Workshop on olive oil authentication

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1 Workshop on olive oil authentication Madrid, Spain 10 & 11 June 2013 Organised by European Commission Directorate General Agriculture and Rural Development & European Commission Joint Research Centre Institute for Reference Materials and Measurements With the participation of the International Olive Council

2 Poster Preparation of certified reference materials of olive oil for physicochemical and sensory characteristics Chromatographic fingerprinting methodology for olive oil authentication Fatty Acid Composition and d13c of Bulk and Individual Fatty Acids as Marker for AuthenticatingItalian PDO/PGI Extra Virgin Olive Oils On-line HPLC-GC-FID for the evaluation of the quality of olive oils though the methyl, ethyl, and wax esters Detection of plant oil DNA using molecular markers and PCR analysis: a tool for disclosure of olive oil adulteration FT-MIR/ATR monitoring of virgin olive oil oxidative stability under mild storage conditions Challenges of U.S. Enforcement Increase with Conflicting Standards & Methods Authors L. Cuadros-Rodríguez, A. González-Casado, et al. A. González-Casado, L. Cuadros-Rodríguez, et al. A. Faberi, F. Fuselli, et al. M. Biedermann M. Vietina, C. Agrimonti, N. Marmiroli M. Z. Tsimidou, N. Nenadis, et al. E. Balch

3 PREPARATION OF CERTIFIED REFERENCE MATERIALS OF OLIVE OIL FOR PHYSICOCHEMICAL AND SENSORY CHARACTERISTICS L. Cuadros-Rodríguez 1, A. González-Casado 1, A. Carrasco-Pancorbo 1, C. Ruiz-Samblás 1, J.A. García-Mesa 2, F.P. Rodríguez-García 3 1 Unit of Chemical metrology and Qualimetrics, Department of Analytical Chemistry, Faculty of Sciences, University of Granada, C/ Fuentenueva s/n, E-18071, Granada, Spain. 2 Centro "Venta del Llano", Agricultural and Fishery Research Institute (IFAPA), Consejería de Agricultura, Pesca y Medio Ambiente, Junta de Andalucía, Ctra. Bailén-Motril, km. 18.5, Apdo. correos nº 50, E Mengíbar, Jaén, Spain 3 Agrofood Quality Control Service, Consejería de Agricultura, Pesca y Medio Ambiente, Junta de Andalucía, C/ Tabladilla s/n, E-41071, Sevilla, Spain What s a Certified Reference Material (CRM)? A material, sufficiently homogeneous and stable with respect to one or more specified properties, which has been established to be fit for its intended use in a measurement process, and has been characterized by a metrologically valid procedure for one or more specified properties, accompanied by a certificate that provides the value of the specified property, its associated uncertainty, and a statement of metrological traceability (ISO/IEC Guide 99:2007). A CRM can: -Improve the comparability of measurement results, and -Be used for calibration, validation and/or quality control purposes Aim of the study Herewith we present the results of a series of studies for the elaboration, certification and distribution of several CRMs of olive oil, which could be used in olive oil quality control laboratories Everything was carried out within the frame of a collaboration between: Andalusian Regional Government (Spain) Andalusian Agricultural and Fishery Research Institute (IFAPA IFAPA) University of Granada Structure of the project 1st stage: InterOLEO CRM The certification of all the analytical parameters is related to the physicochemical characteristics (updated Regulation EU 2568/91). 2nd stage: SensOLEO CRM We focused on the certification of several sensory properties of olive oils. ANALYTICAL PARAMETERS TO BE CERTIFIED Physicochemical analysis Determination of different physicochemical parameters Acidity Peroxide value Fatty acids myristic (C14:0) palmitic (C16:0) palmitoleic (C16:1, n-7) heptadecanoic (C17:0) heptadecenoic (C17:1) stearic (C18:0) oleic (C18:1, n-9) linoleic (C18:2, n-6) linolenic (C18:3, n-3) arachidic (C20:0) eicosenoic (C20:1, n-11) behenic (C22:0) lignoceric (C24:0) Sterols cholesterol brassicasterol 2,4-methylencholesterol campesterol campestanol stigmasterol 7-campesterol 5,23-stigmastadienol clerosterol β-sitosterol sitostanol 5-avenasterol 5,24-stigmastadienol 7-stigmastenol 7-avenasterol apparent β-sitosterol total sterols Fatty acid trans isomers t-oleic (t-c18:1) t-linoleic (t-c18:2) t-linolenic (t-c18:3) t-linoleic + t-linolenic Waxes C36 C38 C40 C42 C44 total waxes Aliphatic alcohols docosanol (C22) tetracosanol (C24) hexacosanol (C26) octacosanol (C28) total aliphatic alcohols Sensory analysis Panel Test Fruity, bitter and pungent attributes and their levels; any negative attribute?... ECN42 triglycerides total ECN42 (HPLC) theoretical ECN42 (GC) Difference ECN42 UV spectrometry K232 K270 K Terpenic alcohols erytrodiol + uvaol Steradienes 3,5-stigmastadiene Alkyl esters methyl ester C16 ethyl ester C16 methyl ester C18 ethyl ester C18 total FAMEs (C16 + C18) total FAEEs (C16 + C18) Further steps: Once the materials have been produced, we consider as necessary: -to assure the homogeneity of the units of the lot, -to characterize the values of the analytical parameters to be certified, and - to evaluate stability of the materials, under the recommended d storage conditions. References - L Cuadros-Rodríguez, J.M. Bosque-Sendra, A.P. de la Mata-Espinosa, A. González-Casado, P. Rodríguez-García, Elaboration of Four Olive Oil Certified Reference Materials: InterOleo-CRM 2006 Certification Study, Food Anal. Methods (2008) 1, J.M. Bosque-Sendra, P. de la Mata-Espinosa, L. Cuadros-Rodríguez, A. González-Casado, F.P. Rodríguez-García, H. García-Toledo, Stability for olive oil control materials, Food Chemistry (2011) 125,

