Volatile profiles of Cabernet Gernischet wine under rain-shelter cultivation and open-field cultivation using solid-phase micro-extraction–gas chromatography/mass spectrometry

Figures & data

Table 1. Mesoclimate of vineyard during the growing season of the 2010 and 2011 vintages.

Parameter	April	May	June	July	August	September	April to September
Vintage 2010
Average temperature (°C)	13.2	19.9	25.4	27.2	24.7	21.3	22.0
Rainfall (mm)	41.0	42.7	23.8	77.0	145.1	85.9	415.5
Sunlight hours	170	150.5	219.6	158	145.4	152.1	995.6
Vintage 2011
Average temperature (°C)	16.5	19.4	25.5	26.5	24.1	18.3	21.7
Rainfall (mm)	15.2	83.5	25.7	50.3	87.2	321.1	583.0
Sunlight hours	224.6	197.5	200.5	183.1	189.1	94.7	1089.5

Table 2. Physicochemical parameters of must and wine in the winemaking phases of different treatments.

			Total sugar (g/L)^a	Total acidity (g/L)^b	pH	Ethanol (% vol)
Must after filling the tank	Vintage 2010	T1^c	179.2 ± 5.4Aa	4.7 ± 0.3Aa (8.0)^e	—	—
		T2^d	171.2 ± 4.2Aa	4.5 ± 0.2Aa (8.0)	—	—
	Vintage2011	T1	176.7 ± 5.3Aa	3.6 ± 0.2Aa (8.0)	—	—
		T2	153.7 ± 4.0Bb	3.9 ± 0.2Aa (8.0)	—	—
At the end of alcoholic fermentation	Vintage 2010	T1	1.8 ± 0.2Aa	5.6 ± 0.4Aa	3.6 ± 0.2Aa	12.6 ± 1.2Aa
		T2	1.9 ± 0.2Aa	6.4 ± 0.5Aa	3.3 ± 0.1Aa	10.05 ± 1.0Aa
	Vintage2011	T1	1.7 ± 0.4Aa	4.8 ± 0.4Bb	3.4 ± 0.1Aa	11.3 ± 0.6Aa
		T2	2.1 ± 0.3Aa	5.9 ± 0.4Aa	3.2 ± 0.1Aa	11.2 ± 0.5Aa

^aConcentration represented by glucose.

^bConcentration presented by tartaric acid.

^cT1: Rain-shelter cultivation.

^dT2: Open-air cultivation.

^eThe data outside the brackets represent the acid content in must before acidity adjusted (the acid content in grape after harvest), and the data inside the brackets represent the acid content in must after acidity adjusted (the acid content of must before fermentation).

The same letter mean are not statistically different in different treatments (p < 0.05).

Table 3. The parameters of volatile compounds identified in the Cabernet Gernischet wines.

