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The high potential of exhaled breath for disease diagnosis has been highlighted in numerous studies. However, exhaled breath analysis is suffering from a lack of standardized sampling and analysis procedures, impacting the robustness of inter‐laboratory results, and thus hampering proper external validation. The aim of this work was to verify compliance and validate the performance of two different comprehensive two‐dimensional gas chromatography coupled to mass spectrometry platforms in different laboratories by monitoring probe metabolites in exhaled breath following the Peppermint Initiative guidelines. An initial assessment of the exhaled breath sampling conditions was performed, selecting the most suitable sampling bag material and volume. Then, a single sampling was performed using Tedlar bags, followed by the trapping of the volatile organic compounds into thermal desorption tubes for the subsequent analysis using two different analytical platforms. The thermal desorption tubes were first analyzed by a (cryogenically modulated) comprehensive two‐dimensional gas chromatography system coupled to high‐resolution time‐of‐flight mass spectrometry. The desorption was performed in split mode and the split part was recollected in the same tube and further analyzed by a different (flow modulated) comprehensive two‐dimensional gas chromatography system with a parallel detection, specifically using a quadrupole mass spectrometer and a vacuum ultraviolet detector. Both the comprehensive two‐dimensional gas chromatography platforms enabled the longitudinal tracking of the peppermint oil metabolites in exhaled breath. The increased sensitivity of comprehensive two‐dimensional gas chromatography enabled to successfully monitor over a 6.5 h period a total of 10 target compounds, namely α‐pinene, camphene, β‐pinene, limonene, cymene, eucalyptol, menthofuran, menthone, isomenthone, and neomenthol. [ABSTRACT FROM AUTHOR]

Headspace gas chromatography is frequently used for aroma profiling thanks to its ability to naturally exploit the volatility of aroma compounds, and also to provide chemical information on sample composition. Its main advantages rely on simplicity, no use of solvent, amenability to automation, and the cleanliness of the extract. In the present contribution, the most effective sampling (dynamic extraction), separation (multidimensional gas chromatography), and detection (mass spectrometry) techniques for untargeted analysis are exploited in combination, showing their potential in unraveling aroma profiles in fruit beers. To complete the overall analytical process, a neat workflow for data analysis is discussed and used for the successful characterization and identification of five different beer flavors (berries, cherry, banana, apple, and peach). From the technical viewpoint, the coupling of purge‐and‐trap, comprehensive two‐dimensional gas chromatography, and mass spectrometry makes the global methodology unique, and it is for the first time discussed. A (low‐)flow modulation approach allowed for the full transfer into the second dimension with mass‐spectrometry compatible flow (< 7 mL/min), avoiding the need of splitting before detection and making the overall method sensitive (1.2–5.2‐fold higher signal to noise ratio compared to unmodulated gas chromatography conditions) and selective. [ABSTRACT FROM AUTHOR]

The present research description is focused on the evaluation of a high-speed triple quadrupole mass spectrometer, carried out under moderately fast gas chromatography conditions (analysis time: 17 min). The mass spectrometric system is capable of operation under high-speed GC conditions, in both full-scan (maximum scan speed: 20 000 amu/s) and multiple reaction monitoring modalities. Furthermore, the triple quadrupole system can generate full scan and multiple reaction monitoring data simultaneously, also in a very rapid manner. A fast method was developed for the: (i) qualitative analysis of untargeted Citrus essential oil compounds, and (ii) the quali/quantitative analysis of targeted ones, namely three preservatives ( o-phenylphenol, butylated hydroxytoluene, butylated hydroxy-anisole). The mass spectrometric system generated a more-than-sufficient number of data points/peak for both identification and quantification purposes. The level of sensitivity, reached through the multiple-reaction-monitoring side of the analysis, widely exceeded the requirements of current legislation. Method validation, related to the targeted analysis, was performed considering precision of retention times, peak areas and ion ratios; limits of detection/quantification, and accuracy were also measured. [ABSTRACT FROM AUTHOR]

The present manuscript reports a comparative study between conventional and split-flow comprehensive GC× GC- MS. Conventional GC× GC- MS was performed by using a single GC oven, and with a widely employed apolar (30 m × 0.25 mm id)-polar (1 m × 0.10 mm id) column combination. Split-flow GC× GC- MS experiments were carried out by using the same first and second analytical columns, and by diverting part of the primary-capillary flow to waste, via a waste line. The latter was located at the conjunction point between the two dimensions. The measurement of fundamental gas chromatography parameters (efficiency, resolution), in both dimensions and under different experimental conditions, enabled the attainment of detailed information related to GC× GC- MS method optimization. Finally, the results derived from the present investigation highlight an important GC× GC issue, namely the efficiency of band reinjection onto the second-dimension capillary. [ABSTRACT FROM AUTHOR]