4 CHROMATOGRAPHIC FINGERPRINTING METHODOLOGY FOR OLIVE OIL AUTHENTICATION A. González Casado 1, L. Cuadros Rodríguez 1,C.Ruiz Samblás 1,E.Pérez Castaño 1,F.P.Rodríguez García 2,M.G.Bagur González 1 1 Department of Analytical Chemistry, Faculty of Sciences, University of Granada, C/ Fuentenueva s/n, E 18071, Granada, Spain. E mail: 2 Agrofood Quality Control Service, Consejería de Agricultura y Pesca, Junta de Andalucía, C/Tabladilla s/n., E 41071, Sevilla, Spain INTRODUCTION There are several approaches that can be applied to the olive oil authentication. They differ in the scientific technical foundation, according to the information obtained. The most common techniques are: (i) chemical composition; (ii) stable isotopes; and (iii) DNA. The chemical based approach needs the accomplishment of chemical analyses to acquire either explicit or implicit information, about chemical constituents or chemical families related with characteristics to authenticate: geographical origin, botanical variety, category, differentiated quality, absence of foreign oils, etc. In order to practical consequence of the chemical based approach, it could be used three analytical methods: chemical markers, compositional profile, and instrumental fingerprinting. Our research focuses on fringerpringting methodologies. They consider the entire analytical signal, which is acquired and recorded by the analytical instrument, directly from olive oil or from a previously isolated fraction, i.e. a spectrum or a chromatogram. The shape and intensity of the recorded signal constitutes the instrumental fingerprint from the whole olive oil sample, or from the considered fraction, because it is characteristic and reflects implicitly its chemical composition. Therefore, the methodology is based on the existence of the chemical composition and they can be applied when the compositional methods are suitable. FINGERPRINT APPLICATIONS TGAs STs VOCs TRIACYLGLYCEROLS STEROLS VOLATILE ORGANIC COMPOUNDS LC GC LC GC GC PTR MS (1), (2), (3) (3), (4), (5) (*) (*) (*) (6) Edible oil (mainly olive oil) Signal acquisition GC, LC, PTR MS METHODOLOGY Pre processing Baseline correction Peak shifting Mean Center Autoescale Models Chemometrics Data mining Exploratory data analysis, Classification, Prediction REFERENCES AUTHENTICATION OBJECTIVES GC MS chromatograms of vegetable oil blends PCA scores plot obtained from the data of the samples after peak shifting pretreatment TAGs chromatographic profile of the olive oils: (icoshift) (5) scores on the PC3 PC2 PC2 plane (4) Categories, varieties Geographical origin Identity, characterisation Adulteration (1) P.A. de la Mata Espinosa, J.M. Bosque Sendra, R. Bro, L. Cuadros Rodríguez. Discriminating olive and non olive oils using HPLC CAD and chemometrics. Anal. Bioanal. Chem., 399, (2011) (2) P.A. de la Mata Espinosa, J.M. Bosque Sendra, R. Bro, L. Cuadros Rodríguez. Olive oil quantification of edible vegetable oil blends using triacylglycerol chromatographic fingerprints and chemometric tools. Talanta, 85, (2011) (3) C. Ruiz Samblás, C. Arrebola Pascual, A. Tres, S.M van Ruth, L. Cuadros Rodríguez. Authentication of geographical origin of palm oil by chromatographic fingerprinting of triacylglycerols and partial least square discriminant analysis. J. Agric. Food Chem. (enviado, abr 2013) (4) C. Ruiz Samblás, L. Cuadros Rodríguez, A. González Casado, F.P. Rodríguez García, P. de la Mata Espinosa, J.M. Bosque Sendra. Multivariate analysis of HT/GC (IT)MS chromatographic profiles of triacylglycerol for classification of olive oil varieties. Anal. Bioanal. Chem., 399, (2011) (5) C. Ruiz Samblás, F. Marini, L. Cuadros Rodríguez, A. González Casado. Quantification of blending of olive oils and edible vegetable oils by triacylglycerols fingerprint gas chromatographic and chemometrics tools. J. Chromatogr. B 910, (2012) (6) C. Ruiz Samblás, A. Tres, A. Koot, S.M. van Ruth, L. Cuadros Rodríguez, A. González Casado. Proton transfer reaction mass spectrometry volatile organic compound fingerprinting for monovarietal extra virgin olive oil identification. Food Chem., 134, (2012) (*) Currently under study

