Use of Response Surface Methodology (RSM) for the Identification of the Best Extraction Conditions for Headspace Solid‐Phase Micro Extraction (HS‐SPME) of the Volatile Profile of cv. Arbequina Extra‐Virgin Olive Oil

Abstract

The effect of the experimental conditions on assessing the global volatile profile of extra virgin olive oils (EVOO) by headspace solid‐phase microextraction/gas chromatography‐mass spectrometry (HS‐SPME/GC–MS) is studied to obtain maximization of the total peak areas of the compounds. Response Surface Methodology (RSM) is applied to Arbequina EVOO, and the influence of oil quantity, extraction time, and extraction temperature on the total area and extraction of the major desirable compounds is analyzed. The experimental data are adequately fitted into second‐order polynomial models with non‐significant lack of fit (p > 0.05) and coefficients of determination (R2 and R2‐adjusted) higher than 0.88 and 0.78, respectively. A strong similarity is found between the predicted and experimental values. Furthermore, the surface plots show that the extraction of the volatile compounds is favored with increasing extraction temperature, time, and oil quantity. The extraction conditions to obtain the maximum response of “green” volatile compounds from Arbequina olive oil by HS‐SPME placed in 50 mL vials are 4.6 g of oil, 43 min, and 59 °C. Practical Applications: The findings of the present work show that specific conditions of HS‐SPME/GC–MS affect the extraction of volatile compounds from cv. Arbequina olive oil and establish the optimum extraction parameters to more efficiently determine the global profile of this fraction, taking into account the organoleptic characteristics of the cultivar. The results also contribute to the knowledge of the volatile profile of the monovarietal olive oil cv. Arbequina, which is one of most cultivated and consumed types of olive oil worldwide. The effects of oil quantity, extraction time, and temperature on the extraction of volatile compounds from the olive oil of the widespread Arbequina variety are investigated. The main volatiles found are C6 compounds, including aldehydes, alcohols, and the corresponding esters. The volatile profile is more affected by temperature and time than the oil quantity. The application of long times and high temperatures increases the total area and the extraction of Z‐3‐hexen‐1‐ol acetate and E‐2‐hexenal to which are associated sensory traits of cut‐green, tomato, and medium bitter taste.

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

“…The applied analytical conditions have to be selected based on the aim of the analysis. 135 Increasing temperature may allow extracting a higher number of VOCs but can create possible artifacts. 68,134 The main inconveniences of HS-SPME are the competition and interaction phenomena during adsorption of VOCs onto the fiber; thus, to avoid unbiased quantitation, suitable devices have to be adopted (Section 6.3).…”

“…The adsorption is based on the partition equilibrium among the three-phase system constituted by oil sample, headspace over the sample, and fiber; the distribution coefficients of each VOC between the sample matrix, gas phase, and fiber coating influence the SPME uptake. The applied analytical conditions have to be selected based on the aim of the analysis . Increasing temperature may allow extracting a higher number of VOCs but can create possible artifacts. , The main inconveniences of HS-SPME are the competition and interaction phenomena during adsorption of VOCs onto the fiber; thus, to avoid unbiased quantitation, suitable devices have to be adopted (Section ).…”

Quantification of Volatile Compounds in Wines by HS-SPME-GC/MS: Critical Issues and Use of Multivariate Statistics in Method Optimization

“…Once the variability ranges have been established for the factors, optimization based on multivariate statistics can be achieved through two fundamental approaches related to the DoE: two-level factorial designs and response surface methodologies (RSM) [28][29][30] with the latter including, among others, central composite (CCD) [25,31], Doehlert matrix (DM) [32,33], three-level factorial (3K) and Box Behnken (BBD) designs [27].…”

Aroma‐Relevant Volatile Compounds as Markers for the Sensory Quality of Argan Oil

“…Profiling and characterization of volatile compounds from edible oils in combination with statistical means seems to be a promising approach to use volatile compounds for the differentiation of oil qualities and to support the sensory evaluation. Especially for virgin extra olive oil, several studies have been published showing that sensory defects are correlated with the presence of certain volatile compounds . Investigations on the profile of volatile compounds have been carried out for other edible oils as well to find key compounds to support sensory evaluation …”