title: Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction-Gas Chromatography-Mass Spectrometry.
abstract: 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.
authors.affiliation: Dept. of Analytical Chemistry, Faculty of Science and Technology, Univ. of the Basque Country (UPV-EHU), P.O. Box 644, Bilbao, 48080, Basque Country, Spain.
authors.forename: Jone
authors.initials: J
authors.lastname: Omar
authors.affiliation: Dept. of Analytical Chemistry, Faculty of Science and Technology, Univ. of the Basque Country (UPV-EHU), P.O. Box 644, Bilbao, 48080, Basque Country, Spain.
authors.forename: Maitane
authors.initials: M
authors.lastname: Olivares
authors.affiliation: IDOKI SFC, Technologic Park of Biscay, Ibaizabal Bidea. Building 502,4816, Derio, Basque Country, Spain.
authors.forename: Ibone
authors.initials: I
authors.lastname: Alonso
authors.affiliation: Dept. of Analytical Chemistry, Faculty of Science and Technology, Univ. of the Basque Country (UPV-EHU), P.O. Box 644, Bilbao, 48080, Basque Country, Spain.
authors.forename: Asier
authors.initials: A
authors.lastname: Vallejo
authors.affiliation: Dept. of Analytical Chemistry, Faculty of Science and Technology, Univ. of the Basque Country (UPV-EHU), P.O. Box 644, Bilbao, 48080, Basque Country, Spain.
authors.forename: Oier
authors.initials: O
authors.lastname: Aizpurua-Olaizola
authors.affiliation: Dept. of Analytical Chemistry, Faculty of Science and Technology, Univ. of the Basque Country (UPV-EHU), P.O. Box 644, Bilbao, 48080, Basque Country, Spain.
authors.forename: Nestor
authors.initials: N
authors.lastname: Etxebarria
mesh_terms: D025924:Chromatography, Supercritical Fluid / Q000379:methods; D028523:Elettaria / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D027523:Lavandula / Q000737:chemistry; D019684:Magnoliopsida / Q000737:chemistry*; D039821:Monoterpenes / Q000032:analysis*; D009822:Oils, Volatile / Q000032:analysis*; D010936:Plant Extracts / Q000737:chemistry*; D015203:Reproducibility of Results; D027542:Rosmarinus / Q000737:chemistry; D027544:Salvia / Q000737:chemistry; D013696:Temperature
chemical_list: D039821:Monoterpenes; D009822:Oils, Volatile; D010936:Plant Extracts
keywords: aromatic plants; dynamic headspace extraction; multiple headspace extraction; supercritical fluid extraction; volatile oils