Water Addition During Oil Extraction Affects on Virgin Olive Oil Ethanol Content,Quality and Composition

Ethanol is the alcoholic precursor of fatty acid ethyl esters (FAEEs) in virgin olive oil (VOO). Because of its miscibility, water addition during oil extraction may affect oil ethanol content and then, the FAEEs synthesis during oil storage. In this work, the effect of water addition on VOO ethanol content and composition is studied. Water addition at two extraction systems (two and three phases) is compared and for vertical centrifuge, water addition at different temperatures is assayed. Ethanol content, quality parameters, and healthy components are determined in the oils. Results indicate three phase system gives oils with a 25% lower ethanol content than two phases. Ethanol reduction because of water addition is more important for three phases system (≈14%). For vertical centrifugation, ethanol is lowered as water dose and temperature increase. In general, water addition for any of the extraction steps analyzed reduces the oil ethanol concentration but other aspects such as fruity intensity and phenol content are also lowered. Practical applications: Virgin olive oil final ethanol content, and then its FAEEs concentration, does not only depend on the health and conservation status of olives, but also on the extraction system used and the amount of water added to the extraction process. The knowledge of the impact on ethanol content of water addition during oil extraction can be useful for olive oil legislators in order to keep the approved limits of FAEEs or to modify them. For oil producers, results can help to reduce the oil ethanol content and then FAEEs synthesis during virgin olive oil storage.     

Phenolic acid content and sensory properties of two Spanish monovarietal virgin olive oils

In recent years, phenolic acids have received considerable attention as they are essential to olive oil quality and nutritional properties. This study aims to validate a rapid and sensitive method based on ultra‐performance liquid chromatography/time‐of‐flight mass spectrometry (UPLC–TOF‐MS) for analyzing the phenolic acid content of olive oil and assessing its impact on virgin olive oil (VOO) sensory attributes. Once this method was validated, we used it to evaluate the phenolic acid composition of several Spanish monovarietal virgin olive oils in relation to nine different olive ripening stages. The results obtained confirm that the methodology developed in this study is valid for extracting and analyzing phenolic acids from VOO. The phenolic acid content of the virgin olive oils sampled was proven to be influenced by the type of cultivar and olive harvest date. Therefore, phenolic acids might be used as potential markers for olive oil cultivar or ripening stage. Finally, the data obtained indicate that the sensory properties of VOO may be differently affected by its phenolic acid content depending on the type of cultivar. Practical applications: The method validated in the present study – based on UPLC‐TOF‐MS – allows experts to assess the phenolic acid content of different VOO cultivars (varieties). This application will probably be very useful to the olive oil industry. The reason is that our study revealed that phenolic acids have an impact on the sensory quality of VOO, which is essential to consumer preferences and choice. In addition, there are phenolic acids that are only found in a particular variety of olive oil obtained from fruits at a specific ripening stage. Consequently, phenolic acids could be used as potential markers for olive oil variety and harvest time.     

Evaluation of virgin olive oil bitterness by total phenol content analysis

Bitterness is an important sensory attribute of virgin olive oil (VOO). It is usually assessed by tasting, which is a time‐consuming method and needs trained tasters. Bitterness is related to the phenolic compounds and can be estimated by the measurement of the specific absorbance at 225 nm (K₂₂₅). This paper proposes to evaluate oil bitterness intensity as estimated from the K₂₂₅ values measuring the phenol content. A significant relationship between phenol content and K₂₂₅ as well as a prediction model for bitterness intensity estimation from the phenol content was obtained. Classification of oil bitterness was based on the phenol content. Furthermore, when 12 VOO samples were classified by their bitterness intensities as estimated by the prediction model and by sensory analysis, more than 92% of the oil samples were correctly classified. Therefore, by measuring the phenol content, the bitterness intensity can be estimated and oils can be classified by their bitterness. This model may represent an easy method to evaluate the bitterness intensity without any sensory assessment.     

