Identification of Trace Volatile Compounds in Freshly Distilled Calvados and Cognac Using Preparative Separations Coupled with Gas Chromatography−Mass Spectrometry

Abstract

Gas chromatography coupled with mass spectrometry (GC-MS) using both electron impact and chemical ionization detection modes led to the determination of the volatile composition of two samples of freshly distilled Cognac and two samples of freshly distilled Calvados. A total of 169 volatile compounds were directly identified in dichloromethane extracts obtained by liquid-liquid extraction. Trace compounds present in both spirits were characterized with the help of preparative separations. In a first step, groups of compounds were separated by preparative GC, and the fractions were analyzed on a polar stationary phase by GC-MS. In a second step, silica gel fractionation was used to separate them by polarity. In this study, 331 compounds, of which 162 can be considered as trace compounds, were characterized in both freshly distilled Cognac and Calvados. Of these, 39 are common to both spirits; 30 are specific to Cognac with numerous hexenyl esters and norisoprenoidic derivatives, whereas 93 are specific to Calvados with compounds such as unsaturated alcohols, phenolic derivatives, and unsaturated aldehydes.

Determination of volatile fatty acid ethyl esters in raw spirits using solid phase microextraction and gas chromatography

“…A number of methods have been developed to analyze volatiles in alcoholic beverages, exploiting such sample preparation techniques as liquid-liquid extraction (LLE) [7][8][9][10][11], liquid-liquid continuous extraction (LLCE) [12][13][14][15], solid phase extraction (SPE) [16][17][18], and steam distillation (SD) [19], and such determination techniques as gas chromatography and electronic noses [20][21][22]. Over the course of recent years, instrumental odor analysis has been dominated by a group of headspace analysis techniques, mainly headspace solid phase microextraction (HS-SPME) [23][24][25][26][27][28][29][30][31][32].…”

Determination of adulterants in adulterant-fruit spirit blends using excitation-emission matrix fluorescence spectroscopy

“…EEM contour map spreads in the excitation wavelength range from 200 nm to 350 nm and the emission wavelength region from 295 nm to 500 nm with the fluorescence maxima at the excitation wavelengths of 250 nm and 300 nm, and the emission wavelengths of 325 nm and 420 nm. Volatile compounds as 2-phenylethanol, guaiacol, 4-vinylanisole, 4-methylguaiacol, methyleugenol, 4-ethylguaiacol, eugenol, 4-ethylphenol, 4-vinylguaiacol identified in apple distillates (Genovese et al, 2004;Ledauphin et al, 2003;Ledauphin et al, 2004) can contribute to the observed fluorescence (Song et al, 2008;Zhan et al, 2008;Sádecká et al, 2015). Many substituted phenols or anisols show similar fluorescence properties, for example eugenol exhibit bands with the respective maxima at l ex = 280 nm and at l em = 320 nm.…”

Olive Oil Composition: Volatile Compounds

“…These results aims to fullfill some part of this gap. Angerosa, 2002;Contini & Esti 2006;Flath et al, 1973;Kanavouras et al, 2005;Ledauphin et al,. 2004;Morales et al, 1994;Morales et al, 1995;Morales et al, 2005;Reiners & Grosch, 1998;Tabanca et al, 2006;Vichi et al, 2003aVichi et al, ., 2003bVichi et al, 2005;Zunin et al, 2004. .…”