First Application of Newly Developed FT-NIR Spectroscopic Methodology to Predict Authenticity of Extra Virgin Olive Oil Retail Products in the USA

Economically motivated adulteration (EMA) of extra virgin olive oils (EVOO) has been a worldwide problem and a concern for government regulators for a long time. The US Food and Drug Administration (FDA) is mandated to protect the US public against intentional adulteration of foods and has jurisdiction over deceptive label declarations. To detect EMA of olive oil and address food safety vulnerabilities, we used a previously developed rapid screening methodology to authenticate EVOO. For the first time, a recently developed FT-NIR spectroscopic methodology in conjunction with partial least squares analysis was applied to commercial products labeled EVOO purchased in College Park, MD, USA to rapidly predict whether they are authentic, potentially mixed with refined olive oil (RO) or other vegetable oil(s), or are of lower quality. Of the 88 commercial products labeled EVOO that were assessed according to published specified ranges, 33 (37.5%) satisfied the three published FT-NIR requirements identified for authentic EVOO products which included the purity test. This test was based on limits established for the contents of three potential adulterants, oils high in linoleic acid (OH-LNA), oils high in oleic acid (OH-OLA), palm olein (PO), and/or RO. The remaining 55 samples (62.5%) did not meet one or more of the criteria established for authentic EVOO. The breakdown of the 55 products was EVOO potentially mixed with OH-LNA (25.5%), OH-OLA (10.9%), PO (5.4%), RO (25.5%), or a combination of any of these four (32.7%). If assessments had been based strictly on whether the fatty acid composition was within the established ranges set by the International Olive Council (IOC), less than 10% would have been identified as non-EVOO. These findings are significant not only because they were consistent with previously published data based on the results of two sensory panels that were accredited by IOC but more importantly each measurement/analysis was accomplished in less than 5 min.     

Evaluation of MALDI-TOF/MS Technology in Olive Oil Adulteration

Adulteration of extra virgin olive oil (EVOO) by addition of other vegetable oils or lower-grade olive oils is a common problem of the oil market worldwide. Therefore, we developed a fast protocol for detection of EVOO adulteration by mass spectrometry fingerprinting of triacylglycerol (TAG) profiles based on MALDI-TOF/MS. For that purpose, EVOO TAG profiles were compared with those of edible sunflower oil and olive oil composed of refined olive oil and virgin olive oils. Adulteration of EVOO was simulated by addition of sunflower and mixture of refined olive oil and virgin olive oils at 1, 10 and 20% w/w. Results of mass spectrometry TAG profiling were compared with routinely assessed K values for identification of adulteration. MALDI-TOF/MS technology coupled with statistical analysis was proven as useful for detection of adulteration in EVOO at a rate down to 1%. In contrast, standard spectrophotometric methods failed to identify minor adulterations. In addition, the ability of MALDI-TOF/MS in detection of adulteration was tested on EVOO samples from different geographical regions. Results demonstrated that MALDI-TOF/MS technology coupled with statistical analysis is able to distinguish adulterated oils from other EVOO.     

Detection of pressed hazelnut oil in admixtures with virgin olive oil by analysis of polar components

Analysis of the polar fraction from virgin olive oil and pressed hazelnut oil by high-performance liquid chromatography showed marked differences in the chromatograms of the polar components in the two oils. Six commercial samples of pressed hazelnut oil and 12 samples of virgin olive oil (or blended olive oil including virgin olive oil) were analyzed. The phenolic content of the pressed hazelnut oil samples was 161±6 mg·kg⁻¹. Inspection of the chromatograms showed that the pressed hazelnut oil extracts contained a component that eluted in a region of the chromatogram that was clear in the olive oil samples, and consequently this component could be used to detect adulteration of virgin olive oil by pressed hazelnut oil. The component had a relative retention time of 0.9 relative to 4-hydroxybenzoic acid added to the oil as an internal standard. The ultraviolet spectrum of the component showed a maximum at 293.8 nm, but the component could not be identified. Analysis of blends of oils showed that adulteration of virgin olive oil by commercial pressed hazelnut oil could be detected at a level of about 2.5%.     