Phenolic composition of virgin olive oils from cross breeding segregating populations

The evaluation and characterization of segregating populations is a critical step in olive breeding programs. In this work, phenolic profiles of virgin olive oils (VOOs) from segregating populations obtained by cross breeding in Cordoba (Spain) have been evaluated. Genotypes obtained from open pollination of the cultivar Manzanilla de Sevilla, and from crosses between the cultivars Arbequina × Arbosana, Picual × Koroneiki and Sikitita × Arbosana were tested. The phenolic composition was determined after liquid–liquid extraction with 60:40 v/v methanol–water and subsequent chromatographic analysis with ultraviolet (UV) detection of both absorption and fluorescence in a sequential configuration. Results for all studied compounds showed high degree of variability between genotypes, with a higher range of variation than the observed for the genitors. Most of the observed variability was attributable to differences in genotypes within crosses rather than among crosses. Some issues related to breeding strategies are discussed. Practical applications: Phenolic compounds are considered to be of paramount importance for the assessment of virgin olive oil quality due to their contribution to the nutraceutical and sensory profile of this natural food. This study focuses on the evaluation of the content of phenolic compounds in olive oils originated from cross breeding in an olive breeding program (Cordoba, Spain). This step is crucial to determine the range of variation of phenolic compounds and the selection of interesting genotypes with higher composition in total phenols or in an individual phenol targeted at a breeding program.     

Detection of Soft‐Deodorized Olive Oil and Refined Vegetable Oils in Virgin Olive Oil Using Near Infrared Spectroscopy and Traditional Analytical Parameters

The European Parliament identifies virgin olive oil (VOO) as one of the foods which are often subject to fraudulent activities. Possibilities of adulteration are the application of illegal soft deodorization of extra virgin olive oil (EVOO) or the commercialization of blends of EVOO with soft‐deodorized EVOO or refined vegetable oils. Despite the search for possibilities to prove the illegal soft deodorization of EVOO or the addition of cheaper vegetable oils to EVOO, suitable methods are still missing. Therefore, the aim of the study is to develop a new analytical and statistical approach addressing detection of mild deodorization or addition of refined foreign oils. For this purpose, VOOs are treated in lab‐scale for 1 h up to 28 days at different temperatures (20, 50, 60, 80,100, 110, and 170 °C) in order to simulate and study the effect of heat treatment on known analytical parameters by near infrared spectroscopy (NIR). A logit regression model enabling the calculation of the probability for a heat treatment is developed. This new methodology allows detecting both soft deodorized olive oils and blends of EVOO with cheaper full refined vegetable oils. Adding only 10% of full refined oil could be detected in extra VOO. Practical Applications: NIR methods combined with chemometrics have become one of the most attractive analytical tools to control quality of food. It is a simple, precise, and rapid method. All relevant analytical parameters of oxidative and thermal fat degradation can be determined in a single run and be used to detect adulterated virgin olive oils (VOOs). The use of a simple equation developed from the logistic regression using peroxide value, K‐values, p‐anisidine value, pyropheophytine, 1,2‐diacylglycerols, total polar compounds and monomeric oxidized triacylglycerols, and other well‐known parameters allows to detect mild deodorized olive oils or also blends of VOO with soft‐deodorized ones or the addition of low amounts of foreign vegetable oils. This technique has potential to be used as a screening method for the detection of adulterated olive oils using both the traditional laboratory methods and the corresponding NIR‐methods.     

Stability of a phenol‐enriched olive oil during storage

The use of an emulsifier to stabilize the phenolic compounds added in the preparation of an enriched olive oil was evaluated. Two emulsifiers, lecithin and monoglyceride, were studied. The results showed lecithin to be the most convenient, due to the increase in the value of the oxidative stability of the phenol‐enriched oils in relation to the enrichments prepared with monoglycerides. After that, the shelf life of the prepared oils was evaluated during a period of 256 days of storage at 25°C in the dark. Oil quality parameters, total phenolic content, bitterness index and oxidative stability were studied during the storage period. Additionally, the phenolic composition and antioxidant capacity (by using the ORAC assay) were evaluated at the end of the storage. The phenolic enrichment of the oils allowed the shelf life of the oils to be extended compared with the control (virgin olive oil without phenol addition), delaying the appearance of peroxides and improving their oxidative stability. In addition, the higher content of phenolic compounds in the oils at all stages of storage is desirable in order to increase the intake of these beneficial compounds. Practical applications : The preparation of phenol‐enriched olive oils with a higher phenolic content than the commercial virgin olive oils is of special interest to increase the ingestion of these healthy compounds the daily intake of which is limited due to the high caloric value of olive oil. There are two key points in the development of this product: (i) the dispersion and stabilization of the phenol extract in the oil matrix and (ii) the stability of the phenols in the prepared oils to guarantee the phenol concentration during their shelf life. It is important to study the use of emulsifiers to determine if they allow an improvement in the dispersion of the phenolic extract, and their stabilization in the final product. In addition, the emulsifiers could mask the bitter taste of the enriched oils, which is desirable to increase consumer acceptance of the enriched oil.     