Compounds	RI^a	ID^b	Purity	Manufacturers	Threshold (μg/L)	Reference of threshold^c	Aroma descriptor	Reference of aroma descriptor^c	Aroma series^d	Reference of aroma seriesd^c
Alcohols
1-Hexanol	1353	A	0.97	Sigma–Aldrich	1100	[1]	Herbaceous, grass,woody	[1,2]	3	[1,2]
(E)-3-Hexen-1-ol	1365	A	0.98	Sigma–Aldrich	1000	[3]	Herbaceous, green	[3]	3	[3]
(Z)-3-Hexen-1-ol	1387	A	0.96	Sigma–Aldrich	1000	[1]	Herbaceous, green,bitter, fatty	[1,3]	3,8	[1,3]
(E)-2-Hexen-1-ol	1409	A	0.95	Sigma–Aldrich	15,000	[3]	Herbaceous, green	[3]	3	[3]
1-Propanol	1057	B			306,000	[1]	Alcohol, ripe fruit	[1]	1,7	[1]
1-Butanol	1158	A	0.99	Sigma–Aldrich	150,000	[1]	Medicinal, phenolic	[1-3]	7	[1-3]
Isobutanol	1111	A	0.99	Sigma–Aldrich	75,000	[1]	Alcohol, solvent,green, bitter	[1]	3,7	[1]
1-Pentanol	1256	A	0.99	Sigma–Aldrich	64,000	[6]	Balsamic, bitter almond	[6]	7,8	[6]
Isopentanol	1220	A	0.99	Sigma–Aldrich	60,000	[1]	Solvent, sweet,alcohol, nail polish	[1,7]	7,5,8	[1,7]
3-Methyl-2-butenol	1322	B
3-Methyl-3-buten-1-ol	1256	B			600	[8]
3-Methyl-1-pentanol	1328	B			500	[8]	Pungent, solvent,green	[2]	3,7	[2]
4-Methyl-1-pentanol	1316	A	0.97	Sigma–Aldrich	50,000	[9]	Almond, toasted	[6,9]	4,5,9	[6,9]
1-Heptanol	1455	A	0.99	Sigma–Aldrich	200	[8]	Oily	[6]	8	[6]
1-Octanol	1562	A	0.99	Sigma–Aldrich	800	[8]	Jasmine, lemon	[10,11]	2	[10,11]
2-Ethyl-1-hexanol	1493	A	0.99	Sigma–Aldrich	8,000	[8]
2-Nonanol	1517	A	0.99	Sigma–Aldrich
1-Decanol	1765	A	0.99	Sigma–Aldrich	400	[9]
1-Dodecanol	1974	A	0.98	Sigma–Aldrich
Benzyl Alcohol	1892	A	0.98	Sigma–Aldrich	200,000	[1]	Roasted, sweet	[1,6]	1,5,9	[1,6]
2-Phenylethanol	1928	A	0.99	Sigma–Aldrich	14,000	[9]	Roses, honey	[7]	2	[7]
laevo-2,3-Butanediol	1542	A	0.99	Sigma–Aldrich	150,000	[6]	Fruity, sweet, butter	[6]	1,5,8	[6]
(S)-3-Ethyl-4-methylpentanol	1509	B
3-(Methylthio)-1-propanol	1726	B
1,9-Nonanediol	1414	B
(3-Methyl-1,5-pentanediol)	1060	B
Esters
Isoamyl acetate	1122	A	0.95	Sigma–Aldrich	160	[1]	Banana	[7]	1	[7]
Phenethyl acetate	1830	A	0.99	Sigma–Aldrich	1800	[1]	Fruity, rose	[1,2]	1,2,5	[1,2]
Ethyl acetate	890	A	0.99	Sigma–Aldrich	7500	[4]	Fruity, sweet	[4]	1	[4]
Ethyl hexoate	1232	A	0.99	Sigma–Aldrich	80	[1]	Banana, green apple	[7]	1	[7]
Ethyl heptanoate	1334	B
Ethyl 2-hexenoate	1346	B		Sigma–Aldrich
Ethyl lactate	1350	A	0.98	Sigma–Aldrich	154,636	[9]	Fruity, buttery	[1]	1,8	[1]
Ethyl octanoate	1437	A	0.99	Sigma–Aldrich	580	[1]	Sweet, floral, fruity,banana, pear	[2]	1,2	[2]
Ethyl laurate	1576	B
Ethyl dodecanoate	1848	A	0.98	Sigma–Aldrich	1500	[12]	Flowery,fruity	[12]
Isoamyl hexanoate	1227	B
Methyl salicylate	1792	A	0.99	Sigma–Aldrich
Ethyl decanoate	1639	A	0.99	Sigma–Aldrich
γ-Butyrolactone	1645	B
Diethyl succinate	1682	A	0.99	Sigma–Aldrich
Ethyl 9-decenoate	1693	B
n-Hexyl isobutyrate	1378	B
Ethyl benzenepropanoate	1898	B
Ethyl octadecanoate	2183	B
Ethyl hydroxycinnamate	1522	B		Sigma–Aldrich
Ethyl eicosanoate	2649	B		Sigma–Aldrich
Acids				Sigma–Aldrich
Propanoic acid	1551	A	0.99	Sigma–Aldrich	8100	[9]	Pungent, rancid, soy	[6]	8	[6]
Hexanoic acid	1860	A	0.99	Sigma–Aldrich	420	[9]	Cheese, fatty	[7]	8	[7]
Octanoic acid	2075	A.	0.99	Sigma–Aldrich	500	[9]	Rancid, cheese, fatty acid	[7]	8	[7]
n-Decanoic acid	2292	A	0.98	Sigma–Aldrich	1000	[9]	Fatty, rancid	[7]	8	[5]
Acetic acid	1463	A	0.99	Sigma–Aldrich
2-Methyl-propanoic acid	1590	B
Carbonyl compounds
Benzaldehyde	1534	A	0.99	Sigma–Aldrich	2000	[1]	Roasted, almond	[3]	9	[3]
Terpenes
Linalool	1547	A	0.97	Sigma–Aldrich	25	[9]	Flowery, muscat	[7]	2,5	[7]
Geraniol	1793	B		Sigma–Aldrich	20	[14]	Citric, geranium	[7,14]	2	[7,15]
C13-norisoprenoid
β-Damascenone	1833	B		Sigma–Aldrich	0.14	[13]	Sweet, exotic	[6,7]	1,2,5	[6,7]
Others
4-Methyl-1-pentene	556	B
Butylated hydroxytoluene	1925	B

^aRetention indices on HP-Innowax column.

^bIdentification of the compounds, ‘A’ means identified by mass spectrum and RI agree with standards, “B” means tentatively identified by mass spectrum agrees with the mass spectral database and RI agrees with literature.

