TY - JOUR T1 - Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers. AU - Moreira,Nathalie, AU - Meireles,Sónia, AU - Brandão,Tiago, AU - de Pinho,Paula Guedes, Y1 - 2013/10/01/ PY - 2013/05/28/received PY - 2013/09/11/revised PY - 2013/09/18/accepted PY - 2013/11/12/entrez PY - 2013/11/12/pubmed PY - 2014/6/16/medline KW - Beer KW - Central composite design (CCD) KW - Gas chromatography–ion trap/mass spectrometry (GC–IT/MS) KW - Headspace solid-phase microextraction (HS-SPME) KW - PFBHA KW - Volatile carbonyl compounds SP - 523 EP - 31 JF - Talanta JO - Talanta VL - 117 N2 - 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. SN - 1873-3573 UR - https://www.unboundmedicine.com/medline/citation/24209376/Optimization_of_the_HS_SPME_GC_IT/MS_method_using_a_central_composite_design_for_volatile_carbonyl_compounds_determination_in_beers_ DB - PRIME DP - Unbound Medicine ER -