Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 67, Issue 50, Pages 13840-13847Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.jafc.9b01091
Keywords
ambient ionization; volatile analysis; high-throughput; DART; mass spectral imaging
Funding
- EJ Gallo Winery
- NY Wine Grape Foundation Enology Program [I-34]
- Agriculture and Food Research Initiative Award from the United States Department of Agriculture (USDA) National Institute of Food and Agriculture [2017-67007-25940]
- National Science Foundation [ECCS-15420819]
- NIFA [914502, 2017-67007-25940] Funding Source: Federal RePORTER
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The use of headspace thin-film microextraction devices (SPMESH) for parallel extraction of trace-level volatiles prior to direct analysis in real-time mass spectrometry (DART-MS) has been reported previously, in which volatiles were extracted from samples in multi-well plates. In this report, we demonstrate that headspace extraction of volatiles by SPMESH sheets can be performed directly from planar surfaces. When coupled with DART-MS, this approach yields volatile mass spectral images with at least 4 mm resolution. When samples were spotted onto general-purpose silica gel thin-layer chromatography (TLC) plates, the SPMESH extraction could reach equilibrium within 2-4 min and 48 samples could be extracted and analyzed in 14 min. Because volatilization of analytes from TLC plates was very rapid, SPMESH extraction was delayed by the addition of 5% polyethylene glycol. Good linearity was achieved in the microgram per liter to milligram per liter range for four odorants (3-isobutyl-2-methoxypyrazine, linalool, methyl anthranilate, and o-aminoacetophenone) in several matrices (water, 10% ethanol, juice, and grape macerate) using 5 mu L sample sizes. Detection limits as low as 50 pg/spot (10 mu g/L in grape macerate) could be achieved. In contrast to many reports on headspace solid-phase microextraction, negligible matrix effects were observed for ethanol and grape macerates compared to water. SPMESH can preserve volatile images from planar surfaces, and SPMESH-DART-MS from TLC plates is well-suited for rapid trace volatile analysis, especially with small sample sizes.
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