Robustness of NMR-based metabolomics to generate comparable data sets for olive oil cultivar classification. An inter-laboratory study on Apulian olive oils

Piccinonna, Sara; Ragone, Rosa; Stocchero, Matteo; Coco, Laura Del; Pascali, Sandra Angelica De; Schena, Francesco Paolo; Fanizzi, Francesco Paolo

doi:10.1016/j.foodchem.2015.12.064

Cited by 38 publications

(23 citation statements)

References 18 publications

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“…Participation from Germany, Denmark, Norway, France, and the United States reflected the international interest and importance of analyzing the PL composition in krill oils by 31 P NMR spectroscopy. Previous successful NMR interlaboratory tests used the 1 H NMR technique and included untargeted metabolomics of biological samples and plant metabolomics data as well quality control of vegetable and fish oils (Igarashi et al, ; Martin et al, ; Piccinonna et al, ; Ward et al, ; Zailer et al, ). In general, the results of our study showed that the 31 P NMR method was precise and reproducible regarding quantitative analysis of the six specific PL species in krill oil.…”

Section: Resultsmentioning

confidence: 99%

³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

Zailer¹,

Monakhova

Diehl³

2018

J Americ Oil Chem Soc

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A high-resolution 31 P NMR method for determining the concentration of phospholipid (PL) species in krill oil was proficiency tested using an international interlaboratory study. Fourteen laboratories from five countries tested five different krill oil samples providing 17 datasets. Krill oil samples were prepared by the organizer using liquid-liquid extraction and sent to the participants who ran the nuclear magnetic resonance (NMR) analysis and evaluated the spectra. The relative standard deviation (RSD) among all the results provided by the participants varied between 2.1% and 3.3% for the phosphatidylcholine (PtdCho) content and between 2.8% and 12.3% for the sum of other PL. Afterward, an automated procedure was applied to all collected NMR data, which significantly improved the RSD values and provided reliable quantitative results for specific PL (PtdCho, 1-lysophosphatidylcholine [LPC], 2-LPS, PtdEtn, acylphosphatidylethanolamine [APE], and lysophosphatidylethanolamine [LPE]). The RSD varied between 1.6% and 2.7% for PtdCho and between 1.6% and 2.9% for the total phosphorus. Higher but acceptable values were obtained for 1-LPC (5.1% to 8.9%), PtdEtn (7.0% to 10.5%), and LPE (5.7% to 16.5%) due to their small concentrations. The influence of different magnetic field strengths (400-600 MHz), probes, and slight differences in acquisition parameters was assessed as nonsignificant. PtdCho hydrolysis during 14 weeks before measurements was the major factor that affects the result distribution. This method was submitted to the AOCS to become an official AOCS method for krill oil analysis.

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Section: Resultsmentioning

confidence: 99%

³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

Zailer¹,

Monakhova

Diehl³

2018

J Americ Oil Chem Soc

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“…The cultivars were initially recorded for each tree as assessed by each producer, and successively genetically confirmed for all samples by extraction of genomic DNA from leaves and detection of specific microsatellite markers, according to a standardized procedure (Salimonti et al, 2013). Each olive oil sample was produced from the drupes of a single tree (Piccinonna et al, 2016). Olive harvest were performed from each marked tree (with identification code) at optimal olive ripening stage in different periods, depending on cultivar and growing conditions (dry or well-watered field).…”

