Application of response surface methodology to optimize solid-phase microextraction procedure for chromatographic determination of aroma-active monoterpenes in berries

Food Chem. 2017 Apr 15:221:1041-1056. doi: 10.1016/j.foodchem.2016.11.057. Epub 2016 Nov 14.

Abstract

Most of scientific papers concern the qualitative or semi-quantitative analysis of aroma-active terpenes in liquid food matrices. Therefore, the procedure based on solid-phase microextraction and two-dimensional gas chromatography-time-of-flight mass spectrometry for determination of monoterpenes in fresh berries was developed. The optimal extraction conditions using divinylbenzene-carboxen-polydimethylsiloxane fiber were: temperature of 50°C, extraction time of 26min, equilibrium time of 29min. The developed procedure provides a high recovery (70.8-99.2%), good repeatability (CV<10.4%), high linearity (r>0.9915) and offers practical advantages over currently used methods: reliability of compounds identification, simplicity of extraction and at least one order of magnitude lower detection limits (0.10-0.011μg/L). The method was successfully applied to determine monoterpenes in 27 berry samples of different varieties and 4 berry products. Tukey's test revealed that monoterpenes content is a reliable indicator of fruit maturity and origin. It suggests that the method may be of interest to researchers and food industry.

Keywords: Berries; Blue honeysuckle; Box-Behnken design; Comprehensive two-dimensional gas chromatography; Monoterpenes; Response surface methodology; Solid-phase microextraction; Time-of-flight mass spectrometry.

MeSH terms

  • Dimethylpolysiloxanes / analysis
  • Fruit / chemistry*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Gas Chromatography-Mass Spectrometry / standards
  • Monoterpenes / analysis*
  • Polyvinyls / analysis
  • Reproducibility of Results
  • Solid Phase Microextraction / methods*
  • Solid Phase Microextraction / standards
  • Temperature
  • Terpenes / analysis

Substances

  • Dimethylpolysiloxanes
  • Monoterpenes
  • Polyvinyls
  • Terpenes
  • poly(dimethylsiloxane-divinylbenzene)