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

•Analytical procedure for determination of bioactive terpenes in berries was developed.•HS-SPME of monoterpenes from blue honeysuckle berries was optimized using RSM.•This method resulted in satisfactory recoveries and low LOD (0.10–0.011μg/L).•Eucalyptol was the most predominant terpene in all berry cultivars, juice and comfiture.•Tukey’s test proved important genotypic effects on terpene composition of berries. 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 (CV0.9915) 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.