5 Fatty Acid Composition and d13c of Bulk and Individual Fatty Acids as Marker for Authenticating Italian PDO/PGI Extra Virgin Olive Oils Angelo Faberi*, Fabio Fuselli* Rosa Maria Marianella* and Manuel Sergi * Ministero delle Politiche Agricole Alimentari e Forestali Dipartimento dell Ispettorato Centrale della tutela della Qualità e Repressione Frodi dei Prodotti Agro-alimentari Laboratorio Centrale di Roma, Via del Fornetto, Università degli Studi di Teramo Facotà di Agraria, Via Carlo R. Lerici Mosciano Sant'Angelo (TE) INTRODUCTION Extra virgin olive oil (EVOO) is a fundamental landmark of the Mediterranean diet which has noticeable nutritional and organoleptic characteristics. European Regulation (EEC) 2568/91 has been setting the minimum requirements in order to allow labelling of an oil as extra virgin. These general requirements, are based on physical-chemical and organoleptic parameters directly linked to freshness and quality of the product (free acidity, peroxide index and ultraviolet absorption, panel test and recently alkyl esters) and other purity parameters, intended to prevent fraudulent mixing with cheaper oils (refined, pomace or seed oils) However EVOOs products exhibit great differences, either in organoleptic or nutritional or functional characteristics (e.g. polyphenols and tocopherols content, aroma, etc.), which are related to cultivar of olives, production techniques and geographical origin. The lack of official methods of analysis for assessing the origin implies that official control of special quality regulated production, such as PDO or PGI, must rely only on checking the accompanying paper documentation. The use of Isotope Ratio Mass Spectrometry (IRMS) has demonstrated as a tool that can improve geographical discrimination of unknown samples, because this technique presents the advantage of giving results which are almost independent from cultivar employed and production technique (1-3). Figure 1a: box-and-whiskers plot of main constituents fatty acids methyl esters as a function of the geographical area of origin; In this work the evaluation of the composition of Fatty Acids Methyl Esters (FAME) alongside with the determination of stable isotope ratio of C in bulk oils and in main FAME constituents has been made EXPERIMENTAL Samples: Sampling of authentic extra virgin olive oil was made by ICQRF inspective personnel at oils mils. Selected olive oils of known origin and designated to achieve the Protected Designation of Status. For each PDO/PGI three oil samples, related to three different maturation stages, were collected at a distance of about days from each other. For each sample additional information regarding agronomical and technological features were also collected. Figure 1b: box-and-whiskers plot of the distribution of δ 13C/12C isotope ratios of bulk oil as a function of the geographical area of origin; Oils samples were collected in 250 ml dark glass bottles covered with a black plastic envelope and then shipped to the laboratory. Upon receive oils were filtered by means of a 0,45 mm barrel type nylon filter, in order to remove any sediment eventually formed which may deteriorate the product. Samples were kept at 8 C until the analysis. An individual set of three samples was taken for each geographical mention for every specific PDOs who has such distinction. Fatty acid analysis by GC/FID : samples were transesterified with methanolic potassium hydroxide according to official method reported in annex X(A) of Regulation (EC) 702/ analysis by gas chromatography of methyl esters of fatty acids. C isotope analysis of bulk oil by EA/IRMS: The carbon isotope ratio (13C/12C) of bulk oils was determined by flash combustion on a Thermo (Bremen, Germany) elemental analyzer (EA) connected to a Thermo Fisher Delta V Plus (Bremen, Germany) isotope ratio mass spectrometer (IRMS) by analyzing the ratio of ionic currents of m/z 44 (12C16O16O), m/z 45 (13C16O16O) ed m/z 46 coming from carbon dioxide arising from sample combustion in the elementar analyzer. The stable isotope composition of carbon, is calculated in delta (δ) notation as the per thousand ( ) deviations of the isotope ratio relative to known standards (d% C = R sample - R standard / R standard) For 13C\12C ratio the standard utilized is Vienna Pee