Geographical origin assessment of extra virgin olive oil (EVOO) is recognised worldwide as raising consumers’ awareness of product authenticity and the need to protect top-quality products. The need for geographical origin assessment is also related to mandatory legislation and/or the obligations of true labelling in some countries. Nevertheless, official methods for such specific authentication of EVOOs are still missing. Among the analytical techniques useful for certification of geographical origin, nuclear magnetic resonance (NMR) and mass spectroscopy (MS), combined with chemometrics, have been widely used. This review considers published works describing the use of these analytical methods, supported by statistical protocols such as multivariate analysis (MVA), for EVOO origin assessment. The research has shown that some specific countries, generally corresponding to the main worldwide producers, are more interested than others in origin assessment and certification. Some specific producers such as Italian EVOO producers may have been focused on this area because of consumers’ interest and/or intrinsic economical value, as testified also by the national concern on the topic. Both NMR- and MS-based approaches represent a mature field where a general validation method for EVOOs geographic origin assessment could be established as a reference recognised procedure.

/pdf/geographical-origin-assessment-of-extra-virgin-olive-oil-via-3itgknc4.pdf

Geographical Origin Assessment of Extra Virgin Olive Oil via NMR and MS Combined with Chemometrics as Analytical Approaches

Virgin olive oil (VOO) is one of the key components of the Mediterranean diet owing to the presence of monounsaturated fatty acids and various bioactive compounds. These beneficial traits, which are usually associated with the cultivar genotype, are highlighting the demand of identifying characteristics of olive oil that will ensure its authenticity. In this work, the fatty acid (FA) composition of 199 VOO samples from Koroneiki, Megaritiki, Amfissis, and Manaki cultivars was determined and studied by chemometrics. Olive cultivar greatly influenced the FA composition, namely, oleic acid (from 75.36% for Amfissis to 65.81% for Megaritiki) and linoleic acid (from 13.35% for Manaki to 6.70% for Koroneiki). Spearman’s rho correlation coefficients revealed differences and similarities among the olive oil cultivars. The use of the forward stepwise algorithm identified the FAs arachidonic acid, gadoleic acid, linoleic acid, α-linolenic acid, palmitoleic acid, and palmitic acid as the most significant for the differentiation of samples. The application of linear and quadratic cross-validation discriminant analysis resulted in the correct classification of 100.00% and 99.37% of samples, respectively. The findings demonstrated the special characteristics of the VOO samples derived from the four cultivars and their successful botanical differentiation based on FA composition.

Chemometric Study of Fatty Acid Composition of Virgin Olive Oil from Four Widespread Greek Cultivars.

Is the volatile compounds profile a suitable tool for authentication of virgin olive oils (Olea europaea L.) according to cultivars? A study by using HS-SPME-GC-MS and chemometrics

Treating polluted wastewater effluents on a large-scale requires the development of high performance and cost-effective adsorbents. The recycling of waste mandarin peels, an environmentally friendly, and copiously available waste biomass into biochar (MRBC), has been approached. In the context of finding affordable and effective solutions for depollution of wastewater, MRBC was used for the adsorption of two dyes: methylene blue (MB) as well as basic fuchsin (BF) from their individual solutions and binary combinations. Batch adsorption studies were performed by employing the Box-Behnken (BB) design. The adsorption competency of dyes was analyzed to find the percentage removal (%R) and the adsorption capacity (qe, mg/g). The dependent parameters (qe and %R) were determined as a function of pH, dose of MRBC (AD), contact time (CT), and concentration of methylene blue [MB]/ basic fuchsin [BF]. Removal of 98.14% of MB and 83.18% of BF was successfully achieved. Equilibrium experiments depicted that Langmuir and Freundlich models suit adsorption of dyes. The maximum adsorption capacity (qmax) was 99.11 (MB) and 78.01 mg/g (BF), individually. However, when the dyes are combined, the qmax decreased to 57.09 and 68.52 mg/g for MB and BF, correspondingly. The cost of MRBC was estimated to be ∼ 4 USD/kg, while the overall cost of wastewater treatment was estimated to be 1.06 USD/m3/year. 

Techno-economic assessment of waste mandarin biochar as a green adsorbent for binary dye wastewater effluents of methylene blue and basic fuchsin: Lab- and large-scale investigations.

A headspace-solid phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) method was developed herein for the analysis of virgin olive oil volatile metabolome. Optimisation of SPME conditions was performed by Design of Experiments (DoE) and Response Surface Methodology (RSM) approaches and factors, such as sample volume, sample stirring, extraction temperature and time, and desorption temperature and time, were examined to reach optimal microextraction conditions. The potential of the optimised method was then investigated for its use in the classification of Cretan virgin olive oil samples with the aid of multivariate statistical analysis. Certain markers were identified with significance in the geographical classification of Cretan extra-virgin olive oil (EVOO) samples. In total, 92 volatile organic compounds were tentatively identified and semi-quantified, and the data obtained confirm that the method is robust, reliable, and analytically powerful for olive oil classification.

/pdf/optimisation-of-the-hs-spme-gc-ms-approach-by-design-of-nk3zpotq.pdf

Optimisation of the HS-SPME/GC-MS Approach by Design of Experiments Combined with Chemometrics for the Classification of Cretan Virgin Olive Oils

Background In recent years, consumers are asking to know the botanical origin of the olive oil they consume. The objects of the present study were the development of robust chemometric models based on gas chromatography-mass spectrometry (GC-MS) and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) for the purpose of botanical differentiation of three Greek commercial olive oil cultivars. Results Using the solid phase microextraction technique (SPME), volatile compounds (VC) were received and analyzed by GC-MS. Five hydrocarbons and one ester were selected by the forward stepwise algorithm that best discriminated the olive oil samples. From the ATR-FTIR analysis, the spectral regions chosen from the forward stepwise algorithm were associated with the C=O stretching vibration of the esters of triglycerides and the C-H bending vibrations of the CH2 aliphatic group and the double bonds. Application of the supervised methods of linear and quadratic discriminant cross-validation analysis, based on VC data, provided a correct classification score of 97.4 and 100.0%, respectively. The corresponding statistical analyses were used in the mid-infrared spectra where the 96.1% of samples were discriminated correctly. Conclusion The ATR-FTIR and SPME-GC-MS techniques in conjunction with the appropriate feature selection algorithm and classification methods, proved to be powerful tools for the authentication of Greek olive oil. The proposed methodology can be used in industrial setting for the determination of the Greek olive oil botanical origin. This article is protected by copyright. All rights reserved.

Discrimination of botanical origin of olive oil from selected Greek cultivars by SPME-GC-MS and ATR-FTIR spectroscopy combined with chemometrics

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Discrimination of botanical origin of olive oil from selected Greek cultivars by SPME-GC-MS and ATR-FTIR spectroscopy combined with chemometrics