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Parallel Headspace Extraction onto Etched Sorbent Sheets Prior to Ambient-Ionization Mass Spectrometry for Automated, Trace-Level Volatile Analyses
journal contribution
posted on 2018-10-26, 00:00 authored by Madeleine
Y. Bee, Jillian A. Jastrzembski, Gavin L. SacksHeadspace (HS) extraction
and preconcentration of volatiles by
solid-phase microextraction (SPME) can improve the sensitivity and
selectivity of ambient ionization-mass spectrometry approaches like
direct analysis in real time (DART), but previous approaches to HS-SPME-DART-MS
have been challenging to automate. This report describes the production
of inexpensive, reusable solid-phase mesh-enhanced sorption from headspace
(SPMESH) sheets by laser-etching mesh patterns into poly(dimethylsiloxane)
(PDMS) sheets. Parallel headspace extraction of volatiles from multiple
samples can be achieved by positioning the SPMESH sheets over multiwell
plates and then attaching to a positioning stage for automated DART-MS
quantitation. Using three representative odorants (3-isobutyl-2-methoxypyrazine,
linalool, and methyl anthranilate), we achieved μg/L–ng/L
detection limits with SPMESH-DART-MS, with the DART-MS step requiring
only 17 min for 24 samples. Acceptable repeatability (24% or less
day-to-day variation) and excellent recovery from a grape matrix (99–106%)
could be achieved. Through use of a Teflon gasket and stainless steel
spacers, cross-contamination between the headspaces of adjacent wells
could be limited to roughly 1%. Optimum SPMESH extraction and desorption
parameters were determined by response surface methodology. In summary,
sheet-based SPMESH provides a sensitive, readily automated approach
for coupling with DART-MS and achieving high-throughput trace-level
volatile analyses.
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DART-MS stepSPMESH sheetslaser-etching mesh patternsTeflon gasketAnalyses HeadspacePDMSsheet-based SPMESHHShigh-throughput trace-levelvolatile17 minsolid-phase mesh-enhanced sorptionHS-SPME-DART-MSParallel headspace extractionmultiwell platesAmbient-Ionization Mass SpectrometryEtched Sorbent Sheetsambient ionization-mass spectrometry approachesresponse surface methodologySPMESH-DART-MSParallel Headspace Extraction24 samplessteel spacersDART-MS quantitationdesorption parameterssolid-phase microextraction
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