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  • Accepted Manuscript

    Solventless microextraction techniques for water analysis

    Nerea Lorenzo-Parodi, Wiebke Kaziur, Nenad Stojanović, Maik A. Jochmann, Torsten C. Schmidt

    PII: S0165-9936(18)30504-1

    DOI: https://doi.org/10.1016/j.trac.2018.11.013

    Reference: TRAC 15315

    To appear in: Trends in Analytical Chemistry

    Received Date: 28 September 2018

    Revised Date: 12 November 2018

    Accepted Date: 12 November 2018

    Please cite this article as: N. Lorenzo-Parodi, W. Kaziur, N. Stojanović, M.A. Jochmann, T.C. Schmidt, Solventless microextraction techniques for water analysis, Trends in Analytical Chemistry, https:// doi.org/10.1016/j.trac.2018.11.013.

    This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

    License:

    This work may be used under a Creative Commons Attribution-NonCommercial- NoDerivatives 4.0 International license

    This is the "Authors Accepted Manuscript" of an article published in: TrAC Trends in Analytical Chemistry, Volume 113, April 2019, Pages 321-331. The final version may be found at: https://doi.org/10.1016/j.trac.2018.11.013

    https://doi.org/10.1016/j.trac.2018.11.013 https://doi.org/10.1016/j.trac.2018.11.013 https://doi.org/10.1016/j.trac.2018.11.013 https://creativecommons.org/licenses/by-nc-nd/4.0/ https://creativecommons.org/licenses/by-nc-nd/4.0/ https://creativecommons.org/licenses/by-nc-nd/4.0/ https://doi.org/10.1016/j.trac.2018.11.013

  • ACCEPTED MANUSCRIPT

  • ACCEPTED MANUSCRIPT

    Solventless microextraction techniques for water analysis 1

    2

    Nerea Lorenzo-Parodi1, Wiebke Kaziur1, Nenad Stojanović1, Maik A. Jochmann1, Torsten C. 3

    Schmidt1, 2, 3. 4 1 Instrumental Analytical Chemistry, University of Duisburg-Essen, Universitätsstrasse 5, 45141 5

    Essen, Germany 6 2 Centre for Water and Environmental Research, University of Duisburg-Essen, 7

    Universitätsstrasse 5, 45141 Essen, Germany 8 3 IWW Water Centre, Moritzstrasse 26, 45476 Mülheim an der Ruhr, Germany 9

    10

    Keywords: SPME; SBSE; ITEX-DHS; SPDE; PAL SPME Arrow; GC-MS; Water analysis, 11

    Pollutants. 12

    13

    Abstract: 14

    Microextraction techniques have been proven to provide similar or better results in terms of 15

    sensitivity and reproducibility in comparison to liquid-liquid extraction (LLE) and solid-phase 16

    extraction (SPE). Furthermore, the high time efficiency and decreased workload leads to a higher 17

    sample throughput. In this review the state of the art of some of these techniques, namely solid-18

    phase microextraction (SPME), stir-bar sorptive extraction (SBSE), solid-phase dynamic 19

    extraction (SPDE), in-tube extraction-dynamic headspace (ITEX-DHS) and PAL SPME Arrow 20

    is shown. Furthermore, their benefits and drawbacks are discussed, together with their 21

    applicability to the analysis of water samples. To that end, the latest publications of 22

    microextraction techniques for a selection of regulated compound classes (chlorophenols (CPs), 23

    polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), pesticides, short-24

    chained chlorinated paraffins (SCCPs) and volatile organic compounds (VOCs)) are compared. 25

    Finally, a guideline for choosing the best microextraction technique for different analytical needs 26

    is described. 27

  • ACCEPTED MANUSCRIPT

    2

    Contents 28

    1 Introduction .................................................................................................................................. 329

    1.1 Solid-phase microextraction ............................................................................................... 330

    1.2 Stir-bar sorptive extraction ................................................................................................. 431

    1.3 Solid-phase dynamic extraction .......................................................................................... 632

    1.4 In-tube extraction dynamic headspace ................................................................................ 633

    1.5 PAL SPME Arrow .............................................................................................................. 734