Dee Belemnite limestone (VPDB). Figure 1c: box-and-whiskers plot of the δ 13C/12C isotope ratio of the methyl esters of fatty acids as a function of the geographical area of origin; Deterrmiantion of isotopic ratio of individual FAME: the determination was realized with a GC Isolink device constitued by a GC Thermo Trace FID coupled to a ThermoFinnigan Delta V Plus isotopie ration mass spectrometer by means of a combustion interface GC/C/IRMS. Results were corrected for the contribution of d 13C the methanol emplyoied for trans-esterification. Esterification procedure was the same as for the determiantion of the fatty acid composition. RESULTS Figure 2: macro-regions where samples were taken In order to carry out the statistical analysis, samples were divided into four categories defined according to the area of origin The distribution of samples within each category was first evaluated by univariate analysis through representation of significant discriminant variables with box and whisker diagrams which show the dispersion of the samples within each class in function of the measured values for the isotopic ratio (Figure 1 - a, b, c).. Samples were divided into the following four macro-regions (figure 2) Nord : including samples produced in the regions of Lombardy, Veneto, Trentino, Liguria and Emilia Romagna Center: including samples produced in Tuscany, Latium,. Abruzzo Umbria, Marche, Sardinia South : including samples produced in Campania, Apulia, and Calabria Sicily : including samples produced in Sicily Composition data has demonstrated that there is a certain degree of correlation among main constituents fatty acids with geographical area of proven origin according to latitude. The values of d13c in both bulk and FAME also have indicated a similar evidence of correlation. However overlapping zones are very wide. Figure 3: graphs of the first and second principal component obtained from (A) compositional variables only; (B) compositional variables and the δ 13C/12C of bulk oil; compositional variables and the δ 13C/12C of bulk oil and of the main constituent fatty acids (C). MULTIVARIATE ANALYSIS The use of multivariate analysis represent a tool that can improve geographical discrimination of unknown samples Principal component analysis (PCA), applied in the first stage of the data processing, represents one of the most frequently used chemometric tools, because allows to project in an easy way data from an higher to a lower dimensional space. In the preliminary analysis of the olive oil data, 3 distinct preliminary PCA were performed to investigate clustering of samples on the basis of the area of provenience (Figure 3). The PCA shows that the geographical discrimination of the samples improves by making of appropriate combinations of the parameters up to now considered individually. As one can see the introduction of the measure of the carbon isotope ratio on bulk oil and of the individual components fatty acids makes gives a better separation of the four classes. The diagrams have been built after an autoscaling pretreatment of each variable. PLS-DA techniques as well shows (Figure-4) that when the whole set of data is considered (isotopic and composition), there is a substantial discrimination of the origin of the oil. As it can be seen, a clear separation between the data related to geographical origin can be observed. Figure 4: Figure shows the PLS-DA score plot of the first three latent variables using d C13 data. In the plot about 61% of the total variance of the data is represented.. REFERENCES 1) Angerosa, F., Breas, O., Contento, S., Guillou, C., Reniero, F., Sada, E. (1999). Application of stable isotope ratio analysis to the characterization of the geographical origin of olive oils. Journal of Agricultural and.food Chemistry, 47, ) Bontempo, L., Camin, F., Larcher, R., Nicolini, G., Perini, M., Rossmann, A. (2008). Discrimination of Tyrrhenian and Adriatic Italian olive oils using H, O, and C stable isotope ratios. Rapid Communications in Mass Spectrometry, 23, ) Camin, F., Larcher, R., Perini, M., Bontempo, L., Bertoldi, D., Gagliano, G., Nicolini, G., Versini, G. (2008). Characterization of authentic Italian extra-virgin olive oils by stable isotope ratios of C, O and H and mineral composition. Food Chemistry, 118,

