Determination of biogenic amines in canned fish samples using head-space solid phase microextraction based on nanostructured polypyrrole fiber coupled to modified ionization region ion mobility spectrometry

J Chromatogr A. 2017 Jan 20:1481:37-43. doi: 10.1016/j.chroma.2016.12.046. Epub 2016 Dec 16.


The head-space solid phase microextraction (HS-SPME) was applied to extraction and determination of histamine (HIS), putrescine (PUT), cadaverine (CAD), tyramine (TYR) in canned fish samples by ion mobility spectrometry (IMS) without any derivatization process. HIS and CAD have the same mobilities in nitrogen as buffer gas and their corresponding peaks are severely overlapped in ion mobility spectrum. Peak separation was acquired in the presence of 18-crown-6 vapor as complexation reagent into carrier gas and modified ionization region of IMS (MIR-IMS) at optimum flow rate. The interaction between 18-crown-6 and the mentioned amines forms nanocluster product ions with different cross section areas and ion mobilities. The effects of main extraction parameters on the efficiency of HS-SPME-MIR-IMS were investigated and optimized. Relative standard deviations (RSD%) of the biogenic amines determination at 50μgL-1 concentration level were obtained in range 5.7%-6.3%. Limits of detection for analytes were in the range of 0.6-1ngg-1. HS-SPME-MIR-IMS results indicate that the proposed method can be successfully used in biogenic amines analysis in water and food samples. Method validation was conducted by comparing our results with those obtained through GC-MS method.

Keywords: Biogenic amines; Canned fish samples; Headspace solid phase microextraction; Ion mobility spectrometry; Nanoclusters.

MeSH terms

  • Biogenic Amines / analysis*
  • Buffers
  • Crown Ethers / chemistry
  • Fish Products / analysis*
  • Gas Chromatography-Mass Spectrometry
  • Hydrogen-Ion Concentration
  • Ions
  • Nanostructures / chemistry*
  • Nitrogen / chemistry
  • Polymers / chemistry*
  • Pyrroles / chemistry*
  • Reproducibility of Results
  • Salts / chemistry
  • Solid Phase Microextraction / methods*
  • Spectrum Analysis / methods*
  • Temperature
  • Time Factors


  • Biogenic Amines
  • Buffers
  • Crown Ethers
  • Ions
  • Polymers
  • Pyrroles
  • Salts
  • polypyrrole
  • 18-crown-6
  • Nitrogen