    1.6 Selection criteria and general considerations ...................................................................... 735

    2 Choice and optimization of an appropriate microextraction technique ....................................... 836

    3 Applications ............................................................................................................................... 1337

    3.1 Chlorophenols ................................................................................................................... 2038

    3.2 Polycyclic aromatic hydrocarbons .................................................................................... 2039

    3.3 Polychlorinated biphenyls ................................................................................................. 2140

    3.4 Pesticides........................................................................................................................... 2241

    3.5 Short chain chlorinated paraffins ...................................................................................... 2242

    3.6 Volatile organic compounds ............................................................................................. 2343

    4 Conclusions ................................................................................................................................ 2444

    5 Acknowledgments...................................................................................................................... 2545

    6 References .................................................................................................................................. 2646

    47

    Abbreviations: AC, Activated carbon; CAR, Carboxen; CPs, Chlorophenols; DBPs, Disinfection 48

    by-products; DI, Direct immersion; DVB, Divinylbenzene; EPA, Environmental Protection 49

    Agency; GC, Gas chromatography; GC/ECNI-MS, Gas chromatography/electron capture 50

    negative ionization-mass spectrometry; GC-HRMS, Gas chromatography-high resolution mass 51

    spectrometry; GC-MS, Gas chromatography-mass spectrometry; GC-MS/MS, Gas 52

    chromatography-tandem mass spectrometry; GC-QqQ-MS/MS, Gas chromatography-triple 53

    quadrupole-mass spectrometry; GCxGC-HRTOF, Comprehensive two-dimensional gas 54

    chromatography-time of flight high resolution mass spectrometry; GCxGC-TOF, Comprehensive 55

    two-dimensional gas chromatography-time of flight mass spectrometry; HS, Headspace; ITEX-56

    DHS, In-tube extraction dynamic headspace; KAW, Air-water partitioning constant; KOW, 57

  • ACCEPTED MANUSCRIPT

    3

    Octanol-water partitioning constant; KPDMSW, Polydimethylsiloxane-water partitioning constant; 58

    KPAW, Polyacrylate-water partitioning constant; LD, Liquid desorption; LLE, Liquid-liquid 59

    extraction; LODs, Limits of detection; LOQs, Limits of quantification; MDLs, Method detection 60

    limits; NR, Not reported; PA, Polyacrylate; PAHs, Polycyclic aromatic hydrocarbons; PCBs, 61

    Polychlorinated biphenyls; PDMS, Polydimethylsiloxane; PP-LFERs, Polyparameter linear free 62

    energy relationship; SBSE, Stir-bar sorptive extraction; SCCPs, Short chain chlorinated 63

    paraffins; SI, Supplementary information; SIM, Single ion monitoring; SPDE, Solid-phase 64

    dynamic extraction; SPE, Solid-phase extraction; SPME, Solid-phase microextraction; TD, 65

    Thermal desorption; TOF, Time of flight; VOCs, Volatile organic compounds; WFD, Water 66

    Framework Directive; WHO, World Health Organization. 67

    68

    1 INTRODUCTION 69

    As green analytical chemistry becomes more important, the reduction of reagents and organic 70

    solvents, and the miniaturization and automation of analytical operations, among others, gain 71

    relevance [1]. LLE and SPE are commonly used techniques in analytical laboratories for the 72

    analysis of water samples [2], however, they need large solvent volumes and are very laborious 73

    [1]. As a result, they are slowly being replaced by novel microextraction techniques, which 74

    enrich and enable the direct injection of the analytes into the separation unit, and which require 75

    less solvents, time and labor [1, 3]. These microextraction techniques are generally used in 76

    combination to gas chromatography-mass spectrometry; which will therefore be the focus of this 77

    review. 78

    1.1 Solid-phase microextraction 79

    SPME was first used for the analysis of water samples in 1992 [4]. With this technique, 80

    sample preparation was improved upon by combining sampling, extraction, enrichment and 81

    sample introduction in a two-step process (Fig. 1a). The analytes partition between the sample 82

    and the extraction phase, absorb/adsorb into/o

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