Comparison of the Novel Thin Film-Solid Phase Microextraction and Sorptive Extraction Methods for Picual and Hojiblanca Olive Oil Volatile Fraction Analysis in Headspace

Abstract

For first time, the new device named thin film solid phase microextraction (TF-SPME) has been used to determine the volatile profile of the Picual and Hojiblanca varieties of extra virgin olive oils. To this end, different traditional sampling methods such as headspace sorptive extraction (HSSE) with polydimethylsiloxane (PDMS) and polyethyleneglycol-modified silicone (EG/Silicone) Twisters® have been compared with the TF-SPME devices coated with different extraction polymeric phases. PARADISe software was used as a non-targeting method to process all data. The best results were obtained by HSSE-PDMS and 2TF-SPME. Moreover, the 2TF-SPME extraction method achieved the most adequate results of linearity for most compounds, according to F-values, while the intermediate precision results were similar for both 2TF-SPME and HSSE-PDMS sampling methods. Different sensitivity was observed between both sampling methods depending on the volatile compound, without being clearly influenced by the polarity of them. Although both sampling methods enabled the main active aroma of olive oil to be determined and for them to be differentiated according to olive variety, the 2TF-SPME method appears to be the most suitable for this goal.

Virgin Olive Oil Volatile Compounds: Composition, Sensory Characteristics, Analytical Approaches, Quality Control, and Authentication

“…128 In another study, SPME with two new thin film (TF-SPME) devices with a larger surface of extracting phase than typical HS-SPME gave better results than HSSE with PDMS Twister and polyethylenglicol-modified silicone (EG/S) Twister, even if currently the former has a higher price. 139 A comparison of these devices with the typically used HS-SPME fibers would be appropriate to confirm their suitability. Application of the vacuum-assisted HS-SPME (vac-HS-SPME) allowed revealing that the positive effect of reduced pressure on sampling is limited for the most volatile compounds, while for all the other VOCs, a nongeneralizable compound-dependent behavior related to the applied sampling time and temperature was observed.…”

“…In the same study, the authors compared three different SHS methods (namely, HS-SPME, headspace sorptive extraction (HSSE), and monoliting material sorptive extraction (MMSE), which differ in the sorptive/adsorptive materials’ characteristics and amount) and the DHS sampling approaches: a nongeneralizable compound-dependent behavior was highlighted, with a different best technique for each class of VOCs . In another study, SPME with two new thin film (TF-SPME) devices with a larger surface of extracting phase than typical HS-SPME gave better results than HSSE with PDMS Twister and polyethylenglicol-modified silicone (EG/S) Twister, even if currently the former has a higher price . A comparison of these devices with the typically used HS-SPME fibers would be appropriate to confirm their suitability.…”

Contribution of specific volatile markers to green and ripe fruity attributes in extra virgin olive oils studied with three analytical methods

“…Given the complexity of positive attributes found in EVOO associated to different volatile profiles rather than single volatile markers, the study of different isolation/extraction techniques and methods are needed to obtain the maximum information of the volatile profile. The perfection and validation of some methods based on headspace-solid-phase micro-extraction (HS-SPME) and gas chromatography (GC) with flame ionization (FID) or mass spectrometry (MS) detectors (Aparicio-Ruiz et al, 2018;Aparicio et al, 2012;Benelli et al, 2015;Casadei et al, 2021;Cecchi et al, 2019;Morales et al, 2005;Oliver-Pozo et al, 2015;Segura-Borrego et al, 2020) also provide the opportunity to determine volatile compounds with a minimized analytical error. The influence of the specificity of the SPME polymer in the volatile adsorption (Oliver-Pozo et al, 2015) could be avoided by using other extraction techniques such as the thermal extraction in micro-vials (ATEX) by Thermal Desorption Unit (TDU) coupled to GC-MS with a previous cryo-concentration with a Cooling Injector System (CIS) that applies liquid nitrogen (Francesca et al, 2015).…”