Analytical and Bioanalytical Chemistry

, Volume 408, Issue 1, pp 191–201 | Cite as

Novel determination of polychlorinated naphthalenes in water by liquid chromatography–mass spectrometry with atmospheric pressure photoionization

  • Athanasios I. Moukas
  • Nikolaos S. Thomaidis
  • Antony C. Calokerinos
Research Paper


This study presents the development, optimization, and validation of a novel method for the determination of polychlorinated naphthalenes (PCNs) by liquid chromatography-atmospheric pressure photoionization (APPI), using toluene as dopant. The mass spectra of PCN 52, 54, 66, 67, 73, and 75 were recorded in negative ionization. The base ions corresponded to [M–Cl+O], where M is the analyte molecule. A strategy, which includes designs of experiments, for the development, the evaluation, and the optimization of the LC-APPI-MS/MS methods is also described. Finally, a highly sensitive method with low instrumental limits of detection (LoDs), ranging from 0.8 pg for PCN 75 to 16 pg for PCN 54 on column, was validated. A Thermo Hypersil Green PAH (100 mm × 2.1 mm, 3 μm) column was used with acetonitrile/water/methanol as mobile phase. The method was applied for the determination of the selected PCNs in surface and tap water samples. A simple liquid–liquid extraction method for the extraction of PCNs from water samples was used. Method LoQs ranged from 29 ng L−1, for PCN 73, to 63 ng L−1, for PCN 54, and the recoveries ranged from 97 to 99 %, for all congeners. This is the first LC-APPI-MS/MS method for the determination of PCNs in water samples.


Polychlorinated naphthalenes (PCNs) Atmospheric pressure photoionization (APPI) Dopant LC-APPI-MS/MS Pseudo-SRM Experimental design 


Compliance with ethical standards

Conflict of interest

The authors declare that they have no competing interests.

Supplementary material

216_2015_9092_MOESM1_ESM.pdf (923 kb)
ESM 1 (PDF 922 kb)


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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  • Athanasios I. Moukas
    • 1
  • Nikolaos S. Thomaidis
    • 1
  • Antony C. Calokerinos
    • 1
  1. 1.Laboratory of Analytical Chemistry, Department of Chemistry, School of SciencesNational and Kapodistrian University of AthensAthensGreece

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