Antioxidative and synergistic effects of bene kernel and hull oils during oxidation of virgin olive oil

Total amounts of conjugated diene hydroperoxides and carbonyl compounds of a virgin olive oil (VOO) and its purified form as affected by 0.1–6% w/w bene kernel (BKO) and hull (BHO) oils were monitored during 16 h heating at 180°C. The VOO was more prone to the production of off‐flavour carbonyl compounds than to the formation of conjugated diene hydroperoxides. The VOOs oxidative stability decreased significantly due to the removal of the indigenous antioxidative compounds. Oxidative stability, especially regarding the secondary oxidation, significantly improved with increasing concentrations of the BKO than with those of the BHO.     

Dynamic viscosity of olive oil as a function of composition and temperature: A first approach

Knowledge of the viscosity of virgin olive oils (VOOs) is of great importance for the design of pilot plants, to determine the time required for the settling of particles at the end of the production chain and from a sensory view point. The dynamic viscosities of French VOOs from four different cultivars (‘Aglandau’, ‘Bouteillan’, ‘Salonenque’ and ‘Tanche’) were studied as a function of their fatty acid and TAG compositions and of the temperature [10–50°C]. These four VOOs had different TAG and fatty acid compositions representative of the range of compositional variations in the main French oils. Their viscosities were similar, although small but measurable differences that depended on their compositions were apparent. All the VOO samples exhibited the same dynamic viscosity pattern over temperature. For a given temperature, the viscosity difference was the greatest between Aglandau and Salonenque oils, Aglandau being the oil with the highest viscosity. The correlation between temperature and viscosity was highlighted by an Arrhenius model for this Newtonian fluid. The Arrhenius activation energy was correlated (R² = 0.993) with the percentage of triolein, the main TAG in olive oil.     

Stability and radical‐scavenging activity of heated olive oil and other vegetable oils

The effect of heating at 180 °C on the antioxidant activity of virgin olive oil (VOO), refined olive oil (ROO) and other vegetable oil samples (sunflower, soybean, cottonseed oils, and a commercial blend specially produced for frying) was determined by measuring the radical‐scavenging activity (RSA) toward 1,1‐diphenyl‐2‐picrylhydrazyl radical (DPPH^?). The RSA of the soluble (polar) and insoluble (non‐polar) in methanol/water fractions of olive oil samples was also measured. The stability of heated oils was assessed by determining their total polar compound (TPC) content. VOO was the most thermostable oil. Total polar phenol content and the RSA of VOO heated for 2.5 h decreased by up to 70 and 78%, respectively, of their initial values; an up to 84% reduction in RSA of VOO polar and non‐polar fractions also occurred. Similar changes were observed in the RSA of ROO and its non‐polar fraction after 2.5 h of heating. The other oils retained their RSA to a relatively high extent (up to 40%) after 10 h of heating, but in the meantime they reached the rejection point (25–27% TPC). The results demonstrate that VOO has a remarkable thermal stability, but when a healthful effect is expected from the presence of phenolic compounds, heating has to be restricted as much as possible.     