Section: Methodsmentioning

confidence: 99%

Harvest year effects on Apulian EVOOs evaluated by¹H NMR based metabolomics

Girelli

Coco

Papadia

et al. 2016

PeerJ

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Nine hundred extra virgin olive oils (EVOO) were extracted from individual olive trees of four olive cultivars (Coratina, Cima di Mola, Ogliarola, Peranzana), originating from the provinces of Bari and Foggia (Apulia region, Southern Italy) and collected during two consecutive harvesting seasons (2013/14 and 2014/15). Following genetic identification of individual olive trees, a detailed Apulian EVOO NMR database was built using 900 oils samples obtained from 900 cultivar certified single trees. A study on the olive oil lipid profile was carried out by statistical multivariate analysis (Principal Component Analysis, PCA, Partial Least-Squares Discriminant Analysis, PLS-DA, Orthogonal Partial Least-Squares Discriminant Analysis, OPLS-DA). Influence of cultivar and weather conditions, such as the summer rainfall, on the oil metabolic profile have been evaluated. Mahalanobis distances and J2 criterion have been measured to assess the quality of resulting scores clusters for each cultivar in the two harvesting campaigns. The four studied cultivars showed non homogeneous behavior. Notwithstanding the geographical spread and the wide number of samples, Coratina showed a consistent behavior of its metabolic profile in the two considered harvests. Among the other three Peranzana showed the second more consistent behavior, while Cima di Mola and Ogliarola having the biggest change over the two years.

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“…Moreover, the need of a scientific tool to assess EVOOs geographical origin represents a hot topic issue since the European Regulation 182 of 6 March 2009-which declared the compulsory labeling of EVOOs with the geographical origin of the olives in all European countries [18]-still lacks an official validation methodology. We are currently involved in several NMR based metabolomics and chemometric studies to assess cultivar composition and geographical areas origin of extra virgin olive oils [19][20][21][22][23][24][25]. In this work we focused on a methodological 1 H-NMR spectroscopy coupled with a chemometrics approach in order to provide a quantitative blend composition assessment.…”

Section: Introductionmentioning

confidence: 99%

Tunisian Extra Virgin Olive Oil Traceability in the EEC Market: Tunisian/Italian (Coratina) EVOOs Blend as a Case Study

2017

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Abstract:In order to check the reliability of an NMR-based metabolomic approach to evaluating blend composition (and declaration), a series of 81 Italian/Tunisian blends samples at different percentage composition (from 10/90 to 90/10% Coratina/Tunisian oil by 10% increase step) were prepared starting from five Coratina (Apulia) and five Tunisian extra virgin olive oil (EVOO) batches. Moreover, a series of nine binary mixtures blend oils were obtained, starting from the two batches' oil sums. The models built showed the linear relationship between the NMR signals and the percentage composition of the blends. In particular, a high correlation with the percentage composition of blends was obtained from the partial least squares (PLS) regression model, when the two batches oil sums were used for the binary mixtures of blend samples. These proposed methods suggest that a multivariate analysis (MVA)-based NMR approach-in particular PLS regression (PLSR)-could be a very useful tool (including for trading purposes) to assess quantitative blend composition. This is important for the sustainability of the goods' free movement, especially in the agrifood sector. This cornerstone policy of current common markets is also clearly linked to the availability of methods for certifying the origin of the foodstuffs and their use in the assembly of final product for the consumer.Keywords: extra virgin olive oil; commercial purpose; 1 H-NMR spectroscopy; EVOOs origin assessment; multivariate statistical analysis; PLSR; projections to latent structure by means of partial least squares regression

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Robustness of NMR-based metabolomics to generate comparable data sets for olive oil cultivar classification. An inter-laboratory study on Apulian olive oils

Cited by 38 publications

References 18 publications

³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

Harvest year effects on Apulian EVOOs evaluated by¹H NMR based metabolomics

Tunisian Extra Virgin Olive Oil Traceability in the EEC Market: Tunisian/Italian (Coratina) EVOOs Blend as a Case Study

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Robustness of NMR-based metabolomics to generate comparable data sets for olive oil cultivar classification. An inter-laboratory study on Apulian olive oils

Cited by 38 publications

References 18 publications

31P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

31P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

Harvest year effects on Apulian EVOOs evaluated by1H NMR based metabolomics

Tunisian Extra Virgin Olive Oil Traceability in the EEC Market: Tunisian/Italian (Coratina) EVOOs Blend as a Case Study

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³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

³¹P NMR Method for Phospholipid Analysis in Krill Oil: Proficiency Testing—A Step toward Becoming an Official Method

Harvest year effects on Apulian EVOOs evaluated by¹H NMR based metabolomics