6 Me-17:0 (VS1) Me-18:1 Me-20:2 (VS2) Et-20:0 (IS1) P-20: :0 (IS2) Et-18:1 Squalene P-18:1 P18:0 P-20: :X On-line HPLC-GC-FID for the evaluation of the quality of olive oils though the methyl, ethyl, and wax esters Maurus Biedermann Authority of the Introduction Increased ester contents in olive oils indicate degraded olives: methanol and ethanol formed during fermentation are transesterified with fatty acids from the triglycerides. Wax esters are more readily extracted from the soft skin of overripe olives. A promising correlation of chemical analysis and sensorial evaluation was confirmed: oils with low concentration of these esters were of high sensory quality, whereas many of the oils with high contents not even met the requirements for extra virgin olive oils. Limits on the alkyl and wax ester content in olive oils are specified in the Commission Regulation 61/2011. Analytical method Diluted oils are pre-separated by normal phase HPLC and the ester fraction on-line transferred into GC via the Y-interface (fig. 1) by fully concurrent solvent evaporation (fig 2). The method includes several verification standards to monitor proper performance in the critical aspects for each analysis: wax and methyl esters are eluted at different times from HPLC; standards were introduced to monitor the edges of the fraction window. Fully concurrent eluent evaporation may cause losses of the most volatile fatty acid methyl esters through the vapor exit. A volatile verification standard was added to optimize the transfer conditions [1]. waste FID vapor exit carrier gas Y-piece tv UV detector bfv iv auto sampler LC column separation column uncoated pre-column 1-15 m LC pump iv: injection valve bfv: backflush valve tv: transfer valve - Partially concurrent solvent evaporation: solvent trapping retains volatile sample components during transfer and solvent discharge via the solvent vapor exit. - The transfer volume and evaporation rate has to be adjusted to meet the capacity of the retention gap given by the dimension of the uncoated pre-column (7-15 m, 0.53 mm i.d.). - Fully concurrent solvent evaporation can be used if volatiles are not analyzed. - It is preferred whenever applicable, since it requires short coated pre-columns of m (less adsorptivity) and the adjustment of the conditions is usually uncritical. - Fatty acid methyl esters are among the most volatile compounds to be transferred without losses using this technique. - Optimization of the condition may be performed by a mixture of n-alkanes (fig. 3). Sterol esters 28-18:X A Me-18:1 Et-18: :X Me-17:0 (VS1) Et-20:0 (IS1) Me-20:2 (VS2) 21-22:0 (IS2) 26-18:X P-18:1 P-20: B Temperature program 7 /min 140 C 360 C Figure 5: HPLC-GC-FID chromatograms of esters of interest; A extra virgin olive oil with rather high concentrations; B extra virgin oil with low concentration of these components. IS: internal standard; VS: verification standard; P: phytol esters Dilution: 25 mg edible oil + internal/verification standard mixture ml hexane Injection volume: 10 µl LC column: 250 x 2 mm, Spherisorb Si 5 µm Eluent: 4% MTBE/pentane at 300 µl/min Transferred fraction: 2-4 min = 600 µl Pre-column: 40 cm x 0.53 mm i.d., 0.03 µm OV-1701-OH, connected to a metal T-piece Separation column: 20 m x 0.25 mm i.d., 0.12 µm PS-255 (dimethyl polysiloxane) Carrier gas: Helium at 60 kpa, reduced to 40 kpa during transfer Oven temp. program: 50 C (3 min), 30 /min to 130 C, 7 /min to 360 C (4 min) Instrumentation: LC-GC 9000, Brechbühler AG: combi PAL autosampler, Phoenix 40 syringe pump, Thermo Trace GC Sensorial testing was done by the Swiss Olive Oil Panel (SOP) from the University of Applied Sciences Wädenswil (ZHAW). Results 100 olive oils from the Swiss marked sold as extra virgin were analyzed chemically. A selection of these (with low and high contents of methyl and ethyl esters) were also sensorial evaluated. According to previous work [2] the best oils were low in contents of methyl and ethyl oleate. Olive oils with elevated contents of these esters and/or straight chain wax esters were devaluated as virgin or lampant oils based on the sensorial testing. The two types of quality markers have little common background (poor correlation, fig. 8): - A high wax ester content is indicative of soft, ripe or overripe olives. - Fatty acid methyl and ethyl esters originate from alcohols formed by fermentation. Refined olive oils: - The concentration of the wax esters is high, however the concentration of methyl/ethyl esters is low. Probably deodoration of the oil removed a large proportion of these more volatile esters. Oil from fresh and partially degraded olives (fig. 6) was isolated in the laboratory and analyzed for there ester composition (fig. 7): - Phytol esters (P) are predominating; presented after reduction by factor 5. - The concentration of the phytol, geranyl-geraniol (G) and benzyl (Bz) esters do not vary significantly times more straight chain palmitates (16:0) and unsaturated C18 acid esters (18:X) of C22-C28 alcohols were extracted from the softer skin of the degraded olives. - Degradation caused the concentration of methyl and ethyl oleate (18:1-Me, 18:1-Et) to increase by a factor of Figure 8: Sum of straight chain wax esters plotted against sum of methyl/ethyl oleate. A selection of oils were sensorial evaluated. Light green box: limits specified in the Commission Regulation 61/2011, dark green box: samples within proposed stricter limits. Conclusions Methyl and ethyl esters of fatty acids are useful indicators for determining the quality of olives and the oil produced from these. Online HPLC-GC provides a largely automated method for routine analysis. The high stability of FID as well as the large number of samples which can be analyzed daily with a minimum of manpower recommends the method for routine use. A more detailed analysis of the wax ester fraction is described in reference [3] Peak areas (%) C-Atoms oc 32 C 50 C 70 C 90 C x5 Concentration (mg/kg) Degraded Fresh :0 18:X P G Bz 18:1-Me 18:1-Et Me-18:1 + Et-18:1 (mg/kg) Large volume on-column transfer partially concurrent solvent evaporation syringe needle solvent vapor carrier gas low boilers retained by solvent trapping fully concurrent solvent evaporation solvent vapor + low boilers high boilers Figure 2: Principle of partially vs. full concurrent solvent evaporation Figure 3: n-alkane mixture transferred at different oven temperatures; normalized peak areas. Verification The performance of each analysis is checked by built in tools: - Losses of fatty acid esters by co-evaporation with the eluent is critical applying concurrent solvent evaporation. The internal standard (IS1, ethyleicosanoate, Et-20:0) is less volatile than the methyl and ethyl oleate. A more volatile verification standard is added, methyl heptadecanoate (VS1, Me-17:0). The ratio Me-17:0/Et-20:0 is monitored. - Another critical point are shifting retention times in NPLC, the analytes may be eluted off the LC fraction window. The wax ester 21-22:0 (IS2) is eluted at the beginning of the fraction. Methyl eicosadienoate (VS2, Me-20:2) is added as second verification standard, its elution determines the end of the fraction (fig. 4). The ratios between IS2, VS2 and IS1 is monitored. Extra virgin, not evaluated Extra virgin Devaluated extra virgin Raffinate Straight chain wax esters (mg/kg) wax esters, IS2 ethyl esters, IS1 methyl esters, VS2 Figure 1: Components of an on-line HPLC-GC-FID instrument. Figure 4: LC elution order of analytes, internal and verification standards LC fraction Figure 6: Olives from the same tree: good shape (left); damaged olives (right) Figure 7: fresh versus degraded olives References

