Development of an Automated Method for Selected Aromas of Red Wines from Cold-Hardy Grapes Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry-Olfactometry
Abstract
:1. Introduction
2. Materials and Methods
2.1. Samples, Internal Standard, SPME
2.2. GC-MS-Olfactometry System
3. Results
3.1. SPME Optimization
3.1.1. SPME Coating Selection
3.1.2. Extraction Time
3.1.3. Extraction Temperature
3.1.4. Incubation Time
3.1.5. Sample Volume
3.1.6. Desorption Time
3.1.7. Salt Addition
3.2. Analysis of Wine Samples
GC-MS-Olfactometry
4. Discussion
Acknowledgments
Author Contributions
Conflicts of Interest
References
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RT (min) | Compound | 50/30 µm DVB/CAR/PDMS | 100 µm PDMS | 7 µm PDMS | 85 µm PA | 65 µm PDMS/DVB | 70 µm CW/DVB | 85 µm CAR/PDMS |
---|---|---|---|---|---|---|---|---|
4.77 | Ethyl isobutyrate | 100 | 58 | 0 | 13 | 75 | 29 | 104 |
5.53 | Isobutyl alcohol | 100 | 42 | 1 | 95 | 81 | 97 | 83 |
8.10 | Isoamyl alcohol | 100 | 35 | 0 | 73 | 75 | 66 | 92 |
11.00 | Ethyl lactate | 100 | 17 | 0 | 71 | 60 | 79 | 132 |
11.75 | Ethyl caproate | 100 | 24 | 0 | 7 | 53 | 17 | 109 |
12.92 | Acetic acid | 100 | 5 | 3 | 124 | 38 | 242 | 158 |
16.38 | Ethyl caprylate | 100 | 67 | 1 | 21 | 98 | 45 | 64 |
18.44 | Vitispirane | 100 | 61 | 0 | 16 | 90 | 38 | 99 |
18.34 | Diethyl succinate | 100 | 52 | 0 | 45 | 105 | 56 | 63 |
20.42 | Ethyl decanoate | 100 | 114 | 12 | 56 | 121 | 72 | 53 |
21.13 | Benzenethanol | 100 | 23 | 0 | 74 | 86 | 67 | 82 |
24.03 | Ethyl myristate | 100 | 94 | 32 | 59 | 92 | 66 | 41 |
30.37 | Ethyl palmitate | 100 | 187 | 132 | 135 | 194 | 155 | 17 |
# | RT (min) | LRI A | Stationary Phase 1–10 | Compound | MW | B Foch | B St. Croix | B Frontenac | B Foch/Frontenac | C Vincent | D Frontenac | D Foch |
---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 3.58 | 949 | 2 | 2,3-Butanedione | 86 | 1.11 | 5.18 | 0.85 | 0.32 | 0.94 | 1.39 | 1.05 |
963 | 2 | |||||||||||
955 | 4 | |||||||||||
558 | 5 | |||||||||||
619 | 8 | |||||||||||
575 | 8 | |||||||||||
976 | 9 | |||||||||||
2 | 3.7 | 880 | 2 | Acetal | 118 | 1.24 | 0.96 | 8.57 | 23.1 | 6.75 | 4.9 | 8.08 |
710 | 8 | |||||||||||
3 | 4.08 | 774 | 3 | Ethyl propanoate | 102 | 1.73 | 1.05 | 7.26 | 19.6 | 3.42 | 6.85 | 5.38 |
4 | 4.72 | 956 | 2 | Ethyl isobutyrate | 116 | 5.94 | 1.67 | 3.99 | 3.54 | 6.36 | 2.3 | 1 |
746 | 8 | |||||||||||
5 | 5.49 | 1110 | 2 | Isobutyl alcohol | 74 | 14.6 | 23.8 | 21.9 | 27.6 | 86.1 | 21.4 | 28.7 |
1054 | 2 | |||||||||||
1083 | 4 | |||||||||||
1093 | 4 | |||||||||||
609 | 6 | |||||||||||
616 | 8 | |||||||||||
6 | 6.07 | 863 | 3 | Ethyl butanoate | 116 | 1.55 | 3.43 | 3.5 | 2.2 | 2.63 | 1.05 | 3.59 |
788 | 5 | |||||||||||
7 | 6.66 | 1138 | 4 | n-Butanol | 74 | 0.9 | 1.85 | 1.44 | 4.07 | 1.76 | 4.32 | 1.68 |
1149 | 4 | |||||||||||
634 | 5 | |||||||||||
653 | 6 | |||||||||||
