Untargeted and Targeted Fingerprinting of Extra Virgin Olive Oil Volatiles by Comprehensive Two-Dimensional Gas Chromatography with Mass Spectrometry: Challenges in Long-Term Studies

2019 ◽  
Vol 67 (18) ◽  
pp. 5289-5302 ◽  
Author(s):  
Federico Stilo ◽  
Erica Liberto ◽  
Stephen E. Reichenbach ◽  
Qingping Tao ◽  
Carlo Bicchi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Olive Oil ◽  
Virgin Olive Oil ◽  
Extra Virgin Olive Oil ◽  
Two Dimensional ◽  
Long Term Studies

Exploring the extra-virgin olive oil volatilome by adding extra dimensions to comprehensive two-dimensional gas chromatography and time of flight mass spectrometry featuring tandem ionization: validation of ripening markers in headspace linearity conditions

2020 ◽  
Author(s):  
Federico Stilo ◽  
Erica Liberto ◽  
Stephen E Reichenbach ◽  
Qingping Tao ◽  
Carlo Bicchi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Olive Oil ◽  
Virgin Olive Oil ◽  
Time Of Flight ◽  
Extra Virgin Olive Oil ◽  
Two Dimensional ◽  
Soft Ionization ◽  
Flight Mass Spectrometry ◽  
Tof Ms

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.

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
Keyword(s):  
Gas Chromatography ◽  
Olive Oil ◽  
Solid Phase ◽  
Virgin Olive Oil ◽  
Extra Virgin Olive Oil ◽  
Volatile Fraction ◽  
Relative Distribution ◽  
Two Dimensional ◽  
High Concentration ◽  
Sorptive Extraction

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.

Comparing diets for weight loss and improvement in biomarkers in men with prostate cancer on surveillance: A pilot study.

2017 ◽  
Vol 35 (5_suppl) ◽  
pp. 159-159 ◽  
Author(s):  
Sharon Benson
Keyword(s):  
Prostate Cancer ◽  
Weight Loss ◽  
Olive Oil ◽  
Virgin Olive Oil ◽  
Dietary Treatment ◽  
Extra Virgin Olive Oil ◽  
Increase Risk ◽  
Diet Compliance ◽  
Similar Weight

159 Background: Weight loss is recommended for treatment of prostate cancer, yet the most efficacious diet is not clear. The diet should improve biomarkers for prostate cancer, not increase risk of other chronic diseases, and be acceptable for long term use. Ascertaining appropriate dietary treatment for men on surveillance is crucial in preventing future cardiovascular disease, which is the leading cause of death in these men. Methods: Men with prostate cancer on surveillance and/or with untreated biochemical relapse followed 2 diets for 8 weeks of weight loss with random assignment to the order: (1) the diet recommended by the Prostate Cancer Foundation (PCF); (2) a plant-based, olive oil diet (PBOO), which included 3 tablespoons of extra virgin olive oil/ daily. After completing both diets, participants selected one of the diets for 6 months of follow-up (FU). Results: 30 started the protocol; 12 dropped out, 11 due to diet compliance (n = 3 PBOO; n = 8 PCF); 18 completed the 8 weeks of both diets and are reported here. Mean age: 66.6 + 5.9; baseline BMI: 30.9 + 2.7 kg/m2. Thirteen of the 18 have chosen the PBOO for FU. Conclusions: These results suggest a benefit with the PBOO diet in lowering insulin and glucose, and improving insulin function compared to the PCF diet. Despite similar weight loss, energy intake was higher on the PBOO diet. In addition, the PBOO diet was preferred over the PCF diet for long-term use. [Table: see text]

Sign in / Sign up

Export Citation Format

Share Document