Quantitative Ester Analysis in Cachaça and Distilled Spirits by Gas Chromatography−Mass Spectrometry (GC−MS)

Abstract

An analytical procedure for the separation and quantification of ethyl acetate, ethyl butyrate, ethyl hexanoate, ethyl lactate, ethyl octanoate, ethyl nonanoate, ethyl decanoate, isoamyl octanoate, and ethyl laurate in cachaca, rum, and whisky by direct injection gas chromatography-mass spectrometry was developed. The analytical method is simple, selective, and appropriated for the determination of esters in distilled spirits. The limit of detection ranged from 29 (ethyl hexanoate) to 530 (ethyl acetate) microg L(-1), whereas the standard deviation for repeatability was between 0.774% (ethyl hexanoate) and 5.05% (isoamyl octanoate). Relative standard deviation values for accuracy vary from 90.3 to 98.5% for ethyl butyrate and ethyl acetate, respectively. Ethyl acetate was shown to be the major ester in cachaca (median content of 22.6 mg 100 mL(-1) anhydrous alcohol), followed by ethyl lactate (median content of 8.32 mg 100 mL(-1) anhydrous alcohol). Cachaca produced in copper and hybrid alembic present a higher content of ethyl acetate and ethyl lactate than those produced in a stainless-steel column, whereas cachaca produced by distillation in a stainless-steel column present a higher content of ethyl octanoate, ethyl decanoate, and ethyl laurate. As expected, ethyl acetate is the major ester in whiskey and rum, followed by ethyl lactate for samples of rum. Nevertheless, whiskey samples exhibit ethyl lactate at contents lower or at the same order of magnitude of the fatty esters.

Quantitative chemical profile and multivariate statistical analysis of alembic distilled sugarcane spirit fractions

“…The ethyl acetate and ethyl lactate are the major ester compounds present in cachaças according to Nascimento et al 19 All esters, other than ethyl lactate, were found in higher concentrations in the head fraction rather than in the other fractions. Ethyl lactate, the most soluble in water among the esters evaluated, was predominant in the heart and tail fraction.…”

Comparação de técnicas de determinação de ésteres em cachaça

“…Nas amostras de uísque este éster está presente em concentrações inferiores a 3 mg 100 mL -1 álcool anidro. 11 A baixa concentração de lactato de etila nas amostras de uísque é um indicativo da ausência de Lactobacillus spp durante o processo de fermentação ou um melhor controle do pH e da temperatura no processo fermentativo. A produção de uísque corriqueiramente emprega leveduras selecionadas e um estrito controle da contaminação microbiológica do pé de cuba e da temperatura.…”

“…Cromatografia gasosa acoplada ao detector de espectrometria de massas (CG/EM-MSI) 11 As análises foram realizadas em um cromatógrafo (Shimadzu GC-17A), equipado com um detector de espectrometria de massas (Shimadzu QP5050A) operando no modo de impacto eletrônico (70 eV), monitoramento seletivo de íons (MSI) e injeção direta da amostra no modo split.…”

“…[4][5][6][7] Os ésteres, presentes nas bebidas destiladas, são provenientes de duas fontes distintas: os ésteres alifáticos, tais como acetato de etila e butanoato de etila, originam-se durante a fermentação alcoólica através do metabolismo secundário intracelular das leveduras; 8 os ésteres gerados através da interconversão dos compostos fenólicos, tais como siringato de etila e o vanilato de etila, e os ésteres extraí-dos da madeira (homovanilato de metila e siringato de metila), são consequência do processo de envelhecimento. 9,10 Em trabalho anterior 11 foi relatada pela primeira vez a presença do éster lactato de etila em aguardente, ressaltando-se o fato de este ser o segundo éster mais abundante na cachaça. A presença de lactato de etila na cachaça está relacionada com a contaminação do mosto por bactérias (Lactobacillus spp.)…”

Influence of Harvest Season and Maturation of Different Sugarcane (Saccharum Spp.) Cultivars on the Chemical Composition of Alembic Brazilian Sugarcane Spirit

“…Nascimento et al [10] described a qualitative and quantitative high-performance liquid chromatographic analysis of aldehydes in cachaça and in other distilled alcoholic beverages. Nascimento et al [11] determined esters in cachaça and other distilled spirits by gas chromatography-mass spectrometry (GC-MS). More recently, Souza et al [12] applied a comprehensive two-dimensional gas chromatography for the determination of volatile compounds in cachaça.…”