8 | 7.22 | 1060 | 2 | Ethyl isovalerate | 130 | 4.29 | 0.41 | 2 | 1.76 | 0.9 | 0.38 | 0.29 |
856 | 6 | |||||||||||
840 | 8 | |||||||||||
9 | 8.05 | 1184 | 2 | Isoamyl alcohol | 88 | 132 | 355 | 275 | 477 | 475 | 221 | 377 |
719 | 8 | |||||||||||
10 | 8.12 | 1110 | 2 | Isoamyl acetate | 130 | 32.2 | 3.89 | 3.87 | 4.02 | 3.89 | 3.22 | 0 |
860 | 8 | |||||||||||
11 | 10.03 | 1250 | 2 | Styrene | 104 | nd | 16.9 | 3.22 | 0.05 | 0.03 | nd | 0.68 |
12 | 10.91 | 1312 | 2 | Ethyl lactate | 118 | 13.7 | 34.1 | 39.9 | 34.3 | 30 | 67.1 | 19.8 |
1341 | 4 | |||||||||||
803 | 8 | |||||||||||
13 | 11.15 | 1230 | 2 | Ethyl caproate | 144 | 26.4 | 71 | 40.4 | 33 | 34.7 | 21.5 | 64.3 |
1060 | 3 | |||||||||||
1232 | 4 | |||||||||||
1238 | 4 | |||||||||||
985 | 5 | |||||||||||
981 | 5 | |||||||||||
996 | 6 | |||||||||||
996 | 6 | |||||||||||
14 | 11.27 | 1316 | 2 | n-Hexanol | 102 | 8.64 | 0 | 0 | 19.6 | 12.6 | 7.82 | 51.7 |
1330 | 2 | |||||||||||
1332 | 2 | |||||||||||
1352 | 4 | |||||||||||
847 | 5 | |||||||||||
848 | 5 | |||||||||||
848 | 5 | |||||||||||
862 | 6 | |||||||||||
1354 | 9 | |||||||||||
15 | 12.81 | 1400 | 2 | Acetic acid | 60 | 51.4 | 6.61 | 58.2 | 10.6 | 11.6 | 13.2 | 18.7 |
1401 | 2 | |||||||||||
791 | 3 | |||||||||||
1435 | 4 | |||||||||||
1442 | 4 | |||||||||||
1459 | 4 | |||||||||||
621 | 5 | |||||||||||
723 | 8 | |||||||||||
16 | 13.25 | 1437 | 2 | Furfural | 96 | nd | nd | nd | 10.2 | nd | nd | nd |
1438 | 2 | |||||||||||
1450 | 2 | |||||||||||
1449 | 2 | |||||||||||
1447 | 4 | |||||||||||
1456 | 4 | |||||||||||
1466 | 4 | |||||||||||
1465 | 4 | |||||||||||
802 | 5 | |||||||||||
829 | 5 | |||||||||||
800 | 5 | |||||||||||
800 | 5 | |||||||||||
836 | 6 | |||||||||||
868 | 6 | |||||||||||
830 | 6 | |||||||||||
815 | 8 | |||||||||||
17 | 13.57 | 3-Nonanone (IS) | 142 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | ||
18 | 14.37 | 1375 | 1 | Methyl octanoate | 158 | 0.39 | 1.01 | 0.32 | 0.23 | 0.35 | 0.18 | 0.33 |
1392 | 4 | |||||||||||
1109 | 10 | |||||||||||
19 | 14.48 | 1692 | 2 | 1,3-Butanediol | 90 | 1.89 | 4.03 | 11 | 3.38 | 1.48 | 8.15 | 4.43 |
941 | 8 | |||||||||||
20 | 14.81 | 1518 | 1 | Benzaldehyde | 106 | 0.18 | 0.93 | 0.95 | 1.14 | 0.73 | 0.12 | 55.2 |
1516 | 1 | |||||||||||
1509 | 2 | |||||||||||
1454 | 2 | |||||||||||
1520 | 2 | |||||||||||
1482 | 2 | |||||||||||
1502 | 2 | |||||||||||
1086 | 3 | |||||||||||
1515 | 4 | |||||||||||
1496 | 4 | |||||||||||
1513 | 4 | |||||||||||
1538 | 4 | |||||||||||
1530 | 4 | |||||||||||
1522 | 4 | |||||||||||
1516 | 4 | |||||||||||
926 | 5 | |||||||||||
926 | 5 | |||||||||||
926 | 5 | |||||||||||
924 | 6 | |||||||||||
960 | 6 | |||||||||||
962 | 6 | |||||||||||
957 | 6 | |||||||||||
961 | 6 | |||||||||||
944 | 7 | |||||||||||
938 | 7 | |||||||||||
947 | 8 | |||||||||||
947 | 8 | |||||||||||
1540 | 9 | |||||||||||
