Implementing Dynamic Headspace With SPME Sampling of Virgin Olive Oil Volatiles: Optimization, Quality Analytical Study, and Performance Testing.

Competition and interaction phenomena among volatiles during their adsorption process by solid phase microextraction (SPME) fibers in static headspace sampling procedure (SHS) cast doubt on its ability to quantify virgin olive oil volatiles. SPME fibers being excellent traps, their use was analyzed with a new device allowing the concentration of volatiles in a dynamic headspace sampling procedure (DHS). A central composite experimental design optimized the main variables of the device (4 g sample weight, 40 °C temperature, 150 mL/min flow rate, 50 min adsorption time), while values of the analytical quality control parameters of the method (repeatability, limits of detection and quantification, working range, sensitivity, and resolution) were compared with those ones from static headspace. DHS shows better precision results for aldehydes and alcohols than SHS and allowed analyzing higher concentrations with no problem of saturation. In 19 of 28 compounds analyzed in 50 samples the chromatographic areas were higher when running DHS. The concentration values of volatile compounds in these samples after applying SHS and DHS are discussed together with the ability of the new method for distinguishing virgin olive oil by their categories (extra virgin, virgin, and lampante) by the volatiles quantified in commercial oils.

Soft-deodorization of virgin olive oil: Study of the changes of quality and chemical composition.

The potential adulteration of extra virgin olive oil (EVOO) with soft-deodorized virgin olive oil (VOO) has raised the interest of researchers in investigating this fraud in recent years. The objective of this study was to determine chemical changes occurring after a soft-deodorization process in terms of volatiles, fatty acid ethyl esters (FAEEs) and pyropheophytins (PPPs) concentrations in VOOs. After testing several conditions (80, 100 and 130°C, for 30 and 60min), the parameters of 100°C and 60min were considered as the optima. These conditions allowed removing volatiles responsible for sensory defects with low losses of total phenols (14%-32%), and values of PPPs (11.83%) and FAEEs (34.53mg/kg) lower than the limits of standard regulations. The experiments show that soft-deodorized VOOs could be added up to 50% to EVOOs and current standard methods would not detect this kind of adulteration.

Characterization of Virgin Olive Oils with Two Kinds of 'Frostbitten Olives' Sensory Defect.

The frost of olives on the tree due to drops of temperature can produce sensory defects in virgin olive oil (VOO). Temperature changes can be abrupt with freeze-thaw cycles or gradual, and they produce sensory and chemical variations in the oil. This study has analyzed the quality parameters (free fatty acids, peroxide value, UV absorption, and fatty acid ethyl esters) and phenols of VOOs described with the 'frostbitten olives' sensory defect. The phenol profiles allowed grouping these VOOs into two types. One of them, characterized with "soapy" and "strawberry-like" aroma descriptors, had higher values of 1-acetoxypinoresinol, pinoresinol, and aldehydic form of the ligstroside aglycon. The other one, characterized with "wood" and "humidity" descriptors, had higher concentrations of luteolin and apigenin. Most VOOs (75%) from the first group, associated with abrupt drops of temperature, have concentration of phenols higher than the value established by the health claim on olive oil polyphenols approved by the European Commission.

Analysis of Volatile Markers for Virgin Olive Oil Aroma Defects by SPME-GC/FID: Possible Sources of Incorrect Data.

The need to explain virgin olive oil (VOO) aroma descriptors by means of volatiles has raised interest in applying analytical techniques for trapping and quantitating volatiles. Static headspace sampling with solid phase microextraction (SPME) as trapping material is one of the most applied solutions for analyzing volatiles. The use of an internal standard and the determination of the response factors of the main volatiles seem to guarantee the correct determination of volatile concentrations in VOOs by SPME-GC/FID. This paper, however, shows that the competition phenomena between volatiles in their adsorption to the SPME fiber, inherent in static headspace sampling, may affect the quantitation. These phenomena are more noticeable in the particular case of highly odorant matrices, such as rancid and vinegary VOOs with high intensity of defect. The competition phenomena can modify the measurement sensitivity, which can be observed in volatile quantitation as well as in the recording of internal standard areas in different matrices. This paper analyzes the bias of the peak areas and concentrations of those volatiles that are markers for each sensory defect of VOOs (rancid, vinegary, musty, and fusty) when the intensity and complexity of aroma are increased. Of the 17 volatile markers studied in this work, 10 presented some anomalies in the quantitation in highly odorant matrices due the competition phenomena. However, quantitation was not affected in the concentration ranges at which each volatile marker is typically found in the defective oils they were characteristic of, validating their use as markers.