7 DETECTION OF PLANT OIL DNA USING MOLECULAR MARKERS AND PCR ANALYSIS: A TOOL FOR DISCLOSURE OF OLIVE OIL ADULTERATION Michelangelo Vietina, Caterina Agrimonti, Nelson Marmiroli Department of Life Sciences, University of Parma, Parco Area delle Scienze 11A, Parma, Italy ABSTRACT Extra virgin olive oil is frequently subjected to adulterations with addition of oils obtained from plants other than olive. DNA analysis is a fast and economic tool to identify plant components in oils. Extraction and amplification of DNA by PCR was tested in olives, in milled seeds and in oils, to investigate its use in olive oil traceability. DNA was extracted from different oils made of hazelnut, maize, sunflower, peanut, sesame, soybean, rice and pumpkin. Comparing the DNA melting profiles in reference plant materials and in the oils, it was possible to identify any plant components in oils and mixtures of oils. Real-Time PCR (RT-PCR) platform has been added of the new methodology of High Resolution Melting (HRM), both were used to analyze olive oils mixed with different percentage of other oils. Results showed HRM a cost effective method for efficient detection of adulterations in olive oils. 1

8 DNA EXTRACTION FROM OILS Yields of DNA (ng/ml of starting volume of oil) after extraction based on NucleoSpinPlant kit and CTAB.. The yields are expressed as averages of three independent extractions, with standard deviation. REAL-TIME PCR ANALYSIS OF OILS Melting curves analysis of amplicons obtained by Real Time PCR conducted on DNA extracted from leaves (or seeds) and oils. (A) olive; (B) hazelnut; (C) maize; (D) sunflower; (E) sesame; (F) rice; (G) pumpkin; (H) peanut. 2

9 SEQUENCE CHARACTERIZED AMPLIFIED REGION The use of a SCAR marker, derived from multilocus markers, such as AFLPs or RAPDs, can allow to find the adulteration of an olive oil with a non olive oil, such as hazelnut oil. Moreover, a SCAR marker can be used in a high-throughput platform to assess and quantify the contribution of a single cultivar in commercial multivarietal oils. In Real-Time PCR, a SCAR marker, named CP-rpl16T, derived from an AFLP fingerprint of olive oil, was applied either on DNA extracted from (1) leaves and from a (2) 100% olive oil and (3) 90% olive oil and 10% hazelnut oil DETECTION OF PLANT OIL DNA USING HIGH RESOLUTION MELTING (HRM) POST PCR ANALYSIS: A TOOL FOR DISCLOSURE OF OLIVE OIL ADULTERATION A. Red curve: HRM of DNA extracted from olive oil; Blue : HRM of DNA extracted from maize seed oil; Green : HRM of DNA extracted from an olive and maize oil mix (90%-10%). B. B. Red : HRM of DNA extracted from olive oil; Blue : HRM of DNA extracted from sunflower seed oil; Green : HRM of DNA extracted from an olive and sunflower oils mix (90%-10%). C. Red : HRM of DNA extracted from olive oil; Blue : HRM of DNA extracted from hazelnut seed oil; Green : HRM of DNA extracted from an olive and hazelnut oils mix (90%-10%). 3

10 Acknowledgements This study has been carried out with financial support from the Commission of the European Communities, specific RTD programme Quality of Life and Management of Living Resources project, QLK1-CT , Traceability of origin and authenticity of olive oil by combined genomic and metabolomic approaches (OLIV-TRACK) coordinated by N. Marmiroli. The content of this paper does not necessarily reflect the Commission of the European Communities views and in no way anticipates the Commission s future policy in this area. This paper had also the contribute of the Italian Minister of University and Research special program PRIN Rintracciabilità della composizione e dell origine di oli d oliva DOP, IGP e 100% Italiani attraverso metodiche genomiche, proteomiche e metabolomiche coordinated also by N. Marmiroli and a contribute from the University of Parma (fund FIL 2002, 2003, 2004, 2005, 2006). This work was also supported financially by Emilia-Romagna (IT) Regional project SIQUAL within the research framework PRRIITT, Misura 3.4. References Pafundo, S., Agrimonti, C., Marmiroli, N. (2005). Traceability of plant contribute in olive oil by AFLPs. Journal of Agricultural and Food Chemistry, 53, Pafundo, S., Agrimonti, C., Maestri, E., Marmiroli, N. (2007). Applicability of SCAR marker to food genomics: olive oil traceability. Journal of Agricultural and Food Chemistry, 55, Vietina, M., Agrimonti, C., Marmiroli., N. (2013). Detection of plant oil DNA using High Resolution Melting (HRM) post PCR analysis: a tool for disclosure of olive oil adulteration. Food Chemistry, In press. 4