Detection of Olive Oil Adulteration Using FT-IR Spectroscopy and PLS with Variable Importance of Projection (VIP) Scores

Determination of adulteration and authenticity of extra virgin olive oil (EVOO) was investigated by means of infrared spectroscopy and chemometric methods. The study was focused on the detection and quantification of extra virgin olive oil adulteration by soybean (SB) and sunflower (SF) oils using FT-IR spectroscopy based on the use of PLS modeling and variable importance of projection (VIP) scores. A PLS model, using orthogonal signal correction and mean centering data pretreatments, and VIP scores variable preselection, was able to predict the concentration of sunflower and soybean oil adulterants in the 1–24 % weight ratio range with relative prediction errors lower than 3 % (w/w), for external validation samples. Moreover, the PLS-DA (discriminant analysis) model using the same preselected wavelengths was able to explain 99.9 % of variance and to predict with 100 % accuracy both classes of adulteration (EVOO–SB and EVOO–SF) in the external validation.     

Sterol fractions in hazelnut and virgin olive oils and 4,4′-dimethylsterols as possible markers for detection of adulteration of virgin olive oil

Reports on the methylsterol fractions of hazelnut oils are scarce. The objectives of this study were to characterize methylsterols in hazelnut and virgin olive oils and to study the possibility of detection of adulteration of virgin olive oils. In hazelnut oils, 4-desmethylsterols were present in higher proportions (86 to 91%) than in virgin olive oils where this fraction was ca. 50% of the total sterol. In the 4-monomethylsterol fraction, citrostadienol was the major component in both kinds of oils followed by cycloeucalenol and obtusifoliol in virgin olive oils, and obtusifoliol in hazelnut oils. 24-Methylenecycloartanol was predominant in both kinds of oils in the 4,4′-dimethylsterols. For the first time, δ-amyrin was tentatively identified by comparing published mass spectral data in the analyzed samples of both kinds of oils. An unknown compound X (containing a lupane skeleton) and lupeol were detected only in the 4,4′-dimethylsterols fraction of hazelnut oils at a level of 2–8 and 6–10%, respectively. GC-MS analysis showed that adulteration of virgin olive oil by hazelnut oil could be detected at a level less than 4% by using these two compounds as possible potential markers.     

Developing FT-NIR and PLS1 Methodology for Predicting Adulteration in Representative Varieties/Blends of Extra Virgin Olive Oils

It was previously demonstrated that Fourier transform near infrared (FT‐NIR) spectroscopy and partial least squares (PLS1) were successfully used to assess whether an olive oil was extra virgin, and if adulterated, with which type of vegetable oil and by how much using previously developed PLS1 calibration models. This last prediction required an initial set of four PLS1 calibration models that were based on gravimetrically prepared mixtures of a specific variety of extra virgin olive oil (EVOO) spiked with adulterants. The current study was undertaken after obtaining a range of EVOO varieties grown in different countries. It was found that all the different types of EVOO varieties investigated belonged to four distinct groups, and each required the development of additional sets of specific PLS1 calibration models to ensure that they can be used to predict low concentrations of vegetable oils high in linoleic, oleic, or palmitic acid, and/or refined olive oil. These four distinct sets of PLS1 calibration models were required to cover the range of EVOO varieties with a linoleic acid content from 1.3 to 15.5 % of total fatty acids. An FT‐NIR library was established with 66 EVOO products obtained from California and Europe. The quality and/or purity of EVOO were assessed by determining the FT‐NIR Index, a measure of the volatile content of EVOO. The use of these PLS1 calibration models made it possible to predict the authenticity of EVOO and the identity and quantity of potential adulterant oils in minutes.     

A Simple and Effective Mass Spectrometric Approach to Identify the Adulteration of the Mediterranean Diet Component Extra-Virgin Olive Oil with Corn Oil

Extra virgin olive oil (EVOO) with its nutraceutical characteristics substantially contributes as a major nutrient to the health benefit of the Mediterranean diet. Unfortunately, the adulteration of EVOO with less expensive oils (e.g., peanut and corn oils), has become one of the biggest source of agricultural fraud in the European Union, with important health implications for consumers, mainly due to the introduction of seed oil-derived allergens causing, especially in children, severe food allergy phenomena. In this regard, revealing adulterations of EVOO is of fundamental importance for health care and prevention reasons, especially in children. To this aim, effective analytical methods to assess EVOO purity are necessary. Here, we propose a simple, rapid, robust and very sensitive method for non-specialized mass spectrometric laboratory, based on the matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS) coupled to unsupervised hierarchical clustering (UHC), principal component (PCA) and Pearson’s correlation analyses, to reveal corn oil (CO) adulterations in EVOO at very low levels (down to 0.5%).     

