scholarly journals Highly Informative Fingerprinting of Extra-Virgin Olive Oil Volatiles: The Role of High Concentration-Capacity Sampling in Combination with Comprehensive Two-Dimensional Gas Chromatography

Separations ◽  
2019 ◽  
Vol 6 (3) ◽  
pp. 34 ◽  
Author(s):  
Federico Stilo ◽  
Chiara Cordero ◽  
Barbara Sgorbini ◽  
Carlo Bicchi ◽  
Erica Liberto

The study explores the complex volatile fraction of extra-virgin olive oil by combining high concentration-capacity headspace approaches with comprehensive two-dimensional gas chromatography, which is coupled with time of flight mass spectrometry. The static headspace techniques in this study are: (a) Solid-phase microextraction, with multi-polymer coating (SPME- Divinylbenzene/Carboxen/Polydimethylsiloxane), which is taken as the reference technique; (b) headspace sorptive extraction (HSSE) with either a single-material coating (polydimethylsiloxane—PDMS) or a dual-phase coating that combines PDMS/Carbopack and PDMS/EG (ethyleneglycol); (c) monolithic material sorptive extraction (MMSE), using octa-decyl silica combined with graphite carbon (ODS/CB); and dynamic headspace (d) with either PDMS foam, operating in partition mode, or Tenax TA™, operating in adsorption mode. The coverage of both targeted and untargeted 2D-peak-region features, which corresponds to detectable analytes, was examined, while concentration factors (CF) for a selection of informative analytes, including key-odorants and off-odors, and homolog-series relative ratios were calculated and the information capacity was discussed. The results highlighted the differences in concentration capacities, which were mainly caused by polymer-accumulation characteristics (sorptive/adsorptive materials) and its amount. The relative concentration capacity for homologues and potent odorants was also discussed, while headspace linearity and the relative distribution of analytes, as a function of different sampling amounts, was examined. This last point is of particular interest in quantitative studies where accurate data is needed to derive consistent conclusions.






Molecules ◽  
2019 ◽  
Vol 24 (13) ◽  
pp. 2379 ◽  
Author(s):  
Lorenzo Cecchi ◽  
Maria Bellumori ◽  
Filomena Corbo ◽  
Gualtiero Milani ◽  
Maria Lisa Clodoveo ◽  
...  

The use of innovative systems, such as the heat exchanger, for production of extra virgin olive oil should allow maintenance of the same quality of those oils derived from traditional processes, and presents specific advantages. The performance of this system was evaluated by (i) determining the parameters directly measurable by the olive millers (i.e., end-user validation based on the production yields when the plant is located in different processing lines) and (ii) assessing the product quality through estimation of the content of phenolic and volatile compounds. The phenols were determined by High Performance Liquid Chromatography with Diode Array Detector (HPLC–DAD) before and after acidic hydrolysis while the volatile fraction was studied by Head-Space Solid-Phase-Micro-Extraction Gas-Chromatography with Mass Detector (HS–SPME–GC–MS). The use of the sono-heat-exchanger presents several advantages: it is a flexible machine, able to interface with all devices of the world’s leading manufacturers of the Extra Virgin Olive Oil (EVOO) extraction plant, and it guarantees shorter processing times and energy savings. Our results also pointed out its capability to increase the oil yields up to 5.5%, particularly when it extracts oil from unripe fruits, which in traditional processes yield oils with higher phenolic contents, but with lower oil yields. Overall, the quality of virgin olive oils was maintained, avoiding decreases of phenolic content or detrimental effects on the sensory characteristics.



Author(s):  
Federico Stilo ◽  
Erica Liberto ◽  
Stephen E Reichenbach ◽  
Qingping Tao ◽  
Carlo Bicchi ◽  
...  

