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Determination of thiol compounds by automated headspace solid‐phase microextraction with in‐fiber derivatization
Author(s) -
Wang Qing,
Chong J. Michael,
Pawliszyn Janusz
Publication year - 2006
Publication title -
flavour and fragrance journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.393
H-Index - 70
eISSN - 1099-1026
pISSN - 0882-5734
DOI - 10.1002/ffj.1724
Subject(s) - derivatization , solid phase microextraction , chemistry , detection limit , chromatography , thiol , extraction (chemistry) , reagent , fiber , sample preparation , standard addition , gas chromatography , gas chromatography–mass spectrometry , high performance liquid chromatography , mass spectrometry , organic chemistry
In this article, headspace solid‐phase microextraction (HS‐SPME) analysis of thiol compounds with both solid and aqueous samples was investigated using N ‐phenylmaleimide as an in‐fiber derivatization reagent. The derivatives were analyzed using GC‐MS. The HS‐SPME method was executed on an automatic sampler and optimized by studying a variety of factors such as the selection of the fiber, extraction time, temperature, agitation speed, etc. Method validation was carried out by spiking known amounts of thiol compounds into the sample and calculating the concentration by standard addition. The relative standard deviations (RSD) for the majority of the thiols were less than 10%. The developed method resulted in a limit of detection (LOD) in the low microgram per liter for most of the thiols analyzed, which was about one order of magnitude lower than the HS‐SPME without derivatization. Finally, the overall method was successfully applied for the determination of thiols in yellow onion, green onion and garlic. Copyright © 2006 John Wiley & Sons, Ltd.