Characterization of Extra Virgin Olive Oil from Southern Brazil

Six olive oils extracted from the cultivars Arbequina, Arbosana, Coratina, Frantoio, Koroneiki, and Picual from 2017 and 2018 harvests, cultivated in Pinheiro Machado, Rio Grande do Sul, Brazil, are evaluated for standard oil composition parameters and bioactive constituents (pigments, tocopherols, and phenolic compounds). Multivariate principal component analysis (PCA) and univariate ANOVA and Fisher's LSD test are used to verify the effect of cultivar and harvest year on oil composition. Olive oil composition met extra virgin olive oil (EVOO) standard parameters and is influenced by both cultivar and harvest year. EVOO produced in 2018 has greater chlorophyll, caffeic acid, ligstroside aglycone, hydroxyoleuropein aglycone, syringic acid, and hydroxytyrosol acetate contents than the EVOOs from 2017. Linoleic acid, ferulic acid, ligstroside aglycone, and hydroxytyrosol acetate are the variables whose contents most contributed to the differentiation of oils by cultivar in both harvest years. Chemical characterization analyses allow for the differentiation of oil composition based on harvest year and cultivar. Metabolic quality data obtained here support the establishment of a local EVOO profile and the compounds that most contributed to treatment differentiation may serve as markers that can be utilized in determining origin, cultivar, and harvest year. Practical Applications: Olive production in Brazil is recent and is based on European cultivars which have not been bred for the local environmental conditions. Therefore, the measurement of olive oil metabolic quality will determine cultivar adaptability to local edaphoclimatic conditions as well as assist in the establishment of a standard of identity for the product and promote the development of its market. Olive oil produced in Southern Brazil shows high quality, and is especially rich in phenolic compounds. Although harvest year influences oil composition, oil from both harvests meet EVOO standards and cultivar specific metabolic markers are observed. This study provides the foundation for olive producers in Southern Brazil to seek authentication of the geographical origin of olive oil.     

Detection of olive oil adulteration with canola oil from triacylglycerol analysis by reversed-phase high-performance liquid chromatography

The objective of this study was to explore the use of reversed-phase high-performance liquid chromatography (RP-HPLC) as a means to detect adulteration of olive oil with less expensive canola oil. Previously this method has been shown to be useful in the detection of some other added seed oils; however, the detection of adulteration with canola oil might be more difficult due to similarities in fatty acid composition between canola oil and olive oil. Various mixtures of canola oil with olive oils were prepared, and RP-HPLC profiles were obtained. Adulteration of olive oil samples with less than 7.5% (w/w) canola oil could not be detected.     

Triglyceride composition of olive oil,cottonseed oil and their mixtures by low temperature crystallization and gas liquid chromatography

Crystallization and gas liquid chromatography (GLC) have been used to characterize the triglyceride composition of olive and cottonseed oil and their precipitates from acetone or methanol/acetone (10:90, v/v) at −2 C. The precipitate obtained after a 24 hr crystallization of a 5% (w/v) solution of the sample in acetone or methanol/acetone (10:90, v/v) at −2 C was named Precipitate I (P-I); that isolated after 2 successive crystallizations under identical conditions was named Precipitate II (P-II). In each case, the ratio of oleic to linoleic acid (O/L) was calculated and proved to be a useful index for detecting adulteration of olive oil with cottonseed oil. In olive oil, the ratio O/L increased from the original sample to its precipitates, whereas in cottonseed oil and the adulterated samples the ratio O/L was lower in the precipitates than in the original sample. For olive oil P-II, the lowest value of the ratio O/L was 8.4; for the adulterated samples it was 7.6. On the basis of this index, adulteration of olive with cottonseed oil as low as 10% can be detected. Hydrolysis of P-1 by porcine pancreatic lipase and analysis of the fatty acids of the sn-2 position showed that the enrichment factor of linoleic acid varied between 1.11–1.30 for olive oil and between 1.55–1.90 for the adulterated samples. Even for adulteration with 5% cottonseed oil, the enrichment factor appears to increase (1.55–1.57) and can be used as a criterion for adulteration.     

