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      Development of a Single-Drop Microextraction with Derivatization Procedure for Analysis of Volatile Fatty Acids in Water Samples


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          A single-drop microextraction (SDME) was developed for the analysis of volatile fatty acids (VFAs) (C 2–C 7) in water by gas chromatography (GC) with flame ionization detection. The significant parameters affecting the SDME performance such as selection of microextraction solvent, extraction time, stirring rate, sample pH and temperature, and ionic strength were studied and optimized. To lower limits of detection, derivatization of VFAs by N-methyl- N-( tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) was performed. The method developed requires very short time of extraction and derivatization (13 min) and it is characterized by a good precision (max RSD = 11.4%), linearity and relatively low limits of detection (from 8.3 mg L −1 for acetic acid to 0.008 mg L −1 for heptanoic acid). The results of the SDME in combination with GC show promising potential for the analysis of VFAs in water samples.

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          Determination of fatty acids using solid phase microextraction

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            Headspace single-drop microextraction for the analysis of chlorobenzenes in water samples.

            Exposing a microlitre organic solvent drop to the headspace of an aqueous sample contaminated with ten chlorobenzene compounds proved to be an excellent preconcentration method for headspace analysis by gas chromatography-mass spectrometry (GC-MS). The proposed headspace single-drop microextraction (SDME) method was initially optimised and the optimum experimental conditions found were: 2.5 microl toluene microdrop exposed for 5 min to the headspace of a 10 ml aqueous sample containing 30% (w/v) NaCl placed in 15 ml vial and stirred at 1000 rpm. The calculated calibration curves gave a high level of linearity for all target analytes with correlation coefficients ranging between 0.9901 and 0.9971, except for hexachlorobenzene where the correlation coefficient was found to be 0.9886. The repeatability of the proposed method, expressed as relative standard deviation varied between 2.1 and 13.2% (n = 5). The limits of detection ranged between 0.003 and 0.031 microg/l using GC-MS with selective ion monitoring. Analysis of spiked tap and well water samples revealed that matrix had little effect on extraction. A comparative study was performed between the proposed method, headspace solid-phase microextraction (SPME), solid-phase extraction (SPE) and EPA method 8121. Overall, headspace SDME proved to be a rapid, simple and sensitive technique for the analysis of chlorobenzenes in water samples, representing an excellent alternative to traditional and other, recently introduced, methods.
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              Strategies for the microextraction of polar organic contaminants in water samples.

              In this paper the most recent developments in the microextraction of polar analytes from aqueous environmental samples are critically reviewed. The particularities of different microextraction approaches, mainly solid-phase microextraction (SPME), stir-bar-sorptive extraction (SBSE), and liquid-phase microextraction (LPME), and their suitability for use in combination with chromatographic or electrically driven separation techniques for determination of polar species are discussed. The compatibility of microextraction techniques, especially SPME, with different derivatisation strategies enabling GC determination of polar analytes and improving their extractability is revised. In addition to the use of derivatisation reactions, the possibility of enhancing the yield of solid-phase microextraction methods for polar analytes by using new coatings and/or larger amounts of sorbent is also considered. Finally, attention is also focussed on describing the versatility of LPME in its different possible formats and its ability to improve selectivity in the extraction of polar analytes with acid-base properties by using separation membranes and buffer solutions, instead of organic solvents, as the acceptor solution.

                Author and article information

                +48 52 3749040 , grazyna@utp.edu.pl
                Springer Berlin Heidelberg (Berlin/Heidelberg )
                25 May 2017
                25 May 2017
                : 80
                : 7
                : 1115-1120
                Department of Food Analytics and Environmental Protection, Faculty of Chemical Technology and Engineering, University of Science and Technology in Bydgoszcz, Seminaryjna 3 St., 85-326 Bydgoszcz, Poland
                © The Author(s) 2017

                Open AccessThis article is distributed under the terms of the Creative Commons Attribution 4.0 International License ( http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.

                : 10 January 2017
                : 17 April 2017
                : 19 April 2017
                Short Communication
                Custom metadata
                © Springer-Verlag GmbH Germany 2017

                Microscopy & Imaging
                derivatization,n-methyl-n-(tert-butyldimethylsilyl)trifluoroacetamide,single-drop microextraction,volatile fatty acids,water analysis


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