11 FT-MIR/ATR monitoring of virgin olive oil oxidative stability under mild storage conditions & Maria Z. Tsimidou, Nikolaos Nenadis, Ioannis Tsikouras Polidoros Xenikakis School of Chemistry, Laboratory of Food Chemistry and Technology, Aristotle University of Thessaloniki, Thessaloniki, Greece, International Workshop in Bioactive compounds from Olea europaea: Chemistry and Biology (EU IOC), Madrid June 2013 Introduction Virgin olive oil (VOO) freshness has become a matter of concern among consumers in relation to VOO exceptional nutritional and sensory characteristics. As loss in the latter are observed in the oil mill transportation or at sale points upon storage due to practices that accelerate oxidation and hydrolysis 1, scientific support is required in cases of dispute. 2 Discussions are on the way for updating the relevant EU regulations on VOO quality characteristics. Toward this direction modernization of methods of analysis is expected Aim of the study The exploitation of the multiple information provided in situ by Fourier Mid-IR spectroscopy equipped with an Attenuated Total Reflectance (ATR) cell as a means to extract information for loss of VOO freshness under mild storage conditions for a period of 12 months

12 Results Table 1. Value ranges of quality indices determined for the test samples (n = 11) at different storage periods in the dark Storage period (months) Quality Index t=0 t=6 t=12 Acidity (% oleic acid) PV (meq O 2 / kg oil) K K Figure 1. Frequency distribution of A) peroxide and B) K 232 values for EVOO samples (n = 11) stored in the dark for 0, 6 and 12 months Discussion For all test samples, regardless storage time, the measured values for each index (Table 1) were within the official limits (EU 2568/91 and amendments) for extra virgin olive oil (EVOO) Thus, upon storage up to 12 months, oxidation of samples was still at early stages Frequency distribution analysis for e.g. peroxide (Figure 1A) and K 232 (Figure 1B) values showed a progressive increase which can be justified by the presence of oxygen (10% headspace of the bottles) Changes in acidity were slight

13 Figure 2. Typical FT-IR/ATR spectra of EVOO samples stored in the dark and frequencies of bands of selected functional groups Figure 3. Score plot of the first two PCs obtained by PCA applied to the intensities of selected wavenumbers of EVOO samples stored in the dark for 0 (n=11), 6 (n=11), and 12 (n=11) months PC2 (1.2%) 4 0 months 3 6 months 2 12 months PC1 (98.1 %) Changes in the intensity values at 3470 cm -1 (hydroperoxides) and in values of intensity ratios (A 3006/2924, A 3006/2853, A 3006/1746, A 3006/1465, A 3006/1163, A 1118/1097, A 2853/1746, A 2853/1417, A 2853/1163, A 2853/1118, A 2853/1097, and A 2853/723 ) relevant to the degree of oil unsaturation did not offer more information than the physicochemical criteria when examined one by one Principal component analysis (PCA) applied to the intensity values of the frequencies used in the above-mentioned ratios (Figure 3) showed that samples stored for 1 year (excluding one as an outlier) clearly differed from the rest. Those stored up to 6 months were grouped together with fresh ones Discriminant analysis (DA) after leave one out cross-validation gave a 81.3% correct classification: [6/11 (t=0), 10/11 (t=6), and 10/10 (t=12)]

14 Table 2 Number of principal components, percentage of total variance of PCA in three spectral regions of the FT-IR spectra (2 d derivative) of EVOO samples stored at t=0 (n=11), 6 (n=11), and 12 months (n=11) and the relative classification results of DA Number Total variance Spectral region Classification of PCs explained Original Cross validated t=0 t=6 t=12 t=0 t=6 t= cm % 10/11 10/11 11/11 8/11 10/11 11/ cm % 9/11 10/11 11/11 8/11 9/11 11/ cm % 10/11 10/11 11/11 10/11 10/11 11/11 PC2 (5.3 %) 2 0 months 6 months 1 12 months PC3 (2.4 %) 3 0 months 6 months 2 12 months PC1 (84.4 %) -3 PC1 (84.4 %) Figure 4. Score plot of the first three PCs obtained by PCA applied to the second derivative of the spectral region cm -1 from the spectrum of EVOO samples stored in the dark for 0 (n= 11), 6 (n= 11), and 12 (n= 11) months Examination of the discriminat activity of the 2 d derivative of almost the whole spectral region ( cm -1 ) and two narrower ( and cm -1 ) recently used on acelerated oxidation studies of olive oil at 60 and 180 o C 3,4 showed that using the narrowest region: Classification using a small number of components (only three PCs) was achieved A better separation among oils stored at 0, 6, and 12 months was obtained on the plane PC1-3 Successful classification of samples by 94% was achieved even after cross-validation The frequencies contributing the most in PC3 according to scatter plot were 1229, 1175 (negative loadings), 1065, and 1053 cm -1 (positive loadings) which should be related to C O group

