Monitoring Cider Aroma Development throughout the Fermentation Process by Headspace Solid Phase Microextraction (HS-SPME) Gas Chromatography–Mass Spectrometry (GC-MS) Analysis
"> Figure 1
<p>Volatile organic species of interest to this study include esters (<b>A</b>), higher alcohols (<b>B</b>), and phenols (<b>C</b>) with specific functional groups color coded above. Esters (<b>A</b>) that are routinely observed herein include ethyl acetate (R = CH<sub>3</sub>), ethyl benzoate (R = C<sub>6</sub>H<sub>5</sub>), ethyl hexanoate (R = CH<sub>3</sub>(CH<sub>2</sub>)<sub>4</sub>), ethyl octanoate (R = CH<sub>3</sub>(CH<sub>2</sub>)<sub>6</sub>), ethyl decanoate (R = CH<sub>3</sub>(CH<sub>2</sub>)<sub>8</sub>), and ethyl dodecanoate (R = CH<sub>3</sub>(CH<sub>2</sub>)<sub>10</sub>). Higher alcohols (<b>B</b>) of importance to cider aroma include 1-hexanol (R = CH<sub>3</sub>(CH<sub>2</sub>)<sub>3</sub>), 3-methyl-1-butanol (R = (CH<sub>3</sub>)<sub>2</sub>CH), and 2-phenylethyl alcohol (C<sub>6</sub>H<sub>5</sub>). Lastly, volatile phenols that are considered defect odors in cider include 4-ethylphenol (R<sub>1</sub> = CH<sub>3</sub>CH<sub>2</sub>) and 4-ethyl-2-methoxyphenol (R<sub>1</sub> = CH<sub>3</sub>CH<sub>2</sub> and R<sub>2</sub> = CH<sub>3</sub>O).</p> "> Figure 2
<p>Overlaid chromatograms of a single cider sample (EsoTerra Cider) analyzed with 3 different solid phase microextraction (SPME) fibers are shown. Polyacrylate (PA: Red), carboxen/polydimethylsiloxane, (CAR/PDMS: Green), and divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS: Blue) were compared. A wider variety of esters (<b>1</b>: Ethyl acetate, <b>2</b>: Methyl formate, <b>6</b>: Hexanoic acid ethyl ester, <b>9</b>: Benzoic acid ethyl ester, <b>10</b>: Octanoic acid ethyl ester, <b>12</b>: Nonanoic acid ethyl ester, <b>13</b>: Ethyl 9-decanoate, <b>14</b>: Decanoic acid ethyl ester, <b>15</b>: Dodecanoic acid ethyl ester), higher alcohols (<b>3</b>: 3-Methyl-1-Butanol, <b>4</b>: 1-Hexanol, <b>7</b>: 1-Octanol, <b>8</b>: 2-Phenylethyl alcohol), phenols (<b>11</b>: 4-ethyl-2-methoxyphenol), and an imine (<b>5</b>: methoxy-phenyl-oxime) were detected consistently at higher abundance in the DVB/CAR/PDMS fiber than the other fibers analyzed.</p> "> Figure 3
<p>Overlaid chromatograms for one cider sample (EsoTerra Cider) were obtained by headspace solid phase microextraction (HS-SPME) using DVB/CAR/PDMS fibers at 40 °C for various exposure times (5 min: blue, 30 min: purple, 90 min: green) to optimize sampling conditions. The five most abundant and reproduceable peaks were identified and labeled on each chromatogram (<b>1:</b> ethyl hexanoate, <b>2:</b> phenethyl alcohol, <b>3:</b> ethyl octanoate, <b>4:</b> ethyl decanoate, and <b>5:</b> ethyl dodecanoate).</p> "> Figure 4