Front Cover: Investigating aroma diversity combining purge-and-trap, comprehensive two-dimensional gas chromatography, and mass spectrometry DOI: 10.1002/jssc.201900902 The cover picture shows the analytical workflow the authors used for the detailed aroma analysis of beers. These were thermally desorbed in a (low-)flow modulated comprehensive two-dimensional gas chromatography system (GC×GC) coupled to time-of-flight mass spectrometry (ToF MS). [Extracted from the article]

Polychlorodibenzo-p-dioxins (PCDDs), polychloro-dibenzofurans (PCDFs), dioxin-like (DL), and non dioxin-like (NDL) polychlorinated biphenyls (PCBs) are currently regulated in food and feed within the European territory (EU 2017/644-771). The confirmatory methods of analysis for checking compliance with maximum levels (MLs) for these involve either the historically-established GC-magnetic sector high-resolution mass spectrometry (GC-HRMS) and, more recently, GC-triple quadrupole mass spectrometry operating in tandem mode (GC-QQQMS/MS). In this study, the performance of a novel triple quadrupole GC-QQQMS/MS system equipped with a programable temperature vaporization (PTV) injector was evaluated for the analysis of regulated PCDD/Fs and PCBs in food and feed. The MS analyzer was equipped with a titanium ionization chamber and a new short collision cell capable to accumulate and eject ions by means of very narrow pulses that allow to minimize the noise and to adapt accumulation times for sensitive multiple reaction monitoring (MRM). The analytical capability of the system was confronted by the strict requirements (selectivity, reproducibility, linearity, quant/qual MRM transitions, accuracy, robustness) set by the EU Regulation for a range of standards, quality control (QC) and food/feed samples. In this respect, the approach showed high precision (1.9–15% relative standard deviation (RSD) at low pg/µL) and accuracy (>80%, except for one hexa-CDD). The quantitative results were also compared to the most used GC-HRMS. In this case, comparable results in terms of single congener concentration basis and total toxic equivalent (TEQ) basis for PCDD/Fs and DL-PCBs were obtained for the QC samples analyzed. [ABSTRACT FROM AUTHOR]

Sampling of volatile organic compounds (VOCs) has shown promise for detection of a range of diseases but results have proved hard to replicate due to a lack of standardization. In this work we introduce the 'Peppermint Initiative'. The initiative seeks to disseminate a standardized experiment that allows comparison of breath sampling and data analysis methods. Further, it seeks to share a set of benchmark values for the measurement of VOCs in breath. Pilot data are presented to illustrate the standardized approach to the interpretation of results obtained from the Peppermint experiment. This pilot study was conducted to determine the washout profile of peppermint compounds in breath, identify appropriate sampling time points, and formalise the data analysis. Five and ten participants were recruited to undertake a standardized intervention by ingesting a peppermint oil capsule that engenders a predictable and controlled change in the VOC profile in exhaled breath. After collecting a pre-ingestion breath sample, five further samples are taken at 2, 4, 6, 8, and 10 h after ingestion. Samples were analysed using ion mobility spectrometry coupled to multi-capillary column and thermal desorption gas chromatography mass spectrometry. A regression analysis of the washout data was used to determine sampling times for the final peppermint protocol, and the time for the compound measurement to return to baseline levels was selected as a benchmark value. A measure of the quality of the data generated from a given technique is proposed by comparing data fidelity. This study protocol has been used for all subsequent measurements by the Peppermint Consortium (16 partners from seven countries). So far 1200 breath samples from 200 participants using a range of sampling and analytical techniques have been collected. The data from the consortium will be disseminated in subsequent technical notes focussing on results from individual platforms.

The influences of various factors, including the symbiosis established with the roots of specific tree species, on the production of volatiles in the fruiting bodies of Tuber magnatum have not been investigated yet. Volatiles in T. magnatum fruiting bodies were quantitatively and qualitatively determined by both PTR-MS and GC-MS in order to compare the accuracy of the two methods. An electronic nose was also used to characterize truffle samples. The influence of environmental changes on the antioxidant capabilities of fruiting bodies was also determined. Statistically significant differences were found between fruiting bodies with different origins. The relationship between the quality of white truffle fruiting bodies and their specific host plant is described along with an analysis of metabolites other than VOCs that have ecological roles. Our results indicate that the geographical origin (Italy and Istria) of the fruiting bodies is correlated with the quantity and quality of volatiles and various antioxidant metabolites. This is the first report characterizing antioxidant compounds other than VOCs in white truffles. The correlation between geographical origin and antioxidant contents suggests that these compounds may be useful for certifying the geographical origin of truffles.