Free and Esterified 4,4′-dimethylsterols in Hazelnut Oil and their Retention During Refining Processes

Free and esterified forms of sterols provide detailed information on the identity and the quality of vegetable oils. In this study, 4,4′-dimethylsterols in free and esterified forms were investigated in hazelnut and virgin olive oils. Moreover, a sample of solvent-extracted hazelnut oil was refined at the laboratory to monitor the effects of processing on the levels of 4,4′-dimethylsterols. Generally, the level of total 4,4′-dimethyslterols was higher in the esterified form (49–68%) compared with that in free form (32–51%) of these compounds in the hazelnut oil. In virgin olive oil samples, cycloartenol and 24-methylenecycloartanol were present in higher amounts in free forms (70–80%) than in esterified forms (20–30%). Among the refining processes, degumming, deodorization, neutralization and bleaching, only neutralization and bleaching considerably reduced 4,4′-dimethylsterols. In fully refined hazelnut oil, 18 and 37% of lupeol and an unknown compound X in the esterified form were lost, respectively. The loss of these two compounds in the free form was considerably higher, 26 and 72%, respectively. GC–MS analysis showed that adulteration of olive oil with a sample of fully refined hazelnut oil could be detected at a level as low as 2% by tracing lupeol in total or only in esterified forms of 4,4′-dimethylsterols. Further studies on the levels of free and esterified 4,4′-dimethylsterols and their retention during refining processes are anticipated in hazelnut cultivars from different origins.     

Adulteration and Presence of Polycyclic Aromatic Hydrocarbons in Extra Virgin Olive Oil Sold on the Brazilian Market

Seventy samples sold in the Brazilian market as extra virgin olive oil (EVOO) were evaluated for the presence of the 13 polycyclic aromatic hydrocarbons (PAH) classified as carcinogenic and genotoxic by the Joint FAO/WHO Expert Committee on Food Additives (JECFA), to verify if the products were adulterated and to evaluate if there is a correlation between PAH presence and adulteration. PAH were detected in 93% of the samples, with summed levels varying from not detected to 41.10 μg/kg. Five samples showed BaP concentration above acceptable levels set by European legislation and by Brazilian regulation (2.0 μg/kg) and 7 presented PAH4 levels above the limit set by European legislation (10.0 µg/kg). The levels of fatty acid composition, sterols content, stigmastadiene and specific extinction did not comply with both Brazilian and International Olive Council (IOC) standards in 18, 31, 30 and 21% of the samples, respectively. The tolerance levels for these analyses in the Brazilian standards are 55.0–83.0 g/100 g (oleic acid), 3.5–21.0 g/100 g (linoleic acid), ≤0.05 g/100 g (trans-oleic acid), ≤0.05 g/100 g (trans-linoleic + trans-linolenic acid), ≤0.15 mg/kg (stigmastadiene), ≤2.50 (K232), ≤0.22 (K270), ≤0.01 (?K), 1000–1600 mg/kg (Σ sterols). Results indicate that 19 samples were adulterated. According to principal component analysis, samples were distinguished as: (1) EVOO with addition of vegetable oil from another source, (2) EVOO with addition of refined oil and (3) samples possibly not adulterated. The variable ΣPAH was related mainly to samples of EVOO with addition of vegetable oil from another source.     

Investigating Chemical Properties and Oxidative Stability of Kernel Oil from Pistacia khinjuk Growing Wild in Iran