<p>A hydrometer was used to measure specific gravity throughout a cider fermentation to monitor fermentation progression (<b>A</b>). Specific gravity measurements were taken before yeast inoculation (<b>red</b>), at various stages during fermentation (<b>purple, black, green</b>), and when fermentation was complete (<b>blue</b>). Four chromatograms were obtained by headspace solid phase microextraction gas chromatography–mass spectrometry (HS-SPME GC-MS), with a DVB/CAR/PDMS fiber, in order to compare changes in aroma profiles based on volatile constituents (<b>B</b>). All chromatographic peaks are numbered in order of their observation throughout the fermentation process. Peaks one through fifteen (<b>1</b>: ethyl acetate, <b>2</b>: ethyl propionate, <b>3</b>: 2-methyl-1-butanol, <b>4</b>: ethyl butyrate, <b>5</b>: butyl acetate, <b>6</b>: ethyl-2-methyl butyrate, <b>7</b>: 1-hexanol, <b>8</b>: 2-methyl butyl acetate, <b>9</b>: propyl butyrate, <b>10</b>: 2-methyl propyl butyrate, <b>11</b>: ethyl hexanoate, <b>12</b>: hexyl acetate, <b>13</b>: butyl 2-methylbutyrate, <b>14</b>: estragole, and <b>15</b>: hexyl 2-methylbutanoate) were detected in the juice sample (<b>red</b>). Peaks one through eight, ten through twelve, and fourteen through twenty-two (<b>16</b>: ethyl 3-methylbutyrate, <b>17</b>: 3-methylbutyl acetate, <b>18</b>: 2-phenylethyl alcohol, <b>19</b>: ethyl octanoate, <b>20</b>: ethyl decanoate, <b>21</b>: 3-methylbutyl octanoate, and <b>22</b>: ethyl dodecanoate) were identified in samples taken on day three (<b>purple</b>), day eight (<b>green</b>), and at the completion of fermentation (<b>blue</b>). Only one species (<b>23</b>: ethyl-9-decenoate) was detected on day 13 (fermentation completion) only.</p> ">
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sample Preparation and Fermentation
2.2. Solid Phase Microextraction (SPME) Optimization
2.3. Gas Chromatography–Mass Spectrometry Analysis
3. Results and Discussion
3.1. Cider VOC Development throughout the Fermentation Process
3.2. Cider VOC Profiles Resulting from Different Yeast Strains
4. Conclusions
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
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Edinburgh Yeast | Relative Peak Area | Retention Time (min) | NIST (%) a | Odor Descriptor | Perception Threshold (μg L−1) |
---|---|---|---|---|---|
Ethyl octanoate | 1.00 | 22.1 | 92.3 | Fruity, candy, pineapple b,c | 580 b |
Ethyl decanoate | 0.85 | 31.0 | 89.1 | Fruity, grape b | 200 b |
3-methyl-1-butanol | 0.18 | 3.1 | 69.0 | Alcohol, nail polish, whiskey b | 30,000 b |
Ethyl hexanoate | 0.16 | 12.3 | 85.5 | fruity, strawberry, green apple b | 14 b |
Ethyl benzoate | 0.14 | 20.6 | 77.3 | Camomile, flower, celery, fruit d | 60 e |
Ethyl dodecanoate | 0.11 | 38.9 | 82.3 | Candy, floral, waxy, soap b | 1500 b |
4-ethyl-2-methoxyphenol | 0.11 | 25.6 | 81.1 | Phenolic, smoked f | 6.9 f |
2-phenylethyl alcohol | 0.11 | 17.8 | 84.3 | Rose, honey g | 390 g |
1-hexanol | 0.09 | 6.5 | 69.0 | Herbaceous, fatty, floral b | 110 b |
4-ethylphenol | 0.08 | 20.7 | 85.3 | Phenolic, leather g,h | 21 g |
Decanoic acid | 0.07 | 30.3 | 97.3 | Rancid fat, animal b | 1000 b |
Belgian II Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
