Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers

Nathalie Moreira, Sónia Meireles, Tiago Brandão, Paula Guedes de Pinho*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

53 Citations (Scopus)


An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography and ion trap mass spectrometry detection (GC-IT/MS) was developed in order to quantify a large number of carbonyl compounds in beers. Carbonyl compounds were previously derivatized with O-(2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). Volatile carbonyl compounds associated with staling beer aroma includes alkanals, alkenals, alkadienals, dicarbonyl compounds, Strecker aldehydes, ketones and furans. The HS-SPME was performed using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber. The procedures were optimized for HS-SPME pre-incubation temperature and time, extraction temperature and time, and PFBHA addition. A central composite design was used in the optimization of extraction conditions and PFBHA addition. The volatile compounds showed optimal extraction incubating 5 ml of beer with 700 mg l-1 of PFBHA for 7 min and extracted for more 20 min at 45 C. The method was validated with regard to the linearity, repeatability, inter and intra-day precision and accuracy. The method achieved detection limits ranging from 0.003 to 0.510 μg l-1, except for furans (1.54-3.44 μg l-1). The quantification limits varied from 0.010 to 1.55 μg l-1, except for 2-furfural (4.68 μg l-1), 5-methyl-2-furfural (5.82 μg l-1) and 5-hyfroxymethylfurfural (10.4 μg l-1). Repeatability values of all compounds were lower than 17%. The method accuracy was satisfactory with recoveries ranging from 88% to 114%. The validated method showed to be suitable for a fast and reliable determination of main carbonyl compounds in beers.
Original languageEnglish
Pages (from-to)523-531
Number of pages9
Publication statusPublished - 2013


  • Beer
  • Central composite design (CCD)
  • Gas chromatography-ion trap/mass spectrometry (GC-IT/MS)
  • Headspace solid-phase microextraction (HS-SPME)
  • Volatile carbonyl compounds


Dive into the research topics of 'Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers'. Together they form a unique fingerprint.

Cite this