Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS
Abstract
:1. Introduction
2. Materials and Methods
2.1. Reagents and Standards
2.2. Sample Preparation
2.3. Method Optimization
2.3.1. SPME Extraction
2.3.2. Dilution
2.3.3. Single Dimension GC-FID (Flame Ionization Detector) Analysis
2.3.4. Second Dimension Heart-Cutting MDGC-MS
2.4. Proposed Method
2.5. Method Validation
2.5.1. Peak Identification
2.5.2. Linearity
2.5.3. Recovery
2.5.4. Limit of Blank, Limit of Detection, Limit of Quantitation, Accuracy, and Precision
2.6. Data Analysis
3. Results and Discussion
3.1. Extraction Optimization
3.2. Method Validation
3.3. Wine Analysis
4. Conclusions
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Analyte | Molecular Weight | Retention Time (min) | Retention Indices | Monitored Ions (m/z) * | ||
---|---|---|---|---|---|---|
Dimension 1 | Dimension 2 | Calculated | Literature | |||
IBMP | 166.22 | 37.20 | 48.38 | 1517 | 1516 | 124, 151 |
IPMP | 152.19 | 31.14 | 43.78 | 1422 | 1423 | 152, 137 |
SBMP | 166.22 | 35.66 | 47.74 | 1494 | 1494 | 124, 138 |
d3-IBMP | 169.24 | 37.14 | 48.29 | 1515 | N/A | 127, 154 |
d3-IPMP | 155.21 | 31.08 | 43.69 | 1421 | N/A | 140, 155 |
Retention Time (2nd Dimension) | Compound | Retention Indices Literature (1st dimension) | % MS Match |
---|---|---|---|
37.41 | (1H)-Pyrrole | 1499 | 95 |
39.01 | 2,3-Butanediol | 1523 | 98 |
39.32 | 1-Octen-3-ol | 1423 | 96 |
40.56 | cis-Hept-4-enol | 1502 | 88 |
40.69 | 6-Hepten-1-ol | n/a | 90 |
41.40 | Benzaldehyde | 1525 | 98 |
43.48 | p-Cymene | 1426 | 80 |
43.78 | IPMP | 1423 | |
43.96 | Siloxane (system peak) | n/a | |
45.15 | 2-Nonanol | 1521 | 95 |
45.67 | β- Linalool | 1537 | 97 |
47.74 | SBMP | 1494 | |
48.38 | IBMP | 1516 | |
49.10 | Decanal | 1512 | 94 |
50.50 | 2-Bornene | 1519 | 89 |
51.96 | Unknown | ||
53.26 | Vitispirane | 1527 | 94 |
53.97 | Unknown |
Compound | Concentration Range (ng/L) | LOB (ng/L) | LOD (ng/L) | %CV b | Equation | R2 c |
---|---|---|---|---|---|---|
IPMP | 0.260–9.96 | 0.159 | 0.192 | 1.4 | y = −0.9383x 2 + 5.401x + 0.0334 | 0.9993 |
SBMP | 0.130–9.99 | 0.016 | 0.061 | 2.8 | y = −0.1479x2 + 13.188x − 0.0216 | 0.9998 |
IBMP | 0.267–41.16 | 0.110 | 0.175 | 3.5 | y = −0.0615x2 + 3.533x − 0.0238 | 0.9996 |
Wine | IPMP | SBMP | IBMP | ||||||
---|---|---|---|---|---|---|---|---|---|
Spike Concentration (ng/L) | % Recovery | % CV | Spike Concentration (ng/L) | % Recovery | % CV | Spike Concentration (ng/L) | % Recovery | % CV | |
Sauvignon blanc | 0.66 | 95.1 | 5.47 | 0.66 | 97.1 | 2.95 | 2.73 | 106.3 | 2.30 |
Sauvignon blanc | 2.26 | 102.0 | 1.41 | 2.21 | 101.2 | 1.15 | 9.14 | 101.8 | 0.57 |
Model wine (mid-range) | 0.66 | 98.0 | 2.27 | 0.66 | 97.0 | 2.81 | 2.73 | 100.3 | 3.04 |
Model wine (high-range) | 3.32 | 100.8 | 1.34 | 3.33 | 101.3 | 2.62 | 13.72 | 100.1 | 2.82 |
Rosé | 0.66 | 97.7 | 3.43 | 0.66 | 94.9 | 5.21 | 2.73 | 99.6 | 6.57 |
Pinot noir | 0.66 | 100.5 | 0.30 | 0.66 | 94.3 | 4.68 | 2.73 | 95.7 | 3.88 |
Wine | IPMP (ng/L) | SMBP (ng/L) | IBMP (ng/L) |
---|---|---|---|
Sauvignon blanc | 0.259 ± 0.031 | 0.191 ± 0.061 | 0.470 ± 0.164 |
Rosé | Detected (0.248 ± 0.026) | 0.192 ± 0.058 | 5.80 ± 0.42 |
Pinot noir | Not Detected | 0.330 ± 0.370 | 0.360 ± 0.070 |
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Olejar, K.J.; Breitmeyer, J.; Wimalasiri, P.M.; Tian, B.; Field, S.K. Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS. Analytica 2021, 2, 1-13. https://doi.org/10.3390/analytica2010001
Olejar KJ, Breitmeyer J, Wimalasiri PM, Tian B, Field SK. Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS. Analytica. 2021; 2(1):1-13. https://doi.org/10.3390/analytica2010001
Chicago/Turabian StyleOlejar, Kenneth J., Jason Breitmeyer, Pradeep M. Wimalasiri, Bin Tian, and Stewart K. Field. 2021. "Detection of Sub-Aroma Threshold Concentrations of Wine Methoxypyrazines by Multidimensional GCMS" Analytica 2, no. 1: 1-13. https://doi.org/10.3390/analytica2010001