Ethyl octanoate | 1.00 | 22.1 | 89.1 | Fruity, candy, pineapple b,c | 580 b |
Ethyl decanoate | 0.86 | 31.0 | 88.9 | Fruity, grape b | 200 b |
2-phenylethyl alcohol | 0.23 | 17.8 | 83.5 | Rose, honey g | 390 g |
Ethyl hexanoate | 0.19 | 12.3 | 88.6 | Fruity, strawberry, green apple b | 14 b |
3-methyl-1-butanol | 0.14 | 3.1 | 41.7 | Alcohol, nail polish, whiskey b | 30,000 b |
Ethyl benzoate | 0.12 | 20.6 | 67.0 | Camomile, flower, celery, fruit d | 60 e |
4-ethyl-2-methoxyphenol | 0.09 | 25.6 | 80.4 | Phenolic, smoked f | 6.9 f |
1-hexanol | 0.07 | 6.5 | 66.1 | Herbaceous, fatty, floral b | 110 b |
Decanoic acid | 0.07 | 30.2 | 98.0 | Rancid fat, animal b | 1000 b |
Ethyl dodecanoate | 0.06 | 38.9 | 85.9 | Candy, floral, waxy, soap b | 1500 b |
French Saison Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
Ethyl octanoate | 1.00 | 22.1 | 93.3 | Fruity, candy, pineapple b,c | 580 b |
Ethyl decanoate | 0.50 | 31.0 | 88.6 | Fruity, grape b | 200 b |
3-methyl-1-butanol | 0.15 | 3.1 | 42.5 | Alcohol, nail polish, whiskey b | 30,000 b |
Ethyl hexanoate | 0.15 | 12.3 | 91.9 | Fruity, strawberry, green apple b | 14 b |
2-phenylethyl alcohol | 0.12 | 17.8 | 86.3 | Rose, honey g | 390 g |
Ethyl dodecanoate | 0.09 | 38.9 | 83.3 | Candy, floral, waxy, soap b | 1500 b |
Ethyl benzoate | 0.09 | 20.5 | 71.4 | Camomile, flower, celery, fruit d | 60 e |
Ethyl-9-decenoate | 0.07 | 30.5 | 99.0 | Roses b | 100 b |
Abbey Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
Ethyl octanoate | 1.00 | 22.1 | 92.4 | Fruity, candy, pineapple b,c | 580 b |
Ethyl decanoate | 0.65 | 31.0 | 90.3 | Fruity, grape b | 200 b |
3-methyl-1-butanol | 0.21 | 3.1 | 44.8 | Alcohol, nail polish, whiskey b | 30,000 b |
Ethyl hexanoate | 0.18 | 12.3 | 92.8 | Fruity, strawberry, green apple b | 14 b |
Ethyl benzoate | 0.18 | 20.6 | 95.0 | Camomile, flower, celery, fruit d | 60 e |
2-phenylethyl alcohol | 0.16 | 17.8 | 87.5 | Rose, honey g | 390 g |
4-ethyl-2-methoxyphenol | 0.10 | 25.6 | 81.4 | Phenolic, smoked f | 6.9 f |
Decanoic acid | 0.07 | 30.3 | 98.0 | Rancid fat, animal g | 1000 g |
1-hexanol | 0.06 | 6.5 | 66.7 | Herbaceous, fatty, floral b | 110 b |
Edinburgh Yeast | Relative Peak Area | Retention Time (min) | NIST (%) a | Odor Descriptor | Perception Threshold (μg L−1) |
---|---|---|---|---|---|
Ethyl nonanoate | 0.012 | 26.5 | 90.7 | Fatty, oily, fruity, nutty b | − |
Ethyl acetate | 0.010 | 1.9 | 86.0 | Solvent, fruity, balsamic b | 12,000 b |
3-methylbutyl octanoate | 0.009 | 33.0 | 70.7 | Fruity, flore b | 125 d |
Phenethyl acetate | 0.008 | 24.6 | 85.3 | Rose, honey e | 3,317,000 f |
Ethyl hexadecanoate | 0.007 | 52.7 | 98.7 | Waxy, greasy g | 1500 g |
3-methylbutyl n-decanoate | 0.006 | 40.7 | 96.3 | Fruity h | − |
Belgian II Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
Ethyl acetate | 0.031 | 2.0 | 95.7 | Solvent, fruity, balsamic b | 12,000 b |
Dodecanoic acid | 0.010 | 37.8 | 97.0 | Fatty c | − |
Ethyl tetradecanoate | 0.007 | 46.1 | 96.7 | Lily g | − |
Ethyl hexadecanoate | 0.007 | 52.7 | 99.0 | Waxy, greasy g | 1500 g |