15 Conclusions FT-MIR/ATR is a sensitive technique providing useful information for the early stages of EVOO oxidative status even when physicochemical indices of oil remain within the official limits Only the samples stored for 12 months were easily discriminated from the rest The most useful approach in checking freshness of an EVOO was the statistical treatment of the 2 d derivative of the spectral region cm -1. Present findings add to the usefulness of IR spectroscopy as a rigorous and low cost technique for internal quality control in the olive oil industry but systematic interlaboratory studies are required before it can be considered as a robust tool in VOO analysis References 1) Boskou, D. Olive Oil: Chemistry and Technology, AOCS Press, Champaign (Illinois) ) Frankel, E. N., Mailer, R. J., Wang, S., Shoemaker, C. F., Flynn, D., INFORM Int. News Fats Oils Related Mater. 2011, 22, ) Maggio, R. M., Valli, E., Bendini, A., Gomez-Caravaca, A. M. et al., Food Chem. 2011, 127, ) Mahesar, S. A., Bendini, A., Cerretani, L., Bonoli-Carbognin, M., Sherazi, S. T. H. Eur.J. Lipid Sci. Technol. 2010, 112, Aknowledgements N.N. thanks Ms A. Androulaki for tutorial in SPSS software use. P.X. acknowledges the Union of Agricultural Cooperatives of Sitia for financial support in terms of oil sampling, storage, and physicochemical analyses that were carried out in its installations Experimental part Oil samples and storage conditions Extra virgin olive oil (EVOO) samples (500 ml) from Koroneiki cv olives and representative of the production in the harvest year were collected directly form the three phase decanter of 11 olive oil mills in the regional union of Lassithi (Crete, Greece). Portions were transferred in transparent glass bottles (10% headspace) and sealed hermetically. Those at t=0 were immediately frozen and kept at -18 o C till analysis. The rest were stored in the dark at RT (23 ± 3 o C) for t=6 and 12 months, respectively, and then kept frozen till analysis. Chemical and FT-IR analyses Acidity, peroxide values and K 232/270 indices were measured according to EU Regulation 2568/91 and amendments. FT-IR spectra were acquired (64 scans/sample or background) in the range of cm -1 at a resolution of 4 cm -1 with the aid of an IRAffinity-1 spectrometer (Shimadzu Corporation Kyoto Japan) using 0.8 ml of sample. Data processing The intensities of selected wavenumbers were collected from the untreated spectra recorded for the samples. For chemometrics, all spectra were baseline corrected with the aid of the IR-solution software

16 Challenges of U.S. Enforcement Increase with Conflicting Standards & Methods Authors: Eryn Balch North American Olive Oil Association, 3301 Route 66, Suite 205 Building C, Neptune, NJ USA As the world s largest volume importer of olive oil and third-largest consuming country, U.S. regulators and importers historically relied on expertise from the IOC and producing supplier countries. Today, some rapidly growing domestic producers are exploiting the lack of public knowledge and limited in-country technical expertise and pursuing a mass media campaign aimed at discrediting all imported olive oil along with existing global standards. Enforcement in the U.S. is already a challenge because there is not a national mandatory standard for grade levels of olive oils and olive-pomace oils. If the FDA established a standard of identity it could be enforced anywhere along the supply chain by either government or private action. The USDA published grade standards in 2010, but compliance is voluntary. Mandatory compliance might be partially achieved through a USDA marketing order, although marketing orders are limited to testing only at time of local production or import. Enforcing marketing orders delays imports and is costly to both domestic and imported suppliers, and will not offer complete insurance against adulteration as ultimately there is no oversight to what is blended or sold after lot testing occurs. There are also four U.S. states that have established olive oil standards (CT, CA, NY and OR) but enforcement is limited within state borders. When the industry was unified in support of the IOC standard, progress toward a path to enforcement was happening all of the state standards and the new USDA standard were implemented from Progress began falling apart when the Australian AOA and U.S. UC Davis Olive Center began promoting research based on new methods claimed to be superior to the IOC methods. As the new methods were not being accepted into global standards, promotion campaigns based on these tests have been targeted to the consumer market instead and have become the basis for urging consumers to purchase only domestic olive oils. Of course, consumers (and even many industry personnel) don t understand the meaning of the various authenticity and quality measures. They also don t have access to confirm authenticity directly. The result is consumers that fear purchasing olive oil cut with olive-pomace oil or seed oils are given a false sense of security by certifications like the COOC Seal, which in reality doesn t include authenticity analysis or even use the newly proposed testing methods. The disagreement on which methods or standard is appropriate has created major barriers in the advancement of enforcement opportunities in the U.S. Any effective standard will need to ensure both quality AND authenticity. In an attempt to reduce testing time and costs, divergent standards are now being proposed at various levels of state and federal government. Ultimately, divergent programs create trade issues and further confuse the marketplace. It is critical for the global industry to come together and agree on a common standard so it can be used as the basis for enforcement in countries like the U.S. References International Olive Council, (Nov. 2011). Trade Standard Applying to Olive Oils and Olive-Pomace Oils, COI/T.15/NC No 3/Rev. 6. USDA-AMS, (April 28, 2010). United States Standards for Grades of Olive Oil and Olive-Pomace Oil. California Olive Oil Council, ( ). COOC Extra Virgin Certification Program Frankel, E. N., Mailer, R. J., Shoemaker, C. F., Wang, S. C., Flynn, J. D. (2010). Report: Tests indicate that imported extra virgin olive oil often fails international and USDA standards. UC Davis Olive Center. American Olive Oil Producers Association, (February 12, 2013). Written Submission on behalf of the U.S. Olive Oil Industry in Investigation No , Olive Oil: Conditions of Competition between U.S. and Major Foreign Supplier Industries.

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