Analytical and Bioanalytical Chemistry

, Volume 410, Issue 9, pp 2403–2411 | Cite as

Multi-layer solid-phase extraction and evaporation—enrichment methods for polar organic chemicals from aqueous matrices

  • Niklas Köke
  • Daniel Zahn
  • Thomas P. Knepper
  • Tobias Frömel
Research Paper


Analysis of polar organic chemicals in the aquatic environment is exacerbated by the lack of suitable and widely applicable enrichment methods. In this work, we assessed the suitability of a novel combination of well-known solid-phase extraction (SPE) materials in one cartridge as well as an evaporation method and for the enrichment of 26 polar model substances (predominantly log D < 0) covering a broad range of physico-chemical properties in three different aqueous matrices. The multi-layer solid-phase extraction (mlSPE) and evaporation method were investigated for the recovery and matrix effects of the model substances and analyzed with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). In total, 65% of the model substances were amenable (> 10% recovery) to the mlSPE method with a mean recovery of 76% while 73% of the model substances were enriched with the evaporation method achieving a mean recovery of 78%. Target and non-target screening comparison of both methods with a frequently used reversed-phase SPE method utilizing “hydrophilic and lipophilic balanced” (HLB) material was performed. Target analysis showed that the mlSPE and evaporation method have pronounced advantages over the HLB method since the HLB material retained only 30% of the model substances. Non-target screening of a ground water sample with the investigated enrichment methods showed that the median retention time of all detected features on a HILIC system decreased in the order mlSPE (3641 features, median tR 9.7 min), evaporation (1391, 9.3 min), HLB (4414, 7.2 min), indicating a higher potential of the described methods to enrich polar analytes from water compared with HLB-SPE.

Graphical abstract

Schematic of the method evaluation (recovery and matrix effects) and method comparison (target and non-target analysis) of the two investigated enrichment methods for very polar chemicals in aqueousmatrices.


Polar organic chemicals Solid-phase extraction Sample preparation Non-target screening HILIC 


Funding information

This work has been funded by the BMBF (02WU1347B) in the frame of the collaborative international consortium WATERJPI2013 - PROMOTE of the Water Challenges for a Changing World Joint Programming Initiative (Water JPI) Pilot Call.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2018_921_MOESM1_ESM.pdf (562 kb)
ESM 1 (PDF 502 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Niklas Köke
    • 1
  • Daniel Zahn
    • 1
  • Thomas P. Knepper
    • 1
  • Tobias Frömel
    • 1
  1. 1.Hochschule Fresenius, University of Applied SciencesIdsteinGermany

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