Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction-Gas Chromatography-Mass Spectrometry

J Food Sci. 2016 Apr;81(4):C867-73. doi: 10.1111/1750-3841.13257. Epub 2016 Feb 29.


Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace-gas chromatography-mass spectrometry (DHS-GC-MS) and multiple headspace extraction-gas chromatography-mass spectrometry (MHSE), respectively. The monoterpenes were 1st extracted by means of supercritical fluid extraction (SFE) and analyzed by an optimized DHS-GC-MS. The optimization of the dynamic extraction step and the desorption/cryo-focusing step were tackled independently by experimental design assays. The best working conditions were set at 30 °C for the incubation temperature, 5 min of incubation time, and 40 mL of purge volume for the dynamic extraction step of these bioactive molecules. The conditions of the desorption/cryo-trapping step from the Tenax TA trap were set at follows: the temperature was increased from 30 to 300 °C at 150 °C/min, although the cryo-trapping was maintained at -70 °C. In order to estimate the efficiency of the SFE process, the analysis of monoterpenes in the 4 aromatic plants was directly carried out by means of MHSE because it did not require any sample preparation. Good linearity (r2) > 0.99) and reproducibility (relative standard deviation % <12) was obtained for solid and liquid quantification approaches, in the ranges of 0.5 to 200 ng and 10 to 500 ng/mL, respectively. The developed methods were applied to analyze the concentration of 7 monoterpenes in aromatic plants obtaining concentrations in the range of 2 to 6000 ng/g and 0.25 to 110 μg/mg, respectively.

Keywords: aromatic plants; dynamic headspace extraction; multiple headspace extraction; supercritical fluid extraction; volatile oils.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, Supercritical Fluid / methods
  • Elettaria / chemistry
  • Gas Chromatography-Mass Spectrometry / methods*
  • Lavandula / chemistry
  • Magnoliopsida / chemistry*
  • Monoterpenes / analysis*
  • Oils, Volatile / analysis*
  • Plant Extracts / chemistry*
  • Reproducibility of Results
  • Rosmarinus / chemistry
  • Salvia / chemistry
  • Temperature


  • Monoterpenes
  • Oils, Volatile
  • Plant Extracts