Composition and Physical Stability of the Colloidal Dispersion in Veiled Virgin Olive Oil

Veiled virgin olive oil (VOO) samples of nine different olive cultivars are chosen to have a wide range of physicochemical and biological properties of colloidal dispersions. The contents of proteins and phospholipids range from 40 to 190 mg kg⁻¹ and from 70 to 200 mg kg⁻¹, respectively. The effect of lab-scale centrifugation on cloudy appearance is studied measuring the decrease of turbidity grade values. The time to obtain unveiled oils (20 NTU) is modeled by a logistic equation, and a clear relationship between the initial water content and the above time is observed with a different trend between two groups of the VOO samples. Four VOO samples are selected to study the aggregation phenomena of microdroplets of water, pulp particles, and olive stone fragments via optical microscopy and dynamic light scattering during lab-scale gravity sedimentation. All VOOs are unstable with the cloudiness disappearing within the 230 days of investigation due to an overall diameter increase of cloudy components which is modeled by a power-law equation. The VOO samples, characterized by both small diameter values of dispersed components (150–250 nm) and high values of water content, show the fastest aggregation kinetics, but they have the longest time of cloudiness stability. Practical Applications: Water content and size distribution of VOO cloudy components can be key factors to control the colloidal stability. If removal of cloudy appearance is required, centrifugation can be applied to obtain a fast oil clarification which shows a power law relationship of water content with time. Instead, if physical stability of the colloidal dispersion is required, the aggregation phenomena should be slow down through VOO processing to obtain small diameters of the cloudy components. Tuning both the water content and dispersed phase diameter in the VOO can be the first step towards the control of phenomena related to the colloidal dispersion for every olive oil processing organization, above and beyond the simple removal of cloudy appearance by filtration.     

Oxidative stabilities of soybean oils that lack lipoxygenases

Lipoxygenase (LOX)-null soybean lines that lack LOX 2, or LOX 2 and 3, and contain normal (8.0–8.6%) or low (2.0–2.8%) linolenate (18∶3) amounts were evaluated for their oil qualities and storage stabilities. Soybean oils of six genotypes were extracted by both laboratory-scale and pilot-plant systems and were refined, bleached, and deodorized in the laboratory. Citric acid was added to oils during the cool-down stage of deodorization. Two replications, separated at the point of conditioning, were evaluated for each genotype. Under storage conditions of 55–60°C in the dark, soybean oils with low 18∶3 contents were significantly (P<-0.05) more stable as measured by peroxide values than were oils with normal 18∶3 contents, regardless of the LOX content of the beans. The volatile analysis showed few differences between oils with low and high 18∶3 contents or among oils from beans that lack different LOX enzymes. After 16 d of storage, the amount of 1-octen-3-ol was significantly greater in oils with low 18∶3 content, and soybean oils from beans with normal LOX content had a significantly (P<-0.05) lower amount of 1-octen-3-ol than did the oils that lacked LOX enzymes. Storage at 35°C under light showed no differences in volatile amounts or sensory evaluations after 14 d of storage. During storage, peroxide values tended to be lower in oils from beans with normal 18∶3 content and in oils from beans with normal LOX content. Generally, the abscence of LOX 2 or LOX 2 and 3, although having a small effect on lipid oxidation, was not as important to oil quality as was the 18∶3 content.     

Profile of enzyme in drupe of oueslati's cv. olives during ripening phases: A support method implementation in the production of extra virgin olive oil

Quality of virgin olive oil (VOO) depends on phenolic molecules content, which depends on the biochemical characteristics of olive fruits, namely endogenous enzymes. In order to ascertain the influence of olive fruit ripening degree on the phenol content, enzyme activities in olive fruits, and the quality of the corresponding oils were studied during Oueslati olive ripening. In fact, three enzymes were studied: peroxidase (POX) in olive seeds, polyphenoloxidase (PPO), and β-glucosidase (β-GL) in olive fruits mesocarp. Each enzyme showed specific trend: POX activity increased gradually until reaching a maximum (17.061 ± 0.101 U g⁻¹ FW) at ripening index (RI) 3.6 and then decreased slowly at advanced ripening stage. However, the maximum of PPO activity (240.421 ± 0.949 U g⁻¹ FW) was observed earlier at RI of 0.7. Concerning β-glucosidase activity, its maximal was 60.857 ± 1.105 U g⁻¹ FW at RI 2.8, then, it decreased sharply to reach 17.096 ± 0.865 U g⁻¹ FW at RI 3.9. A significant increase of total phenol content as well as the antioxidant activity were observed during Oueslati olive ripening. Moreover, phenolic profile indicated that appropriate harvesting date of Oueslati olives coincided with RI 3.9 given that highest content of most important individuals phenolic compounds responsible for the main VOO biological properties achieved on this date. Furthermore, phenols amount of Oueslati VOO was principally due to PPO enzyme activity as the increase in total phenols coincides with the decrease in PPO activity.     

