MilliporeSigma
  • Home
  • Search Results
  • Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

Molecules (Basel, Switzerland) (2015-07-15)
Lauren E Musumeci, Imelda Ryona, Bruce S Pan, Natalia Loscos, Hui Feng, Michael T Cleary, Gavin L Sacks
ABSTRACT

Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME fiber assortment kit 5, needle size 23 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), metal alloy fiber, for use with manual holder
Supelco
SPME fiber assortment kit 4, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 2, for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with manual holder
Supelco
SPME StableFlex fiber assortment kit, needle size 23 ga, for use with autosampler
Supelco
SPME StableFlex fiber assortment kit, for use with autosampler, needle size 24 ga
Supelco
SPME fiber assortment kit 2, for use with manual holder, needle size 24 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 2, for use with autosampler, size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm (PDMS/DVB), for use with manual holder, needle size 23 ga
Supelco
SPME fiber assortment kit 4, for use with manual holder, size 24 ga
Supelco
SPME fiber assortment kit 1, for use with manual holder, needle size 24 ga
Supelco
SPME StableFlex fiber assortment kit, for use with manual holder
Supelco
SPME fiber assortment kit 4, for use with autosampler, size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with autosampler
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with manual holder
Supelco
IonSense® PDMS/DVB SPE-it Tips, pkg of 96 ea
Supelco
SPME LC Tips, C18, tray of 96 ea
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm (PA), for use with autosampler, needle size 24 ga
Supelco
SPME Sampling Stand, for use with 4 mL vials
Supelco
SPME Portable Field Sampler, coating CAR/PDMS
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm (PDMS), for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm (PDMS), needle size 23 ga, for use with autosampler