used successfully to analyze pollutants in environmental matrices. MHS has been developed to achieve one-step, in situ headspace sampling of semivolatile organic compounds in aqueous samples, vegetables, and soil [7, 55-58]. 

Distillation. Essential Oils. Extraction Solvent Extraction Principles Solid-Phase Extraction Solid-Phase Microextraction. Gas Chromatography Detectors Mass Spectrometry Chiral Separations. Headspace Analysis Static Purge and Trap. Mass Spectrometry Principles Selected Ion Monitoring. Quality Assurance Quality Control. Sensors Overview. 

This chapter includes the following techniques for preparing samples for analysis with HPLC, GC, and CE liquid-liquid extraction, solid-phase extraction (SPE), solid-phase microextraction, membrane-based sample preparation, headspace, and protein precipitation. 

A comprehensive overview of the techniques most commonly used for instrumental analysis of flavor compounds in food has been recently reported [3]. Several methods used for sample treatment are described, as well as the following techniques for extraction prior to GC analysis solvent extraction and distillation techniques, headspace methods, and solid-phase microextraction. The use of GC-olfactometry and of ion-trap MS in food aroma analysis is also described. 

S. Hamm, E. Lesellier, J. Bleton, A. Tchapla, Optimization of headspace solid phase micro extraction for gas chromatography/mass spectrometry analysis of widely different volatility and polarity terpenoids in olibanum, J. Chromatogr. A, 1018, 73 83 (2003). 

Bicchi, C., loti, C., Rubiolo, P. and Sandra, P. (2002) Headspace sorptive extraction (HSSE), stir bar sorptive extraction (SBSE) and solid phase microextraction (SPME) applied to the analysis of roasted Arabica coffee and coffee brew. J.Agric. Food Chem. 50, 449-459. 

In 2003, Smith reviewed newer sample preparation techniques, including pressurized liquid extraction, solid phase microextractions, membrane extraction, and headspace analysis. Most of these techniques aim to reduce the amount of sample and solvent required for efficient extraction. 

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)... 

Besides classical headspace analysis, simultaneous distillation-extraction and solvent extraction, new sampling and enrichment developments include solvent-assisted flavour evaporation (SAFE) [3] and sorptive techniques like SPME solid-phase microextraction (SPME) [4,5] and stir-bar sorptive extraction (SBSE) [6], which are treated in a dedicated chapter in this book. This contribution will deal with advanced developments of GC techniques for improvement of separation and identification (classical multidimensional GC, or... 

Solid-phase micro-extraction (SPME), a technique commercialised by Supelco, borrows from column extraction and headspace analysis. In this procedure, a small fibre fixed to the end of a syringe plunger can either exit from or be retracted into... 

Figure 11.14 Analysis of amphetamines by GC-NPD following HS-SPME extraction from human hair (a) Normal hair (b) normal hair after addition of amphetamine (1.5 ng) and methamphetamine (16.1 ng) (c) hair of an amphetamine abuser. Peak identification is as follows 1, a-phenethylamine (internal standard) 2, amphetamine 3, methamphetamine 4, N-propyl-/)-phenethyamine (internal standard). Reprinted from Journal of Chronatography, B 707,1. Koide et al., Determination of amphetamine and methamphetamine in human hair by headspace solid-phase microextraction and gas chromatography with nitrogen-phosphorus detection, pp. 99-104, copyright 1998, with permission from Elsevier Science.

Yang et al. [47,48,53,54] developed a HWG sensing system for liquid and soil analyses based on an extractive polymer membrane coated onto the inside of the HWG. The polymer coating performs a solid-phase microextraction of the analyte from the headspace of the sample and preconcentrates the analyte prior to IR analysis. 

Tolgyessy, R and J. Hrivnak. 2006. Analysis of volatiles in water using headspace solid-phase microcolumn extraction. J. Chromatogr. A 1127 295-297. 

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