French Saison Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
1-hexanol | 0.042 | 6.5 | 67.6 | Herbaceous, fatty, floral b | 110 b |
1-octanol | 0.019 | 15.8 | 49.5 | Citrus, green i | 6.9 i |
Decanoic acid | 0.027 | 30.2 | 98.0 | Rancid fat, animal g | 1000 g |
Methyl salicylate | 0.018 | 21.7 | 96.0 | Peppermint g | 0.1 g |
4-ethyl-2-methoxyphenol | 0.010 | 25.6 | 92.0 | Phenolic, smoked j | 3 j |
4-ethylphenol | 0.008 | 20.8 | 94.7 | Phenolic i | 21 h |
Ethyl nonanoate | 0.006 | 26.5 | 87.7 | Fatty, oily, fruity, nutty b | − |
Ethyl acetate | 0.006 | 2.0 | 92.4 | solvent, fruity, balsamic g | 12,000 g |
2-phenylethyl acetate | 0.005 | 24.6 | 80.0 | Rose, honey j | 108 j |
Abbey Yeast | RPA | RT (min) | NIST (%) | Odor Descriptor | PT (μg L−1) |
Ethyl acetate | 0.034 | 2.0 | 92.5 | Solvent, fruity, balsamic b | 12,000 b |
Ethyl dodecanoate | 0.031 | 38.8 | 66.7 | Candy, floral, waxy, soap b | 1500 b |
3-methylbutyl acetate | 0.030 | 6.8 | 87.9 | Banana i | 30 i |
Ethyl-9-decenoate | 0.020 | 30.5 | 98.7 | Roses g | 100 g |
Hexyl acetate | 0.008 | 13.0 | 87.3 | Banana, apple, pear j | 0.2 k |
1-octanol | 0.007 | 15.8 | 90.0 | Citrus, green i | 6.9 i |
2-phenylethyl acetate | 0.007 | 24.7 | 74.7 | Roses, honey j | 108 j |
Ethyl 2-methylbutanoate | 0.006 | 5.8 | 95.7 | Strawberry, candy, fruit g | 18 g |
Diethyl butanedioate | 0.004 | 21.3 | 78.7 | Wine, caramel, fruity g | 200,000 g |
Analyte (Odor) | Edinburgh Yeast | Belgian II Yeast | French Saison Yeast | Abbey Yeast | Perception Threshold (mg·L−1) |
---|---|---|---|---|---|
Ethyl acetate (solvent, fruity, balsamic) b | 1.89 ± 0.42 a | 33.00 ± 7.26 | 2.52 ± 0.55 | 41.28 ± 9.08 | 12 b |
Ethyl octanoate (fruity, candy, pineapple) b | 0.13 ± 0.03 | 0.16 ± 0.04 | 0.29 ± 0.08 | 0.20 ± 0.05 | 0.014 b |
2-Phenylethyl alcohol (Rose, honey) c | 6.85 ± 1.03 | 11.95 ± 1.79 | 9.59 ± 1.44 | 8.98 ± 1.35 | 0.390 c |
3-methyl-1-butanol (Alcohol, nail polish, whiskey) b | 13.40 ± 3.58 | 32.36 ± 8.64 | 44.47 ± 11.87 | 38.51 ± 10.28 | 30 b |
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Bingman, M.T.; Stellick, C.E.; Pelkey, J.P.; Scott, J.M.; Cole, C.A. Monitoring Cider Aroma Development throughout the Fermentation Process by Headspace Solid Phase Microextraction (HS-SPME) Gas Chromatography–Mass Spectrometry (GC-MS) Analysis. Beverages 2020, 6, 40. https://doi.org/10.3390/beverages6020040
Bingman MT, Stellick CE, Pelkey JP, Scott JM, Cole CA. Monitoring Cider Aroma Development throughout the Fermentation Process by Headspace Solid Phase Microextraction (HS-SPME) Gas Chromatography–Mass Spectrometry (GC-MS) Analysis. Beverages. 2020; 6(2):40. https://doi.org/10.3390/beverages6020040
Chicago/Turabian StyleBingman, Matthew T., Claire E. Stellick, Jordanne P. Pelkey, Jared M. Scott, and Callie A. Cole. 2020. "Monitoring Cider Aroma Development throughout the Fermentation Process by Headspace Solid Phase Microextraction (HS-SPME) Gas Chromatography–Mass Spectrometry (GC-MS) Analysis" Beverages 6, no. 2: 40. https://doi.org/10.3390/beverages6020040