In this study in order to introduce a new vegetable oil, oxidative stability and chemical characteristics of Pistacia khinjuk kernel oil (PKKO) as compared with P. atlantica kernel oil (PAKO) and extra virgin olive oil (EVOO) were investigated. Oxidative stability of studied oils was considered based on the conjugated diene value (CDV), carbonyl value (CV) and oil/oxidative stability index (OSI) through an 8‐h thermal process at 170 °C. Also, chemical characteristics [fatty acid composition, unsaponifiable matter (USM), total tocopherols (TT), total phenolics (TP) and total sterols (TS), iodine value, saponification number and waxes] of these oils were analyzed. The ratio of polyunsaturated fatty acids to saturated fatty acids and the oxidizability (Cox) value of PKKO (1.14 and 2.78; respectively) were between those of PAKO (2.37 and 4.23; respectively) and EVOO (1.14 and 2.78; respectively). USM content of the three studied oils was between 1.1 and 1.51 %. TT and TP contents of PKKO (619.4 and 26.6 ppm) were lower than those of PAKO (845.33 and 75.22 ppm) and higher than those of EVOO (365.23 and 19.78 ppm). TS contents of PKKO, PAKO and EVOO were 2,500, 2,150 and 3,800 ppm, respectively. Oxidative stability data indicated that PKKO is the most resilient oil against lipid oxidation, followed by PAKO and EVOO. CDV significantly increased by the lowest speed for PKKO, followed by PAKO and EVOO. Increase of CV and reduction of OSI for PKKO, PAKO and EVOO were 29.2, 128 and 338.7 and 32.8, 67.9 and 79.3 %; respectively.     

Influence of Irrigation Modalities (Irrigation Management and Dryland), Fruit Ripening,and Cultivation Modality (Organic and Conventional) on Quality and Chemosensory Profile of Hojiblanca and Picual Extra Virgin Olive Oils

A study with controlled field and authentic samples of olives, obtained in similar conditions of soil, climate, region, harvest, and with the same cultivation techniques and considering simultaneously different agronomic factors (olive variety, fruit ripening degree, irrigation, and organic or conventional production system) is performed to evaluate their influence on quality and added value of extra virgin olive oil (EVOO). Agronomical and physicochemical parameters, polyphenols, tocopherols, and fatty acid composition and volatile and sensory profiles are determined in Hojiblanca and Picual VOOs obtained from different fruit ripening degrees and different cultivation modalities (conventional with and without irrigation, and organic with irrigation). Among volatile compounds, 1-hydroxy-2-propanone, (E)-linalool oxide, and 2-acetylfuran are described for the first time in EVOO. The variable that most influences the chemosensory composition of EVOOs is the variety, followed by the stage of ripeness, and, within each variety, the cultivation modality. Organic irrigation differ from conventional modalities, showing significant differences in acidity, stability, tocopherol and polyphenol contents, fatty acid composition, and sensory attributes. Practical Applications: Results are of great importance, due to their applicability to the EVOO sector, allowing one to know the qualitative, chemical and organoleptic differences between organic and conventional EVOO, and factors that improve the quality and performance of EVOO.     

On the composition of Iranian olive oil

Two samples of virgin olive oil and one sample of hexane-extracted husk oil coming from Iran were examined. The analyses included physical and chemical characteristics, the composition of total fatty acids and fatty acids at the glyceride 2-position by gas liquid chromatography (GLC) of methyl esters, the triglycerides composition calculation according to Vander Wal theory, the separation of the alcoholic fractions (sterols, 4-methylsterols, triterpene alcohols, triterpene dialcohols and aliphatic alcohols) of the unsaponifiable matter by thin layer chromatography (TLC), the quantitation and the composition of these fractions by GLC of TMS derivatives. The results were in line with data from literature for olive oils of different origin, with the exception of: a high content of unsaponifiable matter (1.75 and 1.95% for virgin oils, 5.33% for husk oil); a high amount of sterols for husk oil (562 mg/100 g oil); a low content of SE 30 apparent β-sitosterol for husk oil (91.1%); a low amount of triterpene dialcohols (1 mg/100 g oil) and triterpene alcohols (78 and 91 mg/100 g oil) for virgin oils; a content of cycloartenol (60.2–66.9%) higher than the 24-methylenecycloartanol one (22.8–26.6%; a content of C₂₄ linear saturated alcohol (33.9–38.0%) slightly higher than the C₂₆ alcohol one (29.3–32.8%).     

