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Relationship Between Sensory Evaluation Performed by Italian and Spanish Official Panels and Volatile and Phenolic Profiles of Virgin Olive Oils

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Relationship Between Sensory Evaluation Performed by Italian and Spanish Official Panels and Volatile and Phenolic Profiles of Virgin Olive Oils Chem. Percept. (2008) 1:258–267 DOI 10.1007/s12078-008-9031-3 Relationship Between Sensory Evaluation Performed by Italian and Spanish Official Panels and Volatile and Phenolic Profiles of Virgin Olive Oils Lorenzo Cerretani & Maria Desamparados Salvador & Alessandra Bendini & Giuseppe Fregapane Received: 20 May 2008 /Accepted: 30 September 2008 /Published online: 24 October 2008 # 2008 Springer Science + Business Media, LLC Abstract Virgin olive oil (VOO) is typified by character- compounds (sum of aldehydes C6) and orthonasal percep- istic, pleasant sensory notes that differentiate it from other tion of olive fruity and retronasal odor of almond. edible oils. Sensory taste, together with nutritional aspects, Additional correlations with bitterness and pungency were is the main reason for the increase in consumption of VOO observed for tyrosol and oleuropein aglycon, respectively. in recent years. Sensory analysis is required by European Official Regulations for olive oil in order to classify the Keywords Virgin Olive Oil . Sensory Analysis . Panel Test . product in commercial categories. In this study, the Volatile Compounds . Phenolic Compounds relationship between sensory and chemical composition has been investigated. In particular, 16 VOO samples (15 Abbreviations from a single variety of olives), produced in Italy and Spain cGC Capillary gas chromatography (eight from each country), were analyzed. Sensory attrib- DAD Diode-array detector utes were valued by four panels (three officially recognized EI Electron ionization both by IOOC and National Ministry: two Italian and two HPLC High-performance liquid chromatography Spanish) employing a total of 59 tasters. Volatile and IOOC International Olive Oil Council phenolic compounds were related to olfactory and gustative LOX Lipoxygenase notes, respectively. Volatile compounds were then separat- MSD Mass-spectrometer detector ed, identified, and quantified, starting from oil samples, by QDA Quantitative descriptive analysis solid phase microextraction and capillary gas chromato- SPME Solid phase microextraction graphic analysis using a mass spectrometry detector VOO Virgin olive oil (SPME/cGC-MSD). Furthermore, the phenolic profile was examined by high-performance liquid chromatography with diode-array and mass spectrometry detectors (HPLC-DAD/ Introduction MSD). Correlations were found between the major volatile In terms of composition, virgin olive oils (VOO) differ L. Cerretani (*) : A. Bendini from the other edible oils in minor components (Angerosa Dipartimento di Scienze degli Alimenti, Università di Bologna, et al. 2004; Carrasco-Pancorbo et al. 2005a; Bendini et al. P.zza Goidanich 60, 2007a) that determine sensorial stimuli (Andrewes et al. 47023 Cesena (FC), Italy 2003; Gutierrez et al. 2003). For the merceological e-mail: [email protected] classification of virgin olive oils, the European Union M. D. Salvador (*) : G. Fregapane Commission has provided 26 chemical-physical parameters Departamento de Tecnología de Alimentos, and organoleptic evaluation (EEC Reg. 2568/91; EC Reg. Universidad de Castilla-La Mancha, 1989/03). Sensory analysis of VOO initiated from Collab- Avda Camilo José Cela 10, 13071 Ciudad Real, Spain orative International studies, which has been supported for e-mail: [email protected] many years by the International Olive Oil Council (IOOC) Chem. Percept. (2008) 1:258–267 259 that developed the Quantitative descriptive analysis sensory contribute to various VOO aromas have been investigated methodology for virgin olive oils, known as IOOC-Panel extensively by GC sniffing techniques (Morales et al. 1994). test. This study was finally published in June 1987, and the In a large number of investigations on VOO (Andrewes method was adopted for sensory analysis of VOO (IOOC et al. 2003; Gutierrez et al. 1989, 1992, 2003; Siliani et al. 1987). Sensory evaluation was introduced in the current, 2006; Beltrán et al. 2007), sensory and chemical parameters official regulations in 1991 (EEC Reg. 2568/91 Annex have been correlated, but in all cases, sensory analysis has XII). This analysis is carried out by a fully trained panel been carried out only by a single panel group or by panels composed of 8 to 12 assessors, and the regulation provides from the same producer country. a specific sensory sheet for assigning the merceological To assess correlations between sensory attributes and the category. Successively, in 2002, the European Union minor components of VOO, mainly phenolic and volatile Commission adopted the IOOC methodology, which profiles, four official panels