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

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 26 min, equilibrium time of 29 min. The developed procedure provides a high recovery (70.8–99.2%), good repeatability (CV   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 (0.10–0.011 μg/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.