Procedure for the isolation of vanillin from vanilla extracts prior to isotopic authentication by quantitative C-13-NMR

作者：Cicchetti Esmeralda; Silvestre Virginie; Fieber Wolfgang; Sommer Horst; Remaud Gerald; Akoka Serge; Chaintreau Alain^*

来源：Flavour and Fragrance Journal, 2010, 25(6): 463-467.

DOI：10.1002/ffj.2006

• authentication
• isotopic C-13-NMR
• C-13-NMR
• sample preparation
• vanilla

Quantitative isotopic C-13-NMR at natural abundance recently became a new tool for the authentication of natural flavours. In contrast to isotopic-ratio mass spectrometry, which yields the global C-13/C-12 ratio of a molecule, isotopic C-13-NMR allows the determination of isotopic ratios of each spectroscopically differentiable carbon site. Since it requires a significant amount of the purified analyte, an optimized vanillin isolation procedure is presented here. It involves an accelerated solvent extraction of beans, a fat removal step and a subsequent medium-pressure isolation of the vanillin peak on a reusable reverse-phase column, using mostly water as a mobile phase (97%). The overall recovery from the bean extract is 90%. The procedure was automated as much as possible and checked against the risk of isotopic fractionation. The overall protocol was demonstrated to be suitable for isotopic measurements.

• 出版日期2010-12