Determination of phenols in soils by in situ acetylation headspace solid-phase microextraction

Abstract

A headspace solid‐phase microextraction (HSSPME) method for the determination of phenols in soils has been developed. The samples were suspended in water and phenols were derivatized in situ by adding potassium bicarbonate and acetic anhydride. Afterward, the sample was stirred and HSSPME was performed exposing the PDMS fiber with a 100 μ m thickness to the headspace over the sample. Finally, the fiber was inserted in the GC injector port and GC‐MSD analysis was carried out. Parameters affecting the extension of the adsorption process were studied (addition of water to the soil sample, sample size, salting out effect, volume of headspace). Also the extraction kinetics at 25 and 100°C were studied and compared. The proposed HSSPME method exhibits good performance in terms of precision, sensitivity, and linearity. Detection limits were in the sub‐ng/g. This method has been applied to a real contaminated soil and the concentrations of phenols found with the proposed method were in good agreement with the certified phenol values. ©2000 John Wiley & Sons, Inc. J Micro Sep 12: 25–32, 2000

Optimisation of the derivatisation reaction and subsequent headspace solid-phase microextraction method for the direct determination of chlorophenols in red wine

“…As regards the presence of chlorophenols in the environment, air samples [1,17], water (river and seawater [2,8,18,19], natural [20,21], waste [3,6,7,19,[22][23][24][25][26][27] and groundwater [6][7][8]) and soil samples [4,[28][29][30] have been processed. Because of their potential toxicity, numerous studies have focused on the analysis of chlorophenols in drinking water [5,9,[31][32][33] and the study of their bioaccumulation by the processing of urine samples of sawmill workers [34].…”

“…The final aim of this reaction consists in a transformation of chlorophenols into less polar compounds thus improving their chromatographic performance. As result of derivatisation reactions, chlorophenols may be transformed into the corresponding esters using pentafluorobenzoyl chloride [5] or acetic anhydride [1,[6][7][8]17,[20][21][22][23][25][26][27][28][29].…”

“…Supercritical fluid extraction (SFE) has also been used as an extraction method [28]. Recently, there is a tendency to replace the traditional method with techniques such as solid-phase extraction (SPE) [1,2,8,17,21,25,32,33,35], solid-phase microextraction (SPME) [3][4][5][6][7]9,18,19,[22][23][24]26,[29][30][31]34], stir bar sorptive extraction (SBSE) [36] and pervaporation [40] because they are simpler, reduce preparation time and some of them do not require the use of solvents. Although SPME methods have also been applied to analyse various components, off-flavours and contaminants in wine samples (i.e.…”

A simple and efficient method for the determination of pollutant phenols in soils with high levels of organic matter

“…However, microwave assisted extraction (MAE) [7][8][9][10][11][12][13][14] and pressurised liquid extraction (PLE, also known as accelerated solvent extraction, ASE) [15][16][17][18] are used as alternatives despite the use of high temperatures with these techniques having the potential to cause transformation or degradation of some of the analytes, which leads to a decrease in the recoveries and reproducibility [10]. On the other hand, other procedures such as sonication with organic solvents [8,[19][20][21], supercritical fluid extraction (SFE) [8,22,23], purge and trap (P&T) [24] and headspace solid-phase microextraction (HS-SPME) [25] or immersion SPME [26] have been described. Although it is possible to reduce the extraction time and the amount of extraction solvent with these procedures, expensive special equipment and/or the use of hazardous organic solvents is still required.…”

Solid‐phase microextraction liquid chromatography/tandem mass spectrometry for the analysis of chlorophenols in environmental samples

“…Solid‐phase microextraction (SPME) coupled to GC has been successfully used for the analysis of CPs from soils, directly from soil solutions,3,, 4 or by headspace‐SPME after in situ derivatisation 5. Moreover, SPME has also been combined with accelerated solvent extraction (ASE) 6.…”