A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC–MS/MS method for methoxypyrazine analysis in wine

Hjelmeland, Anna K.; Wylie, Philip; Ebeler, Susan E.

doi:10.1016/j.talanta.2015.10.086

Cited by 29 publications

(10 citation statements)

References 32 publications

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“…The obtained values of IPMP and IBMP were within the ranges observed by Wen et al [6] using a stir bar sorptive extraction in white, Rosé, and red wines. Interestingly, while the method employed by Wen was able to detect the compounds in pg/L levels,…”

Section: Wine Analysissupporting

confidence: 86%

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Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS

et al. 2021

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Complex matrices, such as wine, provide a challenge in the quantification of compounds. There exists a high likelihood of co-elution in these matrices, thereby artificially increasing the observed concentration. This can often lead to confusing data where compounds are above aroma detection thresholds, but are not detected by olfactory analysis. Additionally, the lack of sensitivity in assays can lead to the non-detection of sub-aroma threshold concentrations and contrasting data when olfactory analysis detects these aromas. To eliminate these pitfalls and gain a better understanding of the role that methoxypyrazines impart green character to wine, a quantitative method using headspace solid-phase microextraction coupled to heart-cutting multidimensional gas chromatography mass spectrometry was developed. The method can quantitate the three common methoxypyrazines found in wine at the picogram per liter level while resolving co-eluting compounds. The proposed method was validated using model wine and wine solutions and was ultimately used for the comparative analysis of white, rosé, and red wines.

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Section: Wine Analysissupporting

confidence: 86%

“…SPME requires minimal sampling and the fiber coating can be selected to adsorb compound classes of interest [5]. In the case of the volatile MPs, headspace-SPME (HS-SPME) is ideal for being able to effectively sample and to utilize as a first level of MPs isolation from the other aromatics present [6].…”

Section: Introductionmentioning

confidence: 99%

Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS

et al. 2021

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“…Traditional SPME-GC-MS analyses of these compounds performed in biological matrices generally report a lower LOD than our current SPMESH-DART-MS/MS method but require longer run times. For example, IBMP can be detected by GC-MS down to low nanogram per liter concentrations, with an oven cycle time (not including sample preparation and extraction) of approximately 30 min; a different group reported an LOD for linalool of low micrograms per liter, with an oven cycle time of approximately 45 min . Because our preliminary work with SPMESH-DART-MS/MS indicated detection limits were likely compromised by high background noise, particularly for linalool (Figure S-3), we investigated if high resolution mass spectrometry (HRMS) could offer improvements.…”

Section: Resultsmentioning

confidence: 99%

Solid Phase Mesh Enhanced Sorption from Headspace (SPMESH) Coupled to DART-MS for Rapid Quantification of Trace-Level Volatiles

Jastrzembski

Sacks

2016

Anal. Chem.

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Quantitation of trace-level (μg/L to ng/L) volatile compounds is routinely performed in a broad range of applications, including analyses of odorants, pesticide residues, or toxins in foodstuffs and related matrices. Conventional analyses based on gas chromatography-mass spectrometry (GC-MS) are limited by low throughput, and ambient approaches to sample introduction have typically had poor sensitivity. We prepared polydimethylsiloxane-coated stainless steel meshes for extraction and preconcentration of volatiles (Solid Phase Mesh Enhanced Sorption from Headspace, SPMESH), which could then be analyzed by Direct Analysis in Real Time (DART)-MS. The SPMESH cards were characterized by electron microscopy, and figures of merit for the approach were determined using two representative volatiles: 2-isobutyl-3-methoxypyrazine (IBMP) and linalool. Using DART-MS/MS and isotopically labeled internal standards, we achieved detection limits of 21 ng/L and 71 μg/L for IBMP and linalool in water. Good accuracy and precision could also be achieved for IBMP spikes in grape macerate, although accuracy for linalool was compromised by the presence of interferences. Detection limits could be further improved by an order of magnitude through the use of high resolution (HR) MS. Because extraction can be performed inexpensively in parallel and because it requires short data acquisition times (<1 min), SPMESH-DART-MS may be appropriate for high throughput trace level volatile analyses.

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“…Our laboratory observed carryover of certain methoxypyrazines with the DVB/Car/ PDMS fiber. 25 Perera et al 26 reported significant carryover for a Car/PDMS fiber compared to a PDMS fiber when analyzing wounding compounds of plants with HS-SPME comprehensive two-dimensional GC-MS. Mani 27 explains these reports of carryover with Carboxen-containing fibers by a stronger retention of larger compounds (>12 C atoms) on the fiber, making it difficult to desorb them in a reasonable amount of time in the GC inlet.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

HS-SPME-GC-MS/MS Method for the Rapid and Sensitive Quantitation of 2-Acetyl-1-pyrroline in Single Rice Kernels

Hopfer

Jodari²,

Negre-Zakharov

et al. 2016

J. Agric. Food Chem.

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Demand for aromatic rice varieties (e.g., Basmati) is increasing in the US. Aromatic varieties typically have elevated levels of the aroma compound 2-acetyl-1-pyrroline (2AP). Due to its very low aroma threshold, analysis of 2AP provides a useful screening tool for rice breeders. Methods for 2AP analysis in rice should quantitate 2AP at or below sensory threshold level, avoid artifactual 2AP generation, and be able to analyze single rice kernels in cases where only small sample quantities are available (e.g., breeding trials). We combined headspace solid phase microextraction with gas chromatography tandem mass spectrometry (HS-SPME-GC-MS/MS) for analysis of 2AP, using an extraction temperature of 40 °C and a stable isotopologue as internal standard. 2AP calibrations were linear between the concentrations of 53 and 5380 pg/g, with detection limits below the sensory threshold of 2AP. Forty-eight aromatic and nonaromatic, milled rice samples from three harvest years were screened with the method for their 2AP content, and overall reproducibility, observed for all samples, ranged from 5% for experimental aromatic lines to 33% for nonaromatic lines.

show abstract

A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC–MS/MS method for methoxypyrazine analysis in wine

Cited by 29 publications

References 32 publications

Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS

Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS

Solid Phase Mesh Enhanced Sorption from Headspace (SPMESH) Coupled to DART-MS for Rapid Quantification of Trace-Level Volatiles

HS-SPME-GC-MS/MS Method for the Rapid and Sensitive Quantitation of 2-Acetyl-1-pyrroline in Single Rice Kernels

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