Over the last few years, the development of micro-distilleries producing diverse spirits with various flavors has been observed. Versatile analytical techniques for the characterization of aroma compounds in such alcoholic beverages are therefore required. A model mixture embodying a theoretical distilled spirit was made according to the data found in literature to compare usual extraction techniques. When it was applied to the model liquor, the headspace solid phase microextraction (HS-SPME) extraction method was preferred to the liquid-liquid extraction (LLE), solid phase extraction (SPE) and stir bar/headspace sorptive extraction (SBSE/HSSE) methods according to efficiency, cost, and environmental criteria. An optimization study using the model mixture showed that the extraction was optimal with a divinylbenzene/carboxen/poly(dimethylsiloxane) DVB/CAR/PDMS fiber, during 60 min, at 35 °C and with the addition of 10% NaCl. This method was successfully applied to three different commercial liquors and led to the identification of 188 flavor compounds, including alcohols, esters, lactones, carbonyls, acetals, fatty acids, phenols, furans, aromatics, terpenoids, alkenes, and alkanes.
Plastic additives are introduced in plastic material formulations, along with organic polymers, to offer different properties such as stability, plasticity or color. However, plastic additives may migrate from the plastic material to the content (in case of plastic containers) or to the material in contact with the plastic, like human skin. In the case of plastic medical devices, this migration is of particular interest, as plastic additives may be deleterious to health. In the present paper, we examined the interest of combining supercritical fluid extraction (SFE) to supercritical fluid chromatography (SFC) hyphenated to mass spectrometry (MS) in an online system to characterize plastic additives in laboratory gloves, taken as samples of medical devices. A set of target compounds comprising 18 plasticizers, 4 antioxidants and 2 lubricants was defined and their detectability with MS was examined, where it appeared that electrospray ionization (ESI) provided better detectability than atmospheric pressure chemical ionization (APCI). After examining possible stationary phases with the help of Derringer desirability function, an isocratic chromatographic method (CO2:methanol 95:5) was developed on Shim-pack UC Phenyl column. The extraction method was examined with a 3-level full factorial design of experiments to optimize the extraction temperature (40 °C) and pressure (200 bar). The online SFE-SFC-MS method was compared to offline methods where the samples were extracted with liquid solvents at atmospheric pressure or high pressure then analysed with SFC-MS. In all cases, offline methods showed significant contaminants (like the oleamide lubricant) issuing from laboratory plastic materials as nitrogen drying station, syringes and filters, while the online method allowed a complete elimination of laboratory contaminations. Furthermore, the online method saved time, solvents and laboratory consumables. It will also show that transferring a compressible fluid from a loading loop is favourable to high efficiency, as the resulting chromatographic peaks are much thinner than when transferring a liquid. Compared to injecting liquid heptane, the efficiency increase was 3.4-fold, while compared to injecting liquid methanol (a common practice in SFC), the efficiency increase was 13-fold. Finally, the additive composition of different laboratory gloves was compared.
In order to quantify organic impurities in gas produced from renewable sources, thermal desorption coupled with GC-MS or GC×GC-MS is very useful. However, the preparation of the standard tubes appears not to be trivial. For that, different strategies, based on commercial setups, have been developed. The goal of this study was to compare the classical manual deposit of a liquid standard solution with other commercial methods such as gas stream assisted deposit and vaporization followed by adsorption assisted by gas stream. A standard mixture of 48 compounds from different families was used for the comparison of the performances of the three strategies using the accuracy profile methodology. A global validation score was attributed to each strategy as well as a score according to family of compounds and boiling point range, in order to provide a detailed comparison of the techniques. On the set of studied molecules, commercial setups were found to be more efficient than the manual deposit.
The development of renewable and low‐carbon gases for injection into the gas grid obtained by different processes such as anaerobic digestion, pyrogasification, hydrothermal gasification, and methanation, followed by upgrading steps, increases the demand for analysis and characterization in order to fully manage their integration into the gas value chain. If the analysis of the main compounds (methane, carbon dioxide, hydrogen, and carbon monoxide) is well described, the analysis of impurities in renewable gases remains more challenging due to their various natures and quantities.After a brief description of renewable and low‐carbon methane production processes, the review focuses on the methods used for the analysis of the different compounds in renewable gases, from the main ones to impurities at ppbv levels. Gas chromatography (GC), coupled with different detectors, is the preferred technique, enabling the analysis and quantification of siloxanes, terpenes, oxygenates, and sulfur compounds. Recently, comprehensive two‐dimensional GC has been applied to renewable gases, increasing the number of compounds detected. Non‐chromatographic techniques are also reviewed. As sampling is of major importance in the search for reliable analyses, a whole section is devoted to this aspect. Among the available methods, pre‐concentration on adsorbent tubes emerges as the most relevant solution.