Development of a Fully Automated Method HS-SPME-GC-MS/MS for the Determination of Odor-Active Carbonyls in Wines: a “Green” Approach to Improve Robustness and Productivity in the Oenological Analytical Chemistry

Abstract

The aim of this study was the optimization and validation of a green, robust, and comprehensive method for the determination of volatile carbonyl compounds (VCCs) in wines that could be added as a new quality control tool for the evaluation of a complete fermentation, correct winemaking style, and proper bottling and storage. A HS-SPME-GC-MS/MS method was optimized and automated using the autosampler to improve overall performance. A solvent-less technique and a strong minimization of all volumes were implemented to comply with the green analytical chemistry principles. There were as many as 44 VCC (mainly linear aldehydes, Strecker aldehydes, unsaturated aldehydes, ketones, and many other) analytes under investigation. All compounds showed a good linearity, and the LOQs were abundantly under the relevant perception thresholds. Intraday, 5-day interday repeatability, and recovery performances in a spiked real sample were evaluated showing satisfactory results. The method was applied to determine the evolution of VCCs in white and red wines after accelerated aging for 5 weeks at 50 °C. Furans and linear and Strecker aldehydes were the compounds that showed the most important variation; many VCCs increased in both classes of samples, whereas some showed different behaviors between white and red cultivars. The obtained results are in strong accordance with the latest models on carbonyl evolution related to wine aging.

Volatilomics of Fruit Wines

“…Equipping the laboratory with an automatic SPME fibre extraction system coupled to a chromatograph (e.g., Gerstel) enables the significant acceleration of analyses and eliminates human error during determinations [ 162 ]. In order to enhance extraction efficiency, the addition of NaCl to the samples is a common practice [ 151 , 160 , 163 , 164 ]. In addition, internal standards are introduced into the vials prior to extraction.…”

“…In addition, internal standards are introduced into the vials prior to extraction. Depending on the wine under investigation, the authors used a variety of standards, such as 3-acetate [ 161 ], 2-acetate [ 156 ], 4-methyl-2-pentanol [ 157 ], acetone d6, 4-methyl-3-penten-2-one d10, acetanal d16, 4-fluorobenzaldehyde [ 163 ], and cyclohexanone [ 151 ].…”

“…The triple-quadrupole mass spectrometer (QqQ-MS) is a widely recognised detector in the scientific community. The instrument enables the separation, identification, and quantification of volatile components in wines, even at concentrations below 1 ppm [ 140 , 163 ]. The utilisation of high-resolution mass spectrometry with quadrupole time-of-flight measurement (Q-TOF-MS) enables the attainment of an enhanced resolution and sensitivity in chromatographic measurements [ 154 , 156 ].…”

Application of Comprehensive 2D Gas Chromatography Coupled with Mass Spectrometry in Beer and Wine VOC Analysis

“…This well-known phenomenon, which impacts the overall extraction efficiency, especially for polar phases, leads to decreased signal for semi-volatile analytes due to the faster adsorption of ethanol on the fiber surface [86]. The use of a thin hydrophobic polydimethylsiloxane (PDMS) layer on commercial polar fiber materials is an effective strategy to balance the displacement effect of ethanol in the determination of VOC in fermented beverages [87].…”

Decoding the Volatile Profile of White Romanian Fetească Wines

“…This technique allows for the analysis of the volatile profile of wines, providing information on the composition and characteristics of the integrated aroma compounds [7]. It has been used to analyze the volatile compounds in different wine varieties and regions, highlighting the sensory attributes and volatiles that contribute to the diversity of wines [8]. Overall, the HS-SPME/GC-MS assay is a valuable analytical technique for the detection and identification of specific wine components, allowing for a better understanding of the aroma profile and sensory attributes of wines.…”