Analysis of Hop-Derived Thiols in Beer Using On-Fiber Derivatization in Combination with HS-SPME and GC-MS/MS.
Johanna DennenlöhrSarah ThörnerNils RettbergPublished in: Journal of agricultural and food chemistry (2020)
The quantitation of the hop varietal thiols 4-mercapto-4-methyl-2-pentanone (4MMP), 3-mercapto-1-hexanol (3MH), and 3-mercaptohexylacetate (3MHA) from beer is challenging. This primarily relates to their low concentration (ng/L levels) and their reactivity. Published assays for thiol quantitation from beer include complex and/or time-consuming sample preparation procedures involving manual handling and use reagents that are harmful because they contain mercury. To facilitate thiol analysis from beer, the current article is concerned with the implementation of an automated headspace solid-phase microextraction (HS-SPME) on-fiber derivatization (OFD) approach using 2,3,4,5,6-pentafluorobenzyl bromide followed by gas chromatography-tandem mass spectrometry (GC-MS/MS). Optimization of HS-SPME and MRM conditions was based on a central composite design approach. The final OFD-HS-SPME-GC-MS/MS method yielded limits of quantitation below the sensory thresholds of 4MMP, 3MH, and 3MHA. Method validation and application on beers brewed with German, Australian, and US hops, as well as with added fruits displayed excellent method performance.
Keyphrases
- gas chromatography
- tandem mass spectrometry
- ms ms
- ultra high performance liquid chromatography
- high performance liquid chromatography
- mass spectrometry
- liquid chromatography
- simultaneous determination
- liquid chromatography tandem mass spectrometry
- solid phase extraction
- high resolution mass spectrometry
- gas chromatography mass spectrometry
- high resolution
- molecularly imprinted
- healthcare
- primary care
- high throughput
- cell migration
- single cell
- randomized controlled trial