Diego L. García-González

Research in Olive Oil: Challenges for the Near Future

Olive oil, a traditional food product with thousands of years of history, is continually evolving toward a more competitive global market. Being one of the most studied foods across different disciplines, olive oil still needs intensive research activity to face some vulnerabilities and challenges. This perspective describes some of them and shows a vision of research on olive oil for the near future, bringing together those aspects that are more relevant for better understanding and protection of this edible oil. To accomplish the most urgent challenges, some possible strategies are outlined, taking advantage of the latest analytical advances, considering six areas: (i) olive growing; (ii) processing, byproduct, and environmental issues; (iii) virgin olive oil sensory quality; (iv) purity, authentication, and traceability; (v) health and nutrition; (vi) consumers. The coming research, besides achieving those challenges, would increase the understanding of some aspects that are still the subject of debate and controversy among scientists focused on olive oil.

Characterization of French and Spanish dry-cured hams: influence of the volatiles from the muscles and the subcutaneous fat quantified by SPME-GC.

The influence of the volatile compounds on the characterization of Spanish and French dry-cured hams was studied. Thirty volatiles were quantified in each one of four locations (biceps femoris, semimembranosus and semitendinosus muscles and subcutaneous fat) of 29 dry-cured hams by solid-phase microextraction gas-chromatography (SPME-GC). The Brown-Forsythe univariate test allowed determination of the volatiles that individually could characterize (p<0.05) the samples by their geographical origin (France, Spain) and breed type (Iberian, white). Stepwise linear discriminant procedure, under very strict conditions (F-to-Enter for a F-distribution>0.95), then selected the most remarkable volatile compounds. Four compounds from the subcutaneous fat (methyl benzene and octanol) and the semitendinosus muscle (2-butanone and 2-octanone) allowed 100% correct classifications by geographic origin. On the other hand, only two compounds from the subcutaneous fat (octanol) and the biceps femoris muscle (3-methyl 1-butanol) correctly classified all the samples by the breed type. The ability of these variables to classify the samples was checked by the unsupervised procedure of principal components.

Relationship between sensory attributes and volatile compounds qualifying dry-cured hams.

This work studies the relationship between 45 volatile compounds and 17 sensory attributes (13 flavour perceptions) of dry-cured hams. Volatile compounds were quantified by SPME-GC while the sensory assessment was carried out by 13 panellists. GC-sniffing was used to determine the odour impact zones of the chromatogram. The odour thresholds of the volatile compounds and their sensory characterisation were determined by dilution analysis. Six sensory attributes (acorn odour and flavour, rancid odour, rancid taste, fat rancid and fat pungent flavours) were explained by regression equations (adjusted -R(2)⩾0.70) based on ten compounds: benzaldehyde, 2-heptanone, hexanal, hexanol, limonene, 3-methylbutanal, 3-methylbutanol, 2-nonanone, octanol, pentanol. Acorn flavour attribute was successfully emulated by mixing the volatile compounds selected by the equation. Its odour was evaluated by assessors that gave a sensory description that matches with the target. All the procedures performed for the elucidation of volatile-attribute relations showed a basic agreement in their results.

Evaluation of virgin olive oil thermal deterioration by fluorescence spectroscopy.

The evolution of the fluorescent compounds during the thermal deterioration of virgin olive oil is not yet well-known. Samples of heated virgin olive oils collected from a fryer every 2 h up to 94 h were analyzed to study their fluorescence spectra as well as the evolution of the concentrations of alpha-tocopherol and individual phenols by high-performance liquid chromatography (HPLC). The regions of the fluorescence spectra of the heated oils, diluted in hexane at 1%, were explained by the content of these compounds with regression coefficients higher than 0.90 (R2 adjusted). The fluorescence intensity recorded at 350 nm and the wavelength of the spectrum maximum in the range of 390-630 nm also allowed for the explanation of the increase of the percentage of polar compounds during the experiment. On the other hand, the spectra of the undiluted heated oils indicated that the maximum of the spectrum of any undiluted oil at 490 nm or beyond is related to a percentage of the polar compounds higher than 25%, which is the maximum percentage accepted for edible oils used in frying processes.

Quality Characterization of the New Virgin Olive Oil Var. Sikitita by Phenols and Volatile Compounds

New cultivars with greater adaptability to modern irrigated (super-) high-density orchards and producing good sensory quality oils are highly demanded by an olive oil industry in continuous change. This work analyzes olive oil sensory quality, in terms of phenols and volatiles that are responsible for virgin olive oil flavor, for three cultivars: Picual, which is used for >15% of world olive oil production; Arbequina, which is cultivated worldwide; and the new progeny Sikitita, which is derived from the other two. The availability of data at three different levels of ripeness allowed quantifying the genetic and olive maturity effects on the oil composition by means of the analysis of variance (ANOVA) and principal component analysis (PCA). Phenols and volatiles varied greatly both with genotype and, to a lesser extent, with olive maturity. With regard to the phenol profile, the crossbred cultivar Sikitita showed a higher degree of similarity with the Arbequina variety. The volatile composition of var. Sikitita, however, varies significantly from that of Arbequina, in the first stages of the olive ripeness, and becomes more similar to that of Picual as the level of ripeness increases.