^c[1] (Peinado et al., 2004)^[65], [2] (Peinado et al., 2006)^[31], [3] (Franco, Peinado, Medina, et al., 2004)^[66], [4] (Guth, H., et al., 1997)^[40], [5] (Noble et al., 1987)^[29], [6] (Sánchez-Palomo et al., 2010)^[32], [7] (Noguerol-Pato et al., 2012)^[34], [8] (Tao & Zhang, 2010)^[67], [9] (Ferreira et al., 2000)^[68], [10] (La Guerche, Dauphin, Pons, et al., 2006)^[69], [11] (Jiang & Zhang, 2010)^[12], [12] (Li, H., et al., 2006)^[70], [13] (Pineau, Barbe, Van Leeuwen, et al., 2007)^[71], [14] (Gómez-Míguez et al., 2007)^[13].

^d1: fruity, 2: floral, 3: herbaceous (or vegetal, fresh), 4: nutty, 5: caramel (or sweet), 6: earthy, 7: chemical, 8: fatty, 9: roasted.

Table 4. The concentration of volatile compounds and their odor activity values (OAVs) at the end of alcoholic fermentation (AF) in two vintages.

	Vintage 2010 Contents (μg/L)		Vintage 2011 Contents (μg/L)		Vintage 2010 odor activity values^c		Vintage 2011 odor activity values
Compounds	T1^a	T2^b	T1	T2	T1	T2	T1	T2
Alcohols
1-Hexanol	1601.8Aa	1439.7Aa	9858.5Aa	10457.9Aa	1.5	1.3	9.0	9.5
(E)-3-Hexen-1-ol	42.8Aa	36.4Aa	tr	tr	0.0	0.0	–	–
(Z)-3-Hexen-1-ol	281.3Aa	250.9Aa	tr	tr	0.3	0.3	–	–
(E)-2-Hexen-1-ol	19.1	nd	nd	nd	0.0	–	–	–
1-Propanol	5048.9Aa	4234.0Bb	tr	tr	0.0	0.0	–	–
1-Butanol	415.2Ab	485.9Aa	20831.5Aa	19841.5Aa	0.2	0.2	0.5	0.7
Isobutanol	32137.7Ab	40123.1Aa	12430.0Aa	16335.6Aa	0.4	0.5	0.2	0.2
1-Pentanol	tr	tr	6649.6Aa	2578.1Bb	—	—	0.1	0.0
Isoamyl alcohol	24353.8Aa	27075.7Aa	77193.0Aa	104872.7Aa	0.4	0.5	1.3	1.7
3-Methyl-3-buten-l-ol	11.78Ab	15.90Aa	nd	nd	0.0	0.0	—	—
3-Methyl-1-pentanol	48.0Aa	58.7Aa	1072.7Aa	1356.5Aa	0.1	0.1	2.1	2.7
4-Methyl-1-pentanol	28.0Aa	38.7Aa	599.9	nd	0.0	0.0	0.0	—
1-Heptanol	59.6Aa	42.9Bb	nd	nd	0.3	0.2	—	—
1-Octanol	18.3Aa	10.6Bb	117.0Aa	120.3Aa	0.0	0.0	0.1	0.2
2-Ethyl-1-hexanol	nd	7.3	nd	nd	—	0.0	—	—
2-Nonanol	72.9	tr	nd	nd	—	—	—	—
1-Decanol	11.1Aa	11.8Aa	nd	nd	0.0	0.0	—	—
1-Dodecanol	nd	1.7	nd	nd	—	—	—	—
Benzyl alcohol	475.5Aa	374.7Aa	24024.4Aa	11589.9Aa	0.0	0.0	0.1	0.1
2-Phenylethanol	17956.3Aa	22128.4Aa	6135.6Ab	12471.2Aa	1.3	1.6	0.4	0.9
laevo-2,3-Butanediol	343.0Aa	410.2Aa	nd	nd	0.0	0.0	—	—
(S)-3-Ethyl-4-methylpentanol	193.4Aa	86.7Bb	nd	nd	—	—	—	—
3-(Methylthio)-1-propanol	16.1Aa	19.1Aa	13.3Aa	13.3Aa	—	—	—	—
1,9-Nonanediol	2.6	nd	nd	nd	—	—	—	—
(3-Methyl-1,5-pentanediol)	1.0	nd	nd	nd	—	—	—	—
Total alcohols (mg/L)	107.1Ab	123.4Aa	215.3Ab	264.7Aa
Esters
Isoamyl acetate	tr	tr	334.4Aa	281.4Ab	—	—	2.1	1.8
Phenethyl acetate	tr	30.7	5526.1Aa	2225.1Bb	—	0.0	3.1	1.2
Ethyl acetate	56218.64Aa	53056.0Ab	20098.0Aa	23688.5Aa	7.5	7.1	2.7	3.2
Ethyl hexoate	718.93Aa	638.2Aa	639.7Aa	714.4Aa	9.0	8.0	8.8	9.3
Ethyl enanthate	81.9Aa	71.0Aa	tr	tr	0.0	0.0	—	0.0
Ethyl 2-hexenoate	29.9Aa	33.3Aa	nd	nd	—	—	—	—
Ethyl lactate	1582.0Bb	4798.4Aa	tr	4842.2	—	—	—	—
Ethyl octanoate	2112.1Aa	1294.3Bb	tr	tr	3.6	2.2	—	—
