Protocol | Published:

Protocol for solid-phase microextraction method development

Nature Protocols volume 5, pages 122139 (2010) | Download Citation

Abstract

Solid-phase microextraction (SPME) is a sample preparation method developed to solve some of the analytical challenges of sample preparation as well as sample introduction and integration of different analytical steps into one system. Since its development, the utilization of SPME has addressed the need to facilitate rapid sample preparation and integrate sampling, extraction, concentration and sample introduction to an analytical instrument into one solvent-free step. This achievement resulted in fast adoption of the technique in many fields of analytical chemistry and successful hyphenation to continuously developing sophisticated separation and detection systems. However, the facilitation of high-quality analytical methods in combination with SPME requires optimization of the parameters that affect the extraction efficiency of this sample preparation method. Therefore, the objective of the current protocol is to provide a detailed sequence of SPME optimization steps that can be applied toward development of SPME methods for a wide range of analytical applications.

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Acknowledgements

The authors thank the Natural Sciences and Engineering Research Council of Canada (NSERC) for their financial support. The authors also like to acknowledge the contribution of Dr Zhouyao Zhang to the development of fiber-SPME technique.

Author information

Affiliations

  1. Department of Chemistry, University of Waterloo, Waterloo, Ontario, Canada.

    • Sanja Risticevic
    • , Heather Lord
    • , Tadeusz Górecki
    • , Catherine L Arthur
    •  & Janusz Pawliszyn

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Contributions

S.R. contributed to the development and validation of SPME methods, combined the data and wrote the protocol; H.L., T.G. and C.L.A. contributed to the SPME method optimization and validation, as well as development of theoretical principles of SPME; H.L. and T.G. provided helpful suggestions on the improvement of the protocol; and J.P. developed the SPME concept and the ideas on optimization of SPME methods and supervised the projects.

Corresponding author

Correspondence to Janusz Pawliszyn.

Supplementary information

Image files

  1. 1.

    Supplementary Figure 1

    The graphical illustration of commercially available fibre-SPME device for the performance of manual SPME procedures. Manual fibre holder (a). Fibre assembly with built-in fibre inside the needle coated with 1 or 2 cm long polymeric coating (b).

  2. 2.

    Supplementary Figure 2

    Illustration of SPME process. Legend: Kes - fibre coating/sample matrix distribution constant, Ve - fibre coating volume, Vs - sample volume, Co - initial concentration of analyte in the sample.

  3. 3.

    Supplementary Figure 3

    The graphical illustration of the DI-SPME procedure. The sample and a magnetic stir bar are placed in a vial, which is then sealed with a septum-type cap. The vial is placed on the magnetic stirrer (a). The SPME needle pierces the vial septum (b). The fibre coating is extended through the needle into the sample matrix (c). The fibre coating is withdrawn into the needle (d). The needle is withdrawn from the vial septum (e). Subsequent desorption of analytes into analytical instrument is performed.

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https://doi.org/10.1038/nprot.2009.179

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