from Italy and Spain and a set modifies and simplifies the score sheet, employing an of 16 VOO (15 monovarietal) Italian and Spanish samples unstructured 100-mm scale (EC Reg. 796/02). Finally, the were employed in order to verify the quality of the tasters’ 4th July 2008 other modifications suggested by IOOC were scores and determine the variability of the sensory introduced (EC Reg. 640/08) concerning the sensory characteristics of VOO samples. Together, Italy and Spain vocabulary and the conditions for the optional use, on contribute to more than 60% of worldwide olive oil labels, of certain terms and expressions relating to the production (IOOC 2007), and therefore, the capacity of organoleptic characteristics of virgin olive oil. Recently, the Official Taste Panels employed in this research work is the evolution of sensory analysis of VOO has led to the guaranteed. proposal of a method for oil and food pairing (Cerretani et al. 2007). Sensory attributes of VOO mainly depend on the content of Materials and Methods minor components like phenolic and volatile compounds. Each single component can contribute to different sensory Samples perceptions. It is well established that phenolic compounds are responsible for bitterness in VOO (Gutierrez et al. 1989, 1992, Table 1 shows the characteristics of the VOO samples 2003; Siliani et al. 2006; Beltrán et al. 2007). Andrewes et al. employed. With the exception of one sample, all oils were (2003) isolated individual compounds, and for each attribut- produced from a single variety of olives. Samples came ed sensory characteristic, these authors found that carbox- from different industrial olive mills covering the main ymethyl-ligstroside aglycon, also called oleocanthal producing areas in the two countries during two consecu- (Beauchamp et al. 2005), is the major phenolic molecule tive crop seasons: 2003–2004 and 2004–2005. responsible for the burning pungent sensation of VOO. Moreover, the phenolic content has been related to protection Reagents and Standards against important chronic and degenerative diseases (Menendez et al. 2007). The standards used for quantification of volatile and Approximately 180 compounds belonging to several phenolic compounds (1-nonanol and 3,4-dihydroxyphenyl- chemical classes such as aldehydes, ketones, ethers, hydro- acetic acid, respectively) were from Sigma-Aldrich (St. carbons, alcohols, and esters have been separated from the Louis, MO, USA). All solvents used were analytical or volatile fractions of different quality VOO (Angerosa 2002; HPLC grade (Merck, Darmstadt, Germany). Angerosa et al. 2004). Typical flavors and off-flavor compounds that affect the volatile fraction of a VOO Sensory Analysis originate by different mechanisms: enzymatically by linoleic and linolenic fatty acids through the so-called lipoxygenase Sensory analysis was performed by four Official Taste (LOX) pathway, by sugar fermentation or amino acid Panels. The Regional Panel of Agenzia Servizi Settore (leucine, isoleucine, and valine) conversion, or from enzy- Agroalimentare Marche—A.S.S.A.M. (Ancona, Italy) was matic activities of molds or auto-oxidative processes composed by a large number of members (20 plus the panel (Morales and Tsimidou 2000;Angerosa2002). Volatile leader) with an average age of 35 years; this panel was molecules can be perceived in very small amounts (micro- recognized by IOOC in the year 2000 and successively by grams per kilogram). These compounds do not contribute to the Italian Ministry in 2004. The Panel of Institute for the global aroma of VOO with the same importance; in fact, Mediterranean Agriculture and Forest Systems—CNR- their influence must be evaluated not only on the basis of ISAFoM (Perugia, Italy) is composed of 12 tasters with their concentration but also on their sensory threshold values. an average age of 35 years and are in the final training The independent odors of different volatile compounds that process. The Panel of Fundación Consejo Regulador de la 260 Chem. Percept. (2008) 1:258–267 Table 1 Virgin olive oil samples Volatile Compounds Analysis Sample Olive Country of Area of olive code cultivar production production VOO (4 g) was put into a 10-mL vial and heated to 40 °C. After 2 min of equilibrium time, volatile compounds from the A Cerasuola Italy Sicilia, Palermo headspace were adsorbed on a solid phase microextraction B Correggiolo Italy Emilia-Romagna, (SPME) under magnetic stirring. The fiber in PDMS 50/30 μm Rimini (Supelco, Bellefonte, PA, USA) was exposed to the vapor C Dritta Italy Abruzzo, Pescara D Frantoio Italy Emilia-Romagna, phase for 30 min at 40 °C. Desorption of volatile compounds Ravenna trapped in the SPME fiber was done directly in the gas E Leccino Italy Emilia-Romagna, chromatograph injector set at 220 °C in splitless mode using a Forlì-Cesena splitless inlet liner of 0.75 mm i.d. for thermal desorption F Frantoio, Italy Toscana where it was left
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