Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column

Fábio Junior Moreira Novaes, Chadin Kulsing, Humberto Ribeiro Bizzo, Francisco Radler de Aquino Neto, Claudia Moraes Rezende, Philip John Marriott

Research output: Contribution to journalArticle

Abstract

Comprehensive two-dimensional gas chromatography (GC×GC) approaches with cryogenic modulation were developed for the qualitative analysis of selected low volatility compounds in raw coffee bean extracts, without derivatisation. The approaches employed short first (1D) and second (2D) dimension columns, specifically a 1D 65% phenyl methyl siloxane column (11m) and a 2D 5% phenyl methyl siloxane column (1m), which allowed elution of high molar mass compounds (e.g.>600Da). Solutes included hydrocarbons, fatty acids, diterpenes, tocopherols, sterols, diterpene esters, and di- and triacylglycerides. An oven temperature program up to 370°C was employed. The effects of experimental conditions were investigated, revealing that the GC×GC results strongly depended on the cryogenic trap T, and oven T program. An appropriate condition was selected and further applied for group type analysis of low volatility compounds in green Arabica coffee beans. Retention indices were compiled for 1D GC analysis and were similar for the composite column data in GC×GC. The elution of some compounds was confirmed by use of authentic standards. The approach allowed direct analysis of coffee extract in ethyl acetate solution, with improved analyte peak capacity (approximately 200 compounds were detected) without prior fractionation or pre-treatment of the sample. This avoided potential hydrolysis of high molar mass conjugate esters as well as degradation of thermally labile compounds such as the derivatives of the diterpenes cafestol and kahweol.

LanguageEnglish
Pages75–81
Number of pages7
JournalJournal of Chromatography A
Volume1536
DOIs
StatePublished - 2018

Keywords

  • Coffee
  • Comprehensive two-dimensional gas chromatography
  • DAGs
  • High temperature gas chromatography
  • TAGs

Cite this

Novaes, Fábio Junior Moreira ; Kulsing, Chadin ; Bizzo, Humberto Ribeiro ; de Aquino Neto, Francisco Radler ; Rezende, Claudia Moraes ; Marriott, Philip John. / Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column. In: Journal of Chromatography A. 2018 ; Vol. 1536. pp. 75–81
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Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column. / Novaes, Fábio Junior Moreira; Kulsing, Chadin; Bizzo, Humberto Ribeiro; de Aquino Neto, Francisco Radler; Rezende, Claudia Moraes; Marriott, Philip John.

In: Journal of Chromatography A, Vol. 1536, 2018, p. 75–81.

Research output: Contribution to journalArticle

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T1 - Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column

AU - Novaes,Fábio Junior Moreira

AU - Kulsing,Chadin

AU - Bizzo,Humberto Ribeiro

AU - de Aquino Neto,Francisco Radler

AU - Rezende,Claudia Moraes

AU - Marriott,Philip John

PY - 2018

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