Effect of Light Exposure on the Quality and Phenol Content of Commercial Extra Virgin Olive Oil during 12-Month Storage

Storage conditions influence the maximum time for which the composition and sensory characteristics of olive oils can be guaranteed. The purpose of this research was to study the quality and phenol content of extra virgin olive oil (EVOO) after storage for 1 year in different types of containers under darkness or light. Three Spanish cultivars with quantitatively different phenol contents were selected for the study. Storage under light conditions impaired the physicochemical and sensorial properties of the three cultivars, and reduced total phenolics, but there was an increase in hydroxytyrosol and tyrosol concentrations. It also markedly decreased their total phenolic content, especially when kept in polyethylene containers exposed to light, with reductions ranging from 4.28% for vanillic acid in Picual oils stored in dark glass containers under dark conditions to 97.82% for ferulic acid in Arbequina oils stored in polyethylene containers under light conditions. There was a reduced concentration of flavonoid and lignan concentrations after 1 year of storage, with the greatest decrease (98.01% of initial content) being observed for in the flavonoid apigenin. These results indicate that EVOO should be stored in dark glass containers under dark conditions for the optimal preservation of its quality and phenol content.     

Influence of the extraction process on dissolved oxygen in olive oil

The influence of the olive oil processing steps [paste malaxation (PM), decanter centrifugation (DC), and vertical centrifugation (VC)] on the dissolved oxygen (DO) concentration in virgin olive oil (VOO) right after production was investigated at industrial plant scale for two successive years. The influence of this parameter on quality decay during shelf life, assessed by peroxide value (PV) analysis, was also monitored. The VC step showed the higher oxygenation effect (50% increase in comparison to the control), and a good linear regression (r² = 0.83) was found between the initial DO concentration and the PV after 2 days. An 18‐months shelf life test, performed on VOO sampled before and after the VC, indicated the slowest decay kinetics in the oils with the lower initial DO concentration, i.e. the non‐centrifuged oils.     

Influence of olive crushing methods on the yields and oil characteristics

In the last years, metallic crushers substituted granite stone mill with some variations in the organoleptic oil characteristics. To control the influence of the crushing method on the yield and oil quality, the olive pastes were obtained using three different ways: (i) new metallic crusher at mobile knives; (ii) granite stone mill; (iii) double olive crushing by the metallic crusher and the granite stone mill. With the aim to ascertain the useful use of a new metallic crusher (at mobile knives), experimental tests were carried out in an industrial oil mill. This oil mill is equipped by a centrifugal decanter generating two oil flows: first and second extraction (recovery) oils. The results showed that the yields obtained by different methods were satisfactory. No statistically significant differences have been observed in terms of oil yield and quality when different crushing devices were used. All first extracted oils are extra virgin with similar organoleptic characteristics, especially for the fruity intensity and for the bitter and pungent taste, as confirmed by the composition of volatile substances and the content of phenolic oil compounds. The recovery oils (second extraction oils) showed, in contrast to first extraction oils, a more intense green colour and a higher content of total phenols. Practical applications: Processing of sound olives with the right ripening grade and good quality allows to easily obtain an extra virgin olive oil, with commercial qualitative parameters according to the European Union requirements. However, different olive crushing systems affect the concentrations of some compounds responsible of aroma and taste (phenolic compounds). The use of the more violent metallic crushers facilitates obtaining oils with total phenol content higher than when using a stone mill. Here we used a particular metallic crusher (at knives) that, however, is suitable to replace the granite stone mill when a less pungent and bitter oil is required.     