Ethyl laurate	tr	tr	241.3Aa	186.3Bb	—	—	—	—
Isoamyl hexanoate	nd	nd	110.9	tr	—	—	—	—
Methyl salicylate	28.4	nd	tr	tr	—	—	—	—
Ethyl decanoate	211.5Aa	115.4Aa	51.2Aa	22.3Bb	—	—	—	—
γ-butyrolactone	44.09Aa	53.9Aa	nd	nd	—	—	—	—
Diethyl butanedioate	154.5Bb	232.1Aa	tr	tr	—	—	—	—
Ethyl 9-decenoate	1089.6Aa	548.7Ab	8596.1Aa	3238.4Ab	—	—	—	—
n-Hexyl isobutyrate	5.6Aa	14.3Aa	nd	nd	—	—	—	—
Ethyl benzenepropanoate	12.8Aa	22.3Aa	113.9Bb	205.3Aa	—	—	—	—
Ethyl octadecanoate	16.7	nd	nd	nd	—	—	—	—
Ethyl hydroxycinnamate	14.4	nd	nd	nd	—	—	—	—
Ethyl eicosanoate	nd	24.7	nd	nd	—	—	—	—
Total esters (mg/L)	62.3Aa	60.9Ab	59.5Aa	52.9Ab
Acids
Propanoic acid	nd	4234.0	nd	nd	—	0.5	—	—
Hexanoic acid	1464.1Aa	1480.8Aa	1744.9Aa	1238.3Aa	3.5	3.5	4.2	2.9
Octanoic acid	1464.2Aa	1442.4Aa	1134.5Aa	780.5Aa	2.9	2.9	2.3	1.6
N-Decanoic acid	tr	32.7	238.9Aa	155.6Aa	—	0.0	0.2	0.2
Acetic acid	35385.5Aa	31412.0Aa	17526.0Aa	22524.6Aa	—	—	—	—
2-methyl-Propanoic acid	99.1Aa	116.2Aa	tr	tr	—	—	—	—
Total acids (mg/L)	38.4Aa	38.7Aa	20.6Aa	24.7Aa
Carbonyl compounds
Benzaldehyde	tr	tr	335.7Aa	495.7Aa	—	—	0.2	0.2
Total carbonyl compounds	tr	tr	335.7Aa	495.7Aa
Terpenes
Linalool	tr	1.8	3.3Bb	5.2Aa	—	0.1	0.1	0.2
Geraniol	7.1Aa	6.3Aa	63.9Aa	63.1Aa	0.4	0.3	3.2	3.2
Total terpenes	7.1Bb	8.0Aa	67.2Bb	68.3Aa
C13-norisoprenoid
β-Damascenone	5.5Bb	7.9Aa	detected	detected	39.4	56.4	—	—
Total C13-norisoprenoid	5.5Bb	7.9Aa	detected	detected
Others
4-Methyl-1-pentene	nd	46.3	nd	nd	—	—	—	—
Butylated hydroxytoluene	90.9Bb	237.3Aa	nd	2.9	—	—	—	—
Total others	90.9Bb	283.6Aa	nd	2.9

^aT1: Rain-shelter cultivation.

^bT2: Open-air cultivation.

Different letters means significant differences according to Duncan test in different treatments (p < 0.05).

nd not detected; tr the compound was detected but too little to quantitative.

^cThe concentrations of the volatile compounds were calculated by the curves of standards solutions that were listed in additional materials. And the odor activity values were calculated by the ratio of concentration and threshold listed in Table 3.

Figure 1. The total OAVs (∑OAV) of aroma series and tasting scores about volatile compounds in wines. The total OAVs (∑OAV) of aroma series in wines in 2010 (A) and 2011(B); the tasting scores about volatile compounds in wines of 2010(C) and 2011(D). T1: Rain-shelter cultivation; T2: Open-air cultivation.

Figure 2. Distribution of wine samples and loadings of volatile compounds in the first two PCs of volatile compounds. T1-10 Rain-shelter cultivation wine in vintage 2010; T2-10: Open-air cultivation wine in vintage 2010. T1-11: Rain-shelter cultivation wine in vintage 2011. T2-11: Open-air cultivation wine in vintage 2011. V1-V57: The volatile compounds in Table 4 from 1-hexanol to butylated hydroxytoluene in order.

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