Thermal deterioration of virgin olive oil monitored by ATR-FTIR analysis of trans content.

The monitoring of frying oils by an effective and rapid method is one of the demands of food companies and small food retailers. In this work, a method based on ATR-FTIR has been developed for monitoring the oil degradation in frying procedures. The IR bands changing during frying in sunflower, soybean, and virgin olive oils have been examined in their linear relationship with the content of total polar compounds, which is a preferred parameter for frying control. The bands assigned to conjugated and isolated trans double bonds that are commonly used for the determination of trans content provided the best relationships. Then, the area covering 978-960 cm(-1) was chosen to build a model for predicting polar material content for the particular case of virgin olive oil. A virgin olive oil was heated up to 94 h, and samples collected every 2 h constituted the training set. These samples were analyzed to obtain their FTIR spectra and to determine the composition of fatty acids and the content of total polar compounds. The excellent results predicting the polar material content (adjusted R(2) 0.997) was successfully validated with an external set of samples. The analysis of the fatty acid composition confirmed the relationship between the trans content and the content of total polar compounds.

Comparative study of virgin olive oil quality from single varieties cultivated in Chile and Spain

Olive tree varieties that were cultivated only in the Mediterranean basin a few decades ago are now planted in the Southern Hemisphere as well. The chemical composition of the oils produced in countries as far distant as Spain and Chile are affected by differences in latitude and climate. In this work, seven monovarietal virgin olive oils from Chile (Arbequina, Barnea, Frantoio, Koroneiki, Leccino, Manzanilla and Picual) have been characterized by the chemical compounds responsible for taste (phenols) and aroma (volatiles). The oils were produced in five regions of Chile, and the concentration values of some chemical compounds were related to the geographical location of the olive tree orchards. Virgin olive oils from the major cultivars, Arbequina and Picual, were characterized in comparison with the same monovarietal oils produced in Spain. The concentration values of fourteen volatile compounds showed significant differences (p < 0.05) between the oils produced in Spain and Chile. Concerning the phenol composition, main differences were found on the secoiridoids derivatives of oleuropein and ligstroside, apigenin and luteolin.

Validation of SPME-GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects

Volatile compounds are responsible for the aroma of virgin olive oil and also for its quality. The high number and different nature of volatile compounds drive to the need of a reliable analytical method that allows their proper quantification to explain the standard method of panel test. Although there are some analytical solutions available, they have not been validated and the regulatory bodies are reluctant to adopt them since they can be subjected to unknown errors. In this regards, the European Union has encouraged the validation of these analytical tools through the research program Horizon2020, which involves gaining knowledge from the analytical properties of the chemical methods for sensory assessment. This work is focused on the analytical validation of the methodology used to determine the actual concentration of volatiles in virgin olive oils when applying SPME-GCMS. The validation process includes the calibration curves for 29 volatile compounds responsible for the most common sensory perceptions in virgin olive oils, the determination of their working ranges with linear response, the detection and quantification limits, the sensitivity, the accuracy estimated as trueness and precision and the selectivity. Sixty-seven percent of the compounds presented a relative standard deviation in repeatability lower than 10%, and this percentage rises to 95% in lampante virgin olive oils. The accuracy was established in 97% of the studied volatile compounds. Finally, an empirical example of the ability of the method to discriminate virgin olive oils of different categories (extra virgin, virgin, ordinary and lampante) by the quantification of their volatiles is provided.

Geographical traceability of virgin olive oils from south-western Spain by their multi-elemental composition

The geographical traceability of virgin olive oil can be controlled by chemical species that are linked to the production area. Trace elements are among these species. The hypothesis is that the transfer of elements from the soil to the oil is subjected to minor variations and therefore this chemical information can be used for geographical traceability. In order to confirm this hypothesis, the trace elements of virgin olive oils from south-western Spain were analysed, and the same elements were determined in the corresponding olive-pomaces and soils. The differences in the concentration were studied according to cultivars and locations. Results show some coincidences in the selection of elements in soils (W, Fe, Na), olive-pomace (W, Fe, Na, Mg, Mn, Ca, Ba, Li) and olive oils (W, Fe, Mg, Mn, Ca, Ba, Li, Bi), which supports their utility in traceability. In the case of olive oils, 93% of the samples were correctly classified in their geographical origins (96% for Beas, 77% for Gibraleón, 91% for Niebla, and 100% for Sanlúcar de Guadiana).

Interlaboratory evaluation of dry-cured hams (from France and Spain) by assessors from two different nationalities.

Two panels of assessors from France and Spain assessed 41 dry-cured hams from diverse geographical origins, pig breedings and feedings. Univariate (Kolmogorov-Smirnov test and t-test) and multivariate (canonical correlation and principal component analysis) statistical procedures have been used to explain the agreement and disagreement between panels evaluating similar and dissimilar sensory attributes quantified with a 9-points structure scale. The results pointed out that there were basic agreements between panels, although some disagreements were detected in mould, acorn and crust attributes. The classification of Iberian and white dry-cured hams and the sensory attributes that characterise them are also displayed.