Differentiation of Rums Produced from Sugar Cane Juice (Rhum Agricole) from Rums Manufactured from Sugar Cane Molasses by a Metabolomics Approach

Abstract

A large set of volatiles (a metabolome) was isolated by SAFE distillation from 25 high priced rums prepared from sugar cane juice (SCJ) and 26 high priced rums manufactured from sugar cane molasses (SCM). The volatile fractions were first analyzed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF-MS), and the "comprehensive template matching fingerprinting" was used to extract the entire features present in the respective set of volatile compounds. After raw data pretreatment, chemometrics was used to locate marker compounds. Following, a sparse-partial-least-squares discriminant analysis ( sPLS-DA) and a partial-least-squares discriminant analysis (PLS-DA) were applied to a training data set for creating a model. The model was validated using leave-one-out cross validation and tested over an independent data set to evaluate its predictive power. The characteristic fingerprint resulted in a 100% correct classification of sugar cane juice rums, thus achieving the first aim of locating markers for these higher quality rums. Then, past-processing identification within the discriminant features was done to characterize 12 significant marker compounds as 1-decanol, γ-dodecalactone, ethyl 3-methylbutanoate, ethyl nonanoate, 3-furancarboxaldehyde, 1-hexanol, β-ionone, 2- and 3-methylbutanol, methyl decanoate, 3-octanol, and 2-undecanone. Quantitation of eight selected markers by stable isotope dilution assays confirmed higher concentrations in SCJ compared to SCM and served as the final proof to differentiate both types of spirits.

Implementing Dynamic Headspace With SPME Sampling of Virgin Olive Oil Volatiles: Optimization, Quality Analytical Study, and Performance Testing

“…The flow rate of the inert gas (N 2 ) was the first variable to be independently evaluated in duplicate. The experiments, with 5 g of sample and 15 min of exposing SPME fiber to volatiles (adsorption time), were performed with 10 different flow rates of inert gas (12,25,50,100,150,200,250,300,350, and 400 mL/min). Adsorption time (15 min) was selected because it is short enough to allow multiple experiments and it allows enough amount of volatiles trapped in DHS.…”

“…Figure 1 shows two chromatograms in which the volatile compounds identified in this work are indicated with codes. The following compounds (and their codes in the chromatograms) were purchased from Sigma-Aldrich: octane (1), ethyl acetate (2), ethanol (3), ethyl propanoate (4), pentan-3-one (5), pentanal (6), 4methylpentan-2-one (7), 1-penten-3-one (8), butan-2-ol (9), ethyl butanoate (10), 2-methylpropyl butanoate (11), hexanal (12), butan-1-ol (13), 4-methylpentan-2-ol ( 14), heptan-2-one (15), heptanal (16), 3-methylbutan-1-ol ( 17), (2E)-2-hexenal (18), 3-octanone (19), hexyl acetate (20), octanal (21), 1-octen-3-one ( 22), (3Z)-3-hexenyl acetate (23), (2E)-2-heptenal (24), heptan-2-ol (25), 6-methyl-5hepten-2-one (26), hexan-1-ol ( 27), (3Z)-3-hexen-1-ol ( 28), (3E)-3hexen-1-ol (29), nonanal (30), 1-octen-3-ol (31), acetic acid (32), propanoic acid (33), butanoic acid (34), pentanoic acid (35), hexanoic acid (36).…”

“…To compensate this phenomena and reduce their effect on the quantitation, one solution is to use multiple internal standard normalization by selecting the best internal standard for each volatile compound . The quantitation and the procedure of stable isotope dilution − have been also developed to avoid these problems and increase accuracy. However, the use of volatile analysis as a routine method requires a major simplicity in quantitation and an actual improvement in the extraction step.…”

Comprehensive Two-Dimensional Gas Chromatography Advances in Technology and Applications: Biennial Update

“…Another important class of flavored products, beverages require similar quality standards to foods and a similar number of GC×GC studies are noted. Examples of the most common products in this category are tea, − coffee, − wine, ,− spirits, , and beer and hop. ,, …”

An Innovative Metabolomic Approach for Golden Rum Classification Combining Ultrahigh-Performance Liquid Chromatography–Orbitrap Mass Spectrometry and Chemometric Strategies

“…Currently, different methods have been described for the classification of alcoholic beverages on the basis of an analysis of the metabolomic composition, including scarce rum classification studies. , For that purpose, gas chromatography coupled to mass spectrometry (GC-MS) has been one of the most frequently used techniques for analyzing the volatile fraction of the rums.…”