Characterization of Cigar Tobaccos by Gas Chromatographic/Mass Spectrometric Analysis of Nonvolatile Organic Acids:  Application to the Authentication of Cuban Cigars

Abstract

A reliable method based on gas chromatographic/mass spectrometric (GC/MS) profiling of nonvolatile organic acids is described for the characterization of cigars. The method involves an aqueous extraction of ground tobacco and selective isolation of the acids by simply stirring strong anion exchange (SAX) disks in the aqueous tobacco extract. The acids are then directly silylated on the disk with N-methyl-N-trimethylsilyl-trifluroacetamide (MSTFA) in acetonitrile in an autosampler vial. Elution of the derivatized acids in situ allows the sample to be directly analyzed by GC/MS without further sample handling. Compared to the conventional disk-extraction technique using a vacuum manifold, this method is much less labor intensive, and is desirable for multiple sample analysis. Nicotinic acid, succinic acid, glyceric acid, malic acid, pyroglutamic acid, threonic acid, citric acid, uracil, and an unidentified acid were reproducibly quantified in tobacco samples. Principal component analysis (PCA) of the acid profiles of the filler tobaccos of 18 Cuban cigars and 31 non-Cuban cigars shows separation of the two groups, indicating that the acid profiles are potentially useful in the authentication of Cuban cigars.

Simultaneous determination of non‐volatile, semi‐volatile, and volatile organic acids in tobacco by SIM–Scan mode GC–MS

“…An aqueous solution has often been used to extract organic acids in tobacco [9,10,12]. Ng's method [9] included four steps: (i) aqueous extraction of acids from the tobacco sample; (ii) concentration of acids from the aqueous extract by disk extraction; (iii) silylation of acids on the disk and in-situ elution of the derivatives; and (iv) GC -MS analysis.…”

“…Ng's method [9] included four steps: (i) aqueous extraction of acids from the tobacco sample; (ii) concentration of acids from the aqueous extract by disk extraction; (iii) silylation of acids on the disk and in-situ elution of the derivatives; and (iv) GC -MS analysis. Jin et al esterified the polybasic and higher fatty acids in H 2 SO 4 /CH 3 OH at room temperature for 22 h, followed by extraction with CH 2 Cl 2 for 3 min [13].…”

“…Because the concentrations of NVOAs and SVOAs (mg level) were much higher than that of VOAs (lg level) in tobacco and its products, it was difficult to simultaneously determine NVOAs, SVOAs, and VOAs by a general GC -MS method [9]. In the past, full-scan and SIM data of GC -MS were used alternatively in a single run.…”

“…Ng [8] reviewed the analysis of fatty acids and esters in tobacco by full-scan GC -MS, and reported that quantitative data are highly dependent on the mode of sample preparation and the analytical method utilized. Other authors [7 -12] have already reported the determination of organic acids in tobacco leaves and tobacco products, and the analytical approaches adopted were based on HPLC [7], GC -MS [8,9], ion chromatography (IC) [10], capillary isotachophoresis [11], and GC [12] with derivatization steps. Simultaneous determinations of NVOAs, SVOAs, and VOAs were difficult on using general chromatographic methods because of significant concentration differences of NVOAs (mg level), SVOAs (mg level), and VOAs (lg level) in tobacco leaves.…”

Aplicação de métodos quimiométricos na caracterização de charutos utilizando extração por dispersão da matriz em fase sólida e análise por cromatografia gasosa acoplada à espectrometria de massas

“…Os dois primeiros são importantes por conferir aroma e sabor ao tabaco, 7 e o último por ser precursor de compostos carcinogênicos, dando origem a hidrocarbonetos policíclicos aromáticos (HPAs) durante a queima do tabaco. 8 Muitos fatores afetam a qualidade do tabaco, como práticas de cultivo, aspectos ambientais, 9 solo, ano de colheita, variantes genéticas e o processo no qual o tabaco é curado. 10 A discriminação de amostras de produtos de tabaco normalmente é realizada através de análises sensoriais, com base no aspecto visual, sabor e aroma.…”