Handheld Near‐Infrared Spectroscopy for Distinction of Extra Virgin Olive Oil from Other Olive Oil Grades Substantiated by Compositional Data

Miniaturization of analytical technology has paved the way for in‐situ screening of foods. In the current study, the spectral features of olive oils are examined by handheld near‐infrared spectroscopy to explore the technology's capabilities to distinguish extra virgin olive oil (EVOO) from lower grade oils. Eighty EVOO, forty refined olive oil (ROO), and ten pomace olive oil (POO) samples are analysed for their spectral and compositional features. The latter included analysis of the fatty acids (FAs), the chlorophylls and carotenoids, chromatic coordinates and moisture contents. The 1350–1570 nm wavelength range appeared most suitable for distinction of the oils. One‐class classification models with three different classifiers are subsequently estimated using this range, and their quantitative performance is assessed from probabilistic data. Soft independent modeling of class analogies models appears to predict the identity of the oils with a high success rate. Compared to the other oils, POO comprises a significantly higher and lower proportion of polyunsaturated and monounsaturated FAs, respectively. Higher contents of chlorophylls, carotenoids, and moisture are noted for EVOO. The relevant spectral information for distinction of the oils correlates strongly with the degree of unsaturation of the oils as well as their levels of chlorophylls, carotenoids, and moisture. Practical Applications: The findings of this study demonstrate that the handheld NIRS technique is promising for future rapid screening of olive oil grades. The statistical methods used and the robust validation procedure will help potential users to select the optimal strategy for multivariate data analysis. In addition, the exploration of correlations with compositional characteristics provides insight into the handheld NIRS working mechanism in regard to EVOO authentication.     

Use of high-resolution 13C nuclear magnetic resonance spectroscopy for the screening of virgin olive oils

¹³C Nuclear magnetic resonance (NMR) spectra of 104 oil samples were obtained and analyzed in order to study the use of this technique for routine screening of virgin olive oils. The oils studied included the following: virgin olive oils from different cultivars and regions of Europe and north Africa, and refined olive, “lampante” olive, refined olive pomace, high-oleic sunflower, hazelnut, sunflower, corn, soybean, rapeseed, grapeseed, and peanut oils, as well as mixtures of virgin olive oils from different geographical origins and mixtures of 5–50% hazelnut oil in virgin olive oil. The analysis of the spectra allowed us to distinguish among virgin olive oils, oils with a high content of oleic acid, and oils with a high content of linoleic acid, by using stepwise discriminant analysis. This parametric method gave 97.1% correct validated classifications for the oils. In addition, it classified correctly all the hazelnut oil samples and the mixtures of hazelnut oil in virgin olive oil assayed. All of these results suggested that ¹³C NMR may be used satisfactorily for discriminating some specific groups of oils, but to obtain 100% correct classifications for the different oils and mixtures, more information than that obtained from the direct spectra of the oils is needed.     

Chemical Composition of Turkish Olive Oil––Ayvalik

Although large amounts of olive oil are produced in Turkey, not much information on its chemical composition is available in the literature to date. The aim of this study was to evaluate the chemical composition of commercial olive oils produced from the Ayvalik olive cultivar in Canakkale, Turkey. Five different samples corresponding to the olive oil categories of extra virgin (conventional, extra virgin olive oil (EVOO), and organic extra virgin olive oil (OGOO) production), virgin olive oil (OO-1), ordinary virgin olive oil (OO-2) and refined olive oil (RFOO) were evaluated. Olive oils were collected from two consecutive production years. According to the free fatty acids, the absorbance values (K₂₃₂ and K₂₇₀), and peroxide values of all the samples conformed to the European standards for olive oil. The level of oleic acid was in the range of 68–73%; while the linoleic acid content was significantly lower in the refined olive oils. The tocopherol and polyphenol content was in the lower range of some European olive oils. However, pinoresinol was a major phenolic compound (5–77 mg/kg depending on the oil category). Its content was markedly higher than in many other oils, which would be a useful finding for olive oil authentication purposes.     

Off-line coupling of high-performance liquid chromatography and 1H nuclear magnetic resonance for the identification of filbertone in hazelnut oil

A new procedure is presented for off-line coupling of high-performance liquid chromatography and proton nuclear magnetic resonance spectroscopy (¹H NMR) in hazelnut oil analysis. The optimization of some parameters affecting both the liquid chromatography preseparation step and the effective multiple-solvent suppression required for the NMR study enabled us to determine the presence in a hazelnut oil of (E)-5-methyl-hept-2-en-4-one (filbertone), a marker previously proposed to detect the adulteration of olive oil with hazelnut oil. The described procedure requires the filtration of the oil prior to its introduction into the chromatographic system and combines the advantages of providing sufficient sensitivity and selectivity with simple methodology and reduced sample handling.     

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.