PMID- 33887808 OWN - NLM STAT- Publisher LR - 20240222 IS - 1096-9888 (Electronic) IS - 1076-5174 (Linking) VI - 56 IP - 5 DP - 2021 Apr 3 TI - Development and optimization of a quantitative analysis of main odorants causing off flavours in cork stoppers using headspace solid-phase microextraction gas chromatography tandem mass spectrometry. PG - e4728 LID - 10.1002/jms.4728 [doi] AB - A simple and sensitive method was developed and validated to simultaneously separate and determine the 2-Methoxy-3,5-dimethylpyrazine, 2-Isopropyl-3-methoxypyrazine, guaiacol, 2-Isobutyl-3-methoxypyrazine, 2-Methylisoborneol, geosmin, 2,4,6-Trichloroanisole, 2,3,4,6-Tetrachloroanisole, 2,4,6-Tribromoanisole and Pentachloroanisole in cork stoppers via headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography tandem mass spectrometry (GC-MS/MS). The influence of the fibre coating used, the extraction times and temperatures, the sodium chloride additions and the desorption temperatures were investigated. Once done, the optimial HS-SPME conditions established were divinylbenzene/carboxenpolydimethylsiloxane/polydimethylsiloxane (DVB/CAR/PDMS) fibres, a 50 degrees C extraction temperature, 60-min extraction time, an ionic strength of 3-g sodium chlorid and a 290 degrees C desorption temperature. The method showed a good linearity (R(2) >/= 0.994) within the tested range (from 0.1 to 50 ng L(-1) ) for all the compounds. Using TCA-d10 and MIB-d3 as internal standards the precision, expressed as repeatability and reproducibility RSD, was <10% in both. Note that the limits of quantifications (LOQs) are below the sensory threshold levels for such compounds in water and wine. Good recoveries were obtained for cork macerates (from 100.4% to 126%) and when compared with other reported methods using HS-SPME in water and cork stopper samples, the present method had more analytes with the lowest limit of detection for most of the targeted compounds, along with good precision and recovery. CI - (c) 2021 John Wiley & Sons, Ltd. FAU - Jove, Patricia AU - Jove P AUID- ORCID: 0000-0002-3435-8444 AD - Catalan Cork Institute and Foundation, Institut Catala del Suro (ICSuro), Girona, Spain. FAU - Pareras, Anna AU - Pareras A AD - Institute of Food and Agricultural Technology-CIDSAV-XaRTA, University of Girona, Girona, Spain. FAU - De Nadal, Raquel AU - De Nadal R AD - R&D department, J.VIGAS, Girona, Spain. FAU - Verdum, Maria AU - Verdum M AD - Catalan Cork Institute and Foundation, Institut Catala del Suro (ICSuro), Girona, Spain. LA - eng PT - Journal Article DEP - 20210403 PL - England TA - J Mass Spectrom JT - Journal of mass spectrometry : JMS JID - 9504818 SB - IM OTO - NOTNLM OT - GC-Triple quadrupole MS OT - cork stoppers OT - earthy-musty compounds OT - headspace solid phase microextraction (HS-SPME) EDAT- 2021/04/23 06:00 MHDA- 2021/04/23 06:00 CRDT- 2021/04/22 20:34 PHST- 2021/03/19 00:00 [revised] PHST- 2021/01/09 00:00 [received] PHST- 2021/03/30 00:00 [accepted] PHST- 2021/04/22 20:34 [entrez] PHST- 2021/04/23 06:00 [pubmed] PHST- 2021/04/23 06:00 [medline] AID - 10.1002/jms.4728 [doi] PST - aheadofprint SO - J Mass Spectrom. 2021 Apr 3;56(5):e4728. doi: 10.1002/jms.4728.