Solventless Microextration Techniques for Pharmaceutical Analysis: The Greener Solution

Extensive efforts have been made in the last decades to simplify the holistic sample preparation process. The idea of maximizing the extraction efficiency along with the reduction of extraction time, minimization/elimination of hazardous solvents, and miniaturization of the extraction device, eliminating sample pre- and posttreatment steps and reducing the sample volume requirement is always the goal for an analyst as it ensures the method’s congruency with the green analytical chemistry (GAC) principles and steps toward sustainability. In this context, the microextraction techniques such as solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), microextraction by packed sorbent (MEPS), fabric phase sorptive extraction (FPSE), in-tube extraction dynamic headspace (ITEX-DHS), and PAL SPME Arrow are being very active areas of research. To help transition into wider applications, the new solventless microextraction techniques have to be commercialized, automated, and validated, and their operating principles to be anchored to theory. In this work, the benefits and drawbacks of the advanced microextraction techniques will be discussed and compared, together with their applicability to the analysis of pharmaceuticals in different matrices.

Analyzing the minor volatilome of Torulaspora delbrueckii in an alcoholic fermentation

Torulaspora delbrueckii is an emerging yeast species in the beverage and food industry that is suitable for alcoholic fermentation and to improve the organoleptic quality of wine, beer, mead, and other beverages. Modern consumer preference toward new flavors and products drives the application of T. delbrueckii to ferment less traditional fruits and vegetables. Thus, it has become increasingly relevant to define those metabolites produced in minute quantities by T. delbrueckii, because they may have an impact when producing these new alcoholic beverages. In this study, we have identified metabolites of T. delbrueckii and have compared them with those of Saccharomyces cerevisiae in a controlled setting with a synthetic, high glucose medium using gas chromatography coupled to flame ionization detector (GC–FID) and stir bar sorptive extraction (SBSE) with GC coupled to mass spectrometry (MS). Results showed that T. delbrueckii produced metabolites with higher changes in odor activity complexes than S. cerevisiae: ethyl propanoate, 1,1-diethoxyethane, ethyl isobutyrate, ethyl butyrate, isoamyl acetate, ethyl heptanoate, nonanal, and decanal. We also report seven metabolites detected for the first time in T. delbrueckii. This datum serves to expand the knowledge of T. delbrueckii performance and shows that application of this yeast species is more suitable to a wide array of beverage producers.

Smoked-Derived Volatile Phenol Analysis in Wine by Stir Bar Sorptive Extraction-Gas Chromatography-Mass Spectrometry

Smoke-derived taint has become a significant concern for the U.S. wine industry, particularly on the west coast, and climate change is anticipated to aggravate it. High volatile phenols such as guaiacol, 4-methylguaiacol, 4-ethylguaiacol, 4-ethylphenol, and o-, p-, m-cresols have been suggested to be related to smoke-exposed grape and wine. This paper describes an analytical approach based on ethylene glycol/polydimethylsiloxane (EG/PDMS)-stir bar sorptive extraction-gas chromatography-mass spectrometry (SBSE-GC-MS) to quantify or estimate the concentrations of some smoke-related volatile phenols in wines. Correlation coefficients with R2 ≥ 0.990 were obtained. This method can quantify most smoked-related volatile phenols down to 0.5 μg/L in wine in selective ion monitoring mode. Recovery for the targeted volatile phenols ranged from 72.2% to 142.4% in the smoke-tainted wine matrix, except for 4-vinylguaiacol. The standard deviations of the volatile phenols were from 0 to 23% in smoke-tainted wine. The approach provides another tool to evaluate wine smoke exposure and potential smoke taint.