21 | 15.02 | 1501 | 2 | Isobutyric acid | 88 | 2.45 | 0.28 | 1.38 | 0.78 | 2.46 | 0.45 | 0.32 |
935 | 3 | |||||||||||
22 | 15.15 | 2,3-Butanediol | 90 | 1.41 | 1.56 | 2.31 | 2.03 | 1.5 | 2.62 | 2.35 | ||
23 | 15.72 | 1258 | 3 | Ethyl caprylate | 172 | 164 | 398 | 209 | 116 | 187 | 181 | 205 |
1429 | 4 | |||||||||||
1466 | 4 | |||||||||||
1196 | 6 | |||||||||||
1193 | 6 | |||||||||||
1195 | 6 | |||||||||||
24 | 16.83 | 1631 | 2 | Isovaleric acid | 102 | 8.97 | 2.58 | 7.79 | 5.1 | 3.73 | 3.54 | 3.55 |
834 | 6 | |||||||||||
25 | 17.66 | 1276 | 7 | Vitispirane | 192 | 0 | 3.02 | 0.31 | 4.5 | 15.7 | 3.39 | 0 |
26 | 17.79 | 1278 | 5 | Ethyl nonanoate | 186 | 0.83 | nd | 1.68 | 0 | 0 | 0 | 0.78 |
27 | 17.99 | 1642 | 2 | Diethyl succinate | 174 | 3.62 | 11.5 | 18.9 | 43.8 | 12.9 | 5.77 | 122 |
1153 | 8 | |||||||||||
28 | 19.74 | 1390 | 6 | Ethyl decanoate | 200 | 54.9 | 99.5 | 83.9 | 29.8 | 33.3 | 98.5 | 34.4 |
1391 | 6 | |||||||||||
1394 | 6 | |||||||||||
29 | 20.27 | 1788 | 2 | Phenethyl acetate | 164 | 0.95 | 1.56 | 1.26 | 1.41 | 0.95 | 1.47 | 1.2 |
1785 | 2 | |||||||||||
1233 | 8 | |||||||||||
30 | 20.98 | 1903 | 4 | Benzeneethanol | 122 | 41.3 | 146 | 56 | 232 | 111 | 53.7 | 134 |
31 | 23.06 | 2007 | 2 | Octanoic acid | 144 | 1.39 | 1.07 | 6.63 | 0.09 | 1.99 | 2.22 | 0.7 |
2007 | 2 | |||||||||||
2100 | 2 | |||||||||||
2013 | 2 | |||||||||||
2075 | 4 | |||||||||||
1183 | 6 | |||||||||||
1256 | 7 | |||||||||||
32 | 23.36 | 1595 | 6 | Ethyl laurate | 228 | 3.3 | 2.63 | 6.73 | 1.62 | 1.28 | 8.24 | 2.72 |
33 | 24.76 | 4-Ethylphenol | 122 | nd | 7.49 | 2.32 | nd | nd | 3.4 | 2.33 | ||
34 | 24.81 | 8-Pentadecanone | 226 | 1.06 | 7.49 | 2.31 | 2.53 | 2.33 | 3.4 | 2.32 | ||
35 | 26.57 | Glycerol | 92 | nd | nd | 26.8 | nd | nd | nd | nd | ||
36 | 26.63 | 1793 | 6 | Ethyl myristate | 256 | 0.39 | 0.53 | 0.48 | 0.38 | 0.57 | 0.84 | 0.99 |
37 | 29.63 | 1993 | 6 | Ethyl palmitate | 284 | 2.35 | 2.1 | 5.75 | 1.92 | 2.81 | 4.12 | 5.14 |
1985 | 7 |
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Cai, L.; Rice, S.; Koziel, J.A.; Dharmadhikari, M. Development of an Automated Method for Selected Aromas of Red Wines from Cold-Hardy Grapes Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry-Olfactometry. Separations 2017, 4, 24. https://doi.org/10.3390/separations4030024
Cai L, Rice S, Koziel JA, Dharmadhikari M. Development of an Automated Method for Selected Aromas of Red Wines from Cold-Hardy Grapes Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry-Olfactometry. Separations. 2017; 4(3):24. https://doi.org/10.3390/separations4030024
Chicago/Turabian StyleCai, Lingshuang, Somchai Rice, Jacek A. Koziel, and Murlidhar Dharmadhikari. 2017. "Development of an Automated Method for Selected Aromas of Red Wines from Cold-Hardy Grapes Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry-Olfactometry" Separations 4, no. 3: 24. https://doi.org/10.3390/separations4030024