Use of nitrogen to improve stability of virgin olive oil during storage

Experiments were carried out to study the possibility of improving the stability of extra virgin olive oil by using nitrogen as a conditioner gas during storage. With this aim, virgin olive oil samples, obtained from Leccino and Coratina cultivars, were stored in the dark, in closed bottles conditioned with air or nitrogen at 12–20 and 40°C. Results indicated that the FFA percentage increased over 1% only when oils were stored at 40°C. The PV and the K ₂₃₂ value (light absorbance at 232 nm) of oils increased over the limit value allowed by European Union law when the bottles were only partly filled and air was the conditioner gas. The use of nitrogen as conditioner gas helped to avoid this risk during 24 mon of storage at 12–20°C. The total phenolic content of both cultivars oils decreased during storage because their oxidation protected the oils from autoxidation. The content of total volatile compounds in oils decreased continuously during storage at 12–20°C, whereas it increased over 10 (Coratina cv.) and 15 (Leccino cv.) mon and then diminished when the storage temperature was 40°C. The same behavior, i.e., increase then decrease, was ascertained for trans-2-hexenal. The hexanal content of oils increased continuously during storage because this compound is formed by the decomposition of the 13-hydroperoxide of linoleic acid.     

Quality control and storage studies of virgin olive oil: Exploiting UV spectrophotometry potential

The present work was undertaken in order to examine whether K₂₃₂ values and other UV absorbance characteristics could replace the determination of peroxide value (PV) in routine quality control and also in storage studies of virgin olive oil (VOO). For this reason, PV and extinction coefficients were determined for a large number of VOO samples (n = 40). The samples were then stored at 45 °C for several weeks. Changes in the lipid matrices were monitored by periodic measurements of the same quality indices. UV absorption spectra and the respective derivative ones were obtained before and during storage. Regression data showed that the PV is correlated with the K₂₃₂ value not only at time zero but also during storage. Evidence derived from the first derivative spectrum is strongly related to the oxidative status of the oil. The findings may be used (a) to simplify the decision tree suggested for “the verification of consistency of a VOO sample with commercial category declared” in the EEC Regulation N^o 1989 (2003), which takes into account acidity measurement, PV and absorbance values (K₂₇₀, ΔK, K₂₃₂), and (b) to collect qualitative and quantitative information about the oxidation process during storage.     

Effect of extraction systems on the quality of virgin olive oil

Research has been carried out to ascertai the effects of different processing systems on olive oil quality. Tests were performed in industrial oil mills that were equipped with both pressure and centrifugation systems. Results show that oils extracted from good-quality olives do not differ in free fatty acids, peroxide value, ultraviolet absorption and organoleptic properties. Polyphenols ando-diphenols contents and induction times are higher in oils obtained from good-quality olives by the pressure system because it does not require addition of water to the olive paste. The centrifugation system requires the addition of warm water to the olive paste and helps to obtain oils with a lower content of natural antioxidants. Oils obtained from poorquality or from ripe olives in continuous centrifugal plants are lower in free fatty acids than those obtained by the pressure system. Dr. Mario Solinas is deceased—May 23, 1993.     

Investigation of the Effects of Virgin Olive Oil Cleaning Systems on the Secoiridoid Aglycone Content Using High Performance Liquid Chromatography–Mass Spectrometry

Phenolic compounds are useful markers to control olive oil technological processes, including the virgin olive oil (VOO)/water separation after olive oil extraction. In this investigation, VOO extracted from olives of cv. Coratina using a mild oil/water separator called the hydrocyclone sedimentation system (Hydroil) was compared with VOO obtained using a conventional vertical centrifuge separator (Cenoil), which is mostly used in the modern olive oil industry. Secoiridoid aglycones were selected, among phenolic compounds, as markers and analyzed using reversed‐phase liquid chromatography coupled to linear quadrupole ion‐trap mass spectrometry with electrospray ionization in the negative mode. VOO samples obtained using the Hydroil system were found to contain significantly higher levels of secoiridoid aglycones, compared to the Cenoyl‐type samples. In particular, the total content of the aglycones of decarboxymethyl oleuropein, decarboxymethyl ligstroside, ligstroside, and oleuropein, expressed in terms of oleuropein, was estimated as 35.40 ± 0.80 mg kg^?1, compared to 8.06 ± 0.41 mg kg^?1 in the Cenoil samples (n = 3). Since no significant difference in residual water (P < 0.05) was found between the two types of VOO samples, the higher amount of secoiridoids obtained for Hydroil‐type ones was explained by the lower extent of oxidation occurring during the mild oil/water separation achieved using the Hydroil system.