Abstract Background Comprehensive two-dimensional gas chromatography combined with time-of-flight mass spectrometry (GC×GC-TOF MS) is the most informative analytical approach for chemical characterization of the complex food volatilome. Key analytical features include: separation power and resolution enhancement; improved sensitivity; and structured separation patterns from chemically correlated analytes. Objective In this study, we explore the complex extra-virgin olive oil volatilome by combining head-space (HS) solid-phase microextraction, applied under HS linearity conditions to GC×GC-TOF MS featuring hard and soft ionization in tandem. Methods Multiple analytical dimensions are combined in a single run and evaluated in terms of: chemical dimensionality; method absolute and relative sensitivity; identification reliability provided by spectral signatures acquired at 70 and 12 eV; and dynamic and linear range of response provided by soft ionization. Results Method effectiveness is validated on a sample set of oils from Picual olives at different ripening stages. Ripening markers (3,4-diethyl-1,5-hexadiene (RS/SR), 3,4-diethyl-1,5-hexadiene (meso), (5Z)-3-ethyl-1,5-octadiene, (5E)-3-ethyl-1,5-octadiene, (E,Z)-3,7-decadiene and (E,E)-3,7-decadiene, (Z)-2-hexenal, (Z)-3-hexenal and (Z)-3-hexenal, (E)-2-pentenal, (Z)-2-pentenal, 1-pentanol, 1-penten-3-ol, 3-pentanone, and 1-penten-3-one) and quality indexes ((Z)-3-Hexenal/Nonanal, (Z)-3-Hexenal/Octane, (E)-2-Pentenal/Nonanal, and (E)-2-Pentenal/Octane) are confirmed for their validity in HS linearity conditions. Conclusions : For the complex olive oil volatilome, the proposed approach offers concrete advantages for the validation of the informative role of existing analytes while suggesting new potential markers to be studied in larger sample sets. Highlights The accurate fingerprinting of volatiles by HS-SPME operating in HS linearity conditions followed by GC×GC-TOF MS featuring tandem ionization gives the opportunity to improve the quality of analytical data and reliability of results.



Antioxidants ◽  
2021 ◽  
Vol 10 (3) ◽  
pp. 368
Author(s):  
Paula Garcia-Oliveira ◽  
Cecilia Jimenez-Lopez ◽  
Catarina Lourenço-Lopes ◽  
Franklin Chamorro ◽  
Antia Gonzalez Pereira ◽  
...  

Extra virgin olive oil (EVOO) is one of the most distinctive ingredients of the Mediterranean diet. There are many properties related to this golden ingredient, from supreme organoleptic characteristics to benefits for human health. EVOO contains in its composition molecules capable of exerting bioactivities such as cardio protection, antioxidant, anti-inflammatory, antidiabetic, and anticancer activity, among others, mainly caused by unsaturated fatty acids and certain minor compounds such as tocopherols or phenolic compounds. EVOO is considered the highest quality vegetable oil, which also implies a high sensory quality. The organoleptic properties related to the flavor of this valued product are also due to the presence of a series of compounds in its composition, mainly some carbonyl compounds found in the volatile fraction, although some minor compounds such as phenolic compounds also contribute. However, these properties are greatly affected by the incidence of certain factors, both intrinsic, such as the olive variety, and extrinsic, such as the growing conditions, so that each EVOO has a particular flavor. Furthermore, these flavors are susceptible to change under the influence of other factors throughout the oil's shelf-life, such as oxidation or temperature. This work offers a description of some of the most remarkable compounds responsible for EVOO’s unique flavor and aroma, the factors affecting them, the mechanism that lead to the degradation of EVOO, and how flavors can be altered during the shelf-life of the oil, as well as several strategies suggested for the preservation of this flavor, on which the quality of the product also depends.



Foods ◽  
2020 ◽  
Vol 9 (7) ◽  
pp. 862 ◽  
Author(s):  
Sara Barbieri ◽  
Chiara Cevoli ◽  
Alessandra Bendini ◽  
Beatriz Quintanilla-Casas ◽  
Diego Luis García-González ◽  
...  

This research aims to develop a classification model based on untargeted elaboration of volatile fraction fingerprints of virgin olive oils (n = 331) analyzed by flash gas chromatography to predict the commercial category of samples (extra virgin olive oil, EVOO; virgin olive oil, VOO; lampante olive oil, LOO). The raw data related to volatile profiles were considered as independent variables, while the quality grades provided by sensory assessment were defined as a reference parameter. This data matrix was elaborated using the linear technique partial least squares-discriminant analysis (PLS-DA), applying, in sequence, two sequential classification models with two categories (EVOO vs. no-EVOO followed by VOO vs. LOO and LOO vs. no-LOO followed by VOO vs. EVOO). The results from this large set of samples provide satisfactory percentages of correctly classified samples, ranging from 72% to 85%, in external validation. This confirms the reliability of this approach in rapid screening of quality grades and that it represents a valid solution for supporting sensory panels, increasing the efficiency of the controls, and also applicable to the industrial sector.





2014 ◽  
Vol 1334 ◽  
pp. 101-111 ◽  
Author(s):  
Giorgia Purcaro ◽  
Chiara Cordero ◽  
Erica Liberto ◽  
Carlo Bicchi ◽  
Lanfranco S. Conte


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