Caviar is considered a delicacy by luxury product consumers, but few data are available about its flavour chemistry to date. In this study, a multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography and mass spectrometry (GC-MS) approach was developed and employed to identify and quantitatively estimate key volatile organic compounds (VOCs) representative in white sturgeon (A. transmontanus) caviar at five different stages of ripening: raw eggs (t0), after 60 days (t1), 120 days (t2), 180 days (t3), and 240 days (t4) of ripening. The method showed the ability to detect and estimate the quantity of 25 flavour compounds, without any severe alteration of the matrix before the analysis and in a short time. The VOCs detected as representative in caviar samples were primarily aldehydes and alcohols, already well known as responsible of fresh fish and seafood flavours, and mainly deriving from lipid peroxidation processes and microbial activity against lipids and amino acids. We found a significant (p < 0.01) increase in the amount of total aldehydes within t0 (29.64 ng/g) and t4 (121.96 ng/g); moreover, an interesting, great arise of 3-hydroxy-2-butanone at the final stage of storage (48.17 ng/g) was recorded. Alcohols were not detected in raw eggs (t0) and then a decrease from t1 (17.77 ng/g) to t4 (10.18 ng/g) was recorded in their amount, with no statistical significance.
Keywords: SPME; caviar; flavour